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Journal Cover Geo UERJ
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  This is an Open Access Journal Open Access journal
   ISSN (Print) 1415-7543 - ISSN (Online) 1981-9021
   Published by Universidade do Estado do Rio de Janeiro Homepage  [38 journals]
  • Multiresidue determination of 114 multiclass pesticides in flue-cured
           tobacco by solid-phase extraction coupled with gas chromatography and
           tandem mass spectrometry

    • Authors: Jianmin Cao; Na Sun, Weisong Yu, Xueli Pang, Yingnan Lin, Fanyu Kong, Jun Qiu
      Abstract: A sensitive and robust multiresidue method for the simultaneous analysis of 114 pesticides in tobacco was developed based on solid-phase extraction coupled with gas chromatography and tandem mass spectrometry. In this strategy, tobacco samples were extracted with acetonitrile and cleaned up with a multilayer solid-phase extraction cartridge Cleanert TPT using acetonitrile/toluene (3:1) as the elution solvent. Two internal standards of different polarity were used to meet simultaneous pesticides quantification demands in the tobacco matrix. Satisfactory linearity in the range of 10–500 ng/mL was obtained for all 114 pesticides with linear regression coefficients higher than 0.994. The limit of detection and limit of quantification values were 0.02–5.27 and 0.06–17.6 ng/g, respectively. For most of the pesticides, acceptable recoveries in the range of 70–120% and repeatabilities (relative standard deviation) of
      PubDate: 2016-10-18T02:20:29.109276-05:
      DOI: 10.1002/jssc.201600914
  • Separation of polyethylene glycols and maleimide-terminated polyethylene

    • Authors: Yanzhen Wei; Renxi Zhuo, Xulin Jiang
      Abstract: The separation of polyethylene glycols and maleimide-substituted polyethylene glycol derivatives based on the number of maleimide end-groups under critical liquid chromatography conditions has been investigated on a reversed-phase column. The critical solvent compositions for nonfunctional polyethylene glycols and bifunctional maleimide-substituted polyethylene glycols were determined to be identical at about 40% acetonitrile in water on a reversed-phase octadecyl carbon chain-bonded silica column using mixtures of acetonitrile and water of varying composition as the mobile phase at 25°C. The maleimide-functionalized polyethylene glycols were successfully separated according to maleimide functionality (with zero, one, two, or three maleimide end-groups, respectively) under the critical isocratic elution conditions without obvious effect of molar mass. The separation was mainly due to the hydrophobic interaction between the maleimide end-groups and the column packing. Off-line matrix-assisted laser desorption/ionization time of flight mass spectrometry was used to identify the repeating units and, especially, the end-groups of the maleimide-substituted polyethylene glycols. Liquid chromatography analysis at critical conditions could provide useful information to optimize the synthesis of functional polyethylene glycols. To our knowledge, this is the first report of the baseline separation of maleimide-functionalized polyethylene glycols based on the functionality independent of the molar mass without derivatization by isocratic elution.
      PubDate: 2016-10-18T01:35:25.360789-05:
      DOI: 10.1002/jssc.201600904
  • Molecularly imprinted polymer membranes and thin films for the separation
           and sensing of biomacromolecules

    • Authors: Reinhard I. Boysen; Lachlan J. Schwarz, Dan V. Nicolau, Milton T. W. Hearn
      Abstract: This review describes recent advances associated with the development of surface imprinting methods for the synthesis of polymeric membranes and thin films, which possess the capability to selectively and specifically recognize biomacromolecules, such as proteins and single- and double-stranded DNA, employing “epitope” or “whole molecule” approaches. Synthetic procedures to create different molecularly imprinted polymer membranes or thin films are discussed, including grafting/in situ polymerization, drop-, dip-, or spin-coating procedures, electropolymerization as well as micro-contact or stamp lithography imprinting methods. Highly sensitive techniques for surface characterization and analyte detection are described, encompassing luminescence and fluorescence spectroscopy, X-ray photoelectron spectroscopy, FTIR spectroscopy, surface-enhanced Raman spectroscopy, atomic force microscopy, quartz crystal microbalance analysis, cyclic voltammetry, and surface plasmon resonance. These developments are providing new avenues to produce bioelectronic sensors and new ways to explore through advanced separation science procedures complex phenomena associated with the origins of biorecognition in nature.
      PubDate: 2016-10-18T01:25:26.129686-05:
      DOI: 10.1002/jssc.201600849
  • Gas chromatography analysis of major free mono- and disaccharides in milk:
           Method assessment, validation and application to real samples

    • Authors: Ilenia Idda; Nadia Spano, Marco Ciulu, Valeria M. Nurchi, Angelo Panzanelli, Maria I. Pilo, Gavino Sanna
      Abstract: Saccharides are functional constituents of milk. Although d-lactose represents almost the totality of the saccharides in the milk, minor species, like d-glucose, d-galactose, myo-inositol and, as a result of severe thermal treatments, monosaccharides like d-tagatose, are also detectable. Although chromatography has been the main analytical approach used for accomplishing this task, quite surprisingly a validated gas chromatographic method aimed at the simultaneous determination of these compounds is still needed. Hence, our contribution is devoted to fill this gap. After the optimization of clean-up and derivatization (conversion of saccharides in their trimethyl silyl ethers) steps, the adoption of a highly cross-linked silphenylene stationary phase permitted to obtain high resolution and a fast chromatographic run. Validation was accomplished in terms of limit of detection, limit of quantification, linearity, precision and trueness. The accuracy of the method was successfully tested on a number of partially skimmed milk samples. Excellent limits of detection for all analytes make this method eligible, also with respect of a gas chromatographic/mass spectrometry approach, for routine analysis and quality control in the dairy industries.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-17T07:20:30.836618-05:
      DOI: 10.1002/jssc.201600583
  • Retention of nucleic acids in ion-pair reversed-phase high-performance
           liquid chromatography depends not only on base composition but also on
           base sequence

    • Authors: Jun-qin Qiao; Chao Liang, Lan-chun Wei, Zhao-ming Cao, Hong-zhen Lian
      Abstract: The study on nucleic acid retention in ion-pair reversed-phase high-performance liquid chromatography mainly focuses on size-dependence, however, other factors influencing retention behaviors have not been comprehensively clarified up to date. In this present work, the retention behaviors of oligonucleotides and double-stranded DNAs were investigated on silica-based C18 stationary phase by ion-pair reversed-phase high-performance liquid chromatography. It is found that the retention of oligonucleotides was influenced by base composition and base sequence as well as size, and oligonucleotides prone to self-dimerization have weaker retention than those not prone to self-dimerization but with the same base composition. However, homo-oligonucleotides are suitable for the size-dependent separation as a special case of oligonucleotides. For double-stranded DNAs, the retention is also influenced by base composition and base sequence, as well as size. This may be attributed to the interaction of exposed bases in major or minor grooves with the hydrophobic alky chains of stationary phase. In addition, no specific influence of guanine and cytosine content was confirmed on retention of double-stranded DNAs. Notably, the space effect resulted from the stereostructure of nucleic acids also influences the retention behavior in ion-pair reversed-phase high-performance liquid chromatography.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-17T01:57:36.165401-05:
      DOI: 10.1002/jssc.201600701
  • First separation of four aromatic acids and two analogues with similar
           structures and polarities from Clematis akebioides by high-speed
           counter-current chromatography

    • Authors: Chengcheng Gong; Tao Chen, Huifeng Chen, Shanshan Zhang, Xinzhu Wang, Weiqing Wang, Jing Sun, Yulin Li, Zhixin Liao
      Abstract: In this paper, we report an efficient method by high-speed counter-current chromatography for the first separation of four aromatic acids and two analogues with similar structures and polarities from Clematis akebioides. Firstly, the ethyl acetate extract was treated by silica gel column chromatography to enrich the target compounds. And then the fraction with target compounds were purified by high-speed counter-counter chromatography using a two-phase solvent system consisting of chloroform/acetonitrile/water (10:6:4, v/v). The results showed high-speed counter-current chromatography could be a powerful technology for separation of compounds with similar structures and polarities. Besides, it was found acetonitrile could be a good methanol substitutes when a chloroform/methanol/water system could not provide a good separation factor. This study provides a reference for the separation compounds from Clematis akebioides.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-17T01:52:33.629433-05:
      DOI: 10.1002/jssc.201600805
  • Inorganic–organic hybrid coating material for the online in-tube
           solid-phase microextraction of monohydroxy polycyclic aromatic
           hydrocarbons in urine

    • Authors: ShuLing Wang; Hui Xu
      Abstract: An inorganic–organic hybrid nanocomposite (zinc oxide/polypyrrole) that represents a novel kind of coating for in-tube solid-phase microextraction is reported. The composite coating was prepared by a facile electrochemical polymerization strategy on the inner surface of a stainless steel tube. Based on the coating tube, a novel online in-tube solid-phase microextraction with liquid chromatography and mass spectrometry method was developed and applied for the extraction of three monohydroxy polycyclic aromatic hydrocarbons in human urine. The coating displayed good extraction ability toward monohydroxy polycyclic aromatic hydrocarbons. In addition, long lifespan, excellent stability, and good compression resistance were also obtained for the coating. The experimental conditions affecting the extraction were optimized systematically. Under the optimal conditions, the limits of detection and quantification were in the range of 0.039–0.050 and 0.130–0.167 ng mL−1, respectively. Good linearity (0.2–100 ng mL−1) was obtained with correlation coefficients larger than 0.9967. The repeatability, expressed as relative standard deviation, ranged between 2.5 and 9.4 %. The method offered the advantage of process simplicity, rapidity, automation, and sensitivity in the analysis of human urinary monohydroxy polycyclic aromatic hydrocarbons in two different cities of Hubei province. An acceptable recovery of monohydroxy polycyclic aromatic hydrocarbons (64–122%) represented the additional attractive features of the method in real urine analysis.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-17T01:52:17.512427-05:
      DOI: 10.1002/jssc.201600712
  • Progress and development of analytical methods for gibberellins

    • Authors: Chaozhi Pan; Swee Ngin Tan, Jean Wan Hong Yong, Liya Ge
      Abstract: Gibberellins, as a group of phytohormones, exhibit a wide variety of bio-functions within plant growth and development, which have been used to increase crop yields. Many analytical procedures, therefore, have been developed for the determination of the types and levels of endogenous and exogenous gibberellins. As plant tissues contain gibberellins in trace amounts (usually at the level of nanogram per gram fresh weight or even lower), the sample pre-treatment steps (extraction, pre-concentration, and purification) for gibberellins are reviewed in details. The primary focus of this comprehensive review is on the various analytical methods designed to meet the requirements for gibberellins analyses in complex matrices with particular emphasis on high-throughput analytical methods, such as gas chromatography, liquid chromatography, and capillary electrophoresis, mostly combined with mass spectrometry. The advantages and drawbacks of the each described analytical method are discussed. The overall aim of this review is to provide a comprehensive and critical view on the different analytical methods nowadays employed to analyze gibberellins in complex sample matrices and their foreseeable trends.
      PubDate: 2016-10-14T10:22:21.02635-05:0
      DOI: 10.1002/jssc.201600857
  • Quality evaluation of Shenmaidihuang Pills based on the chromatographic
           fingerprints and simultaneous determination of seven bioactive

    • Authors: Liu Sifei; Zhang Guangrui, Qiu Ying, Wang Xiaobo, Guo Lihan, Zhao Yanxin, Tong Meng, Wei Lan, Sun Lixin
      Abstract: In this study, we aimed to establish a comprehensive and practical quality evaluation system for Shenmaidihuang pills. A simple and reliable high-performance liquid chromatography coupled with photodiode array detection method was developed both for fingerprint analysis and quantitative determination. In fingerprint analysis, relative retention time and relative peak area were used to identify the common peaks in 18 samples for investigation. 21 peaks were selected as the common peaks to evaluate the similarities of 18 Shenmaidihuang pills samples with different manufacture dates. Furthermore, similarity analysis was applied to evaluate the similarity of samples. Hierarchical cluster analysis and principal component analysis were also performed to evaluate the variation of Shenmaidihuang pills. In quantitative analysis, linear regressions, injection precisions, recovery, repeatability and sample stability were all tested and good results were obtained to simultaneously determine the seven identified compounds, namely, 5-hydroxymethylfurfural, morroniside, loganin, paeonol, paeoniflorin, psoralen, isopsoralen in Shenmaidihuang pills. The contents of some analytes in different batches of samples indicated significant difference, especially for 5-hydroxymethylfurfural. So, it was concluded that the chromatographic fingerprint method obtained by high-performance liquid chromatography coupled with photodiode array detection associated with multiple compounds determination is a powerful and meaningful tool to comprehensively conduct the quality control of Shenmaidihuang pills.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-14T04:51:24.320127-05:
      DOI: 10.1002/jssc.201600718
  • Core–shell column Tanaka characterization and additional tests using
           active pharmaceutical ingredients

    • Authors: Jufang Wu Ludvigsson; Anders Karlsson, Viktor Kjellberg
      Abstract: In the last decade, core–shell particles have gained more and more attention in fast liquid chromatography separations due to their comparable performance with fully porous sub-2 μm particles and their significantly lower back pressure. Core–shell particles are made of a solid core surrounded by a shell of classic fully porous material. To embrace the developed core–shell column market and use these columns in pharmaceutical analytical applications, 17 core–shell C18 columns purchased from various vendors with various dimensions (50 mm x 2.1 mm to 100 mm x 3 mm) and particle sizes (1.6 μm to 2.7 μm) were characterized using Tanaka test protocols. Furthermore, four selected active pharmaceutical ingredients were chosen as test probes to investigate the batch to batch reproducibility for core–shell columns of particle size 2.6–2.7 μm, with dimension of 100×3 mm and columns of particle size 1.6 μm, with dimension 100×2.1 mm under isocratic elution. Columns of particle size 2.6–2.7 μm were also tested under gradient elution conditions. To confirm the claimed comparable efficiency of 2.6 μm core–shell particles as sub-2 μm fully porous particles, column performances of the selected core–shell columns were compared with BEH C18, 1.7 μm, a fully porous column material as well.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-14T04:51:19.023886-05:
      DOI: 10.1002/jssc.201600769
  • Longest Distance Shifting: A simple and efficient approach for the
           alignment of shifted chromatographic peaks

    • Authors: Bao Qiong Li; Jing Chen, Xue Wang, Min Li Xu, Hong Lin Zhai
      Abstract: The preprocessing of chromatograms such as the alignment of retention time shifts is often a crucial step in the proper data analysis chain. Here, an efficient approach to align shifted chromatographic signals, longest distance shifting, is presented and highlighted. The performance of this novel strategy was demonstrated by using both simulated chromatograms that covered the different kinds of retention time shifts and the real experimental chromatograms of Pudilan Xiaoyan Tablets obtained by high performance liquid chromatography-photodiode array detector. The averaged correlation coefficient were in the range of 0.9517–0.9840 and the peak factors were higher than 0.9717. As a comparison, all the chromatograms have also been aligned using correlation optimized warping and Interval Correlation Optimized Shifting algorithms. The obtained results indicate that the longest distance shifting algorithm is simpler, faster and more effective, and will be potentially suitable for the alignment of other types of signals.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-14T00:21:56.536847-05:
      DOI: 10.1002/jssc.201600811
  • Solid-phase extraction combined with dispersive liquid–liquid
           microextraction for the determination of pyrethroid pesticides in wheat
           and maize samples

    • Authors: Xiaodan Zhu; Chunhong Jia, Zuntao Zheng, Xiaoyuan Feng, Yue He, Ercheng Zhao
      Abstract: A rapid, selective and sensitive sample preparation method based on solid-phase extraction combined with dispersive liquid–liquid microextration was developed for the determination of pyrethroid pesticides in wheat and maize samples. Initially, the samples were extracted with acetonitrile and water solution followed phase separation with the salt addition. The following sample preparation involves a solid-phase extraction and dispersive liquid–liquid microextraction step which effectively provide cleanup and enrichment effects. The main experimental factors affecting the performance both of solid-phase extraction and dispersive liquid–liquid microextration were investigated. The validation results indicated the suitability of the proposed method for routine analyze of pyrethroid pesticides in wheat and maize samples. The fortified recoveries at three levels ranged between 76.4 and 109.8% with relative standard deviations of less than 10.7%. The limit of quantification of the proposed method was below 0.0125 mg/kg for the pyrethoroid pesticides. The proposed method was successfully used for the rapid determination of pyrethroid residues in real wheat and maize samples from crop field in Beijng China.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-14T00:21:43.688454-05:
      DOI: 10.1002/jssc.201600840
  • Synthesis of molecularly imprinted polymers using
           acrylamide-β-cyclodextrin as a co-functional monomer for the specific
           capture of tea saponins from the defatted cake extract of Camellia

    • Authors: Huiqin Guo; Jingjing Xiong, Wentian Ma, Minghuo Wu, Liushui Yan, Kexin Li, Yu Liu
      Abstract: Molecularly imprinted polymers were synthesized using mixed tea saponins as a template and acrylamide-β-cyclodextrin as a co-functional monomer for the specific binding and purification of tea saponins from the defatted cake extract of Camellia oleifera. The adsorption properties of the prepared polymers were systematically evaluated including adsorption kinetics, adsorption isotherms and selective recognition characteristics. It showed that the adsorption kinetics followed the pseudo-first-order kinetic model (R2 = 0.995) with an equilibrium time of 3 h, adsorption isotherm data fitted well with the Langmuir–Freundlich model (R2 = 0.984) with an adsorption capacity of 14.23 mg·g−1. The relative selectivity coefficient (k´) in the presence of the analogues glycyrrhizic acid and glycyrrhetinic acid were 1.16 and 17.21, respectively. The performance of the MIPs as solid-phase extraction materials was investigated and the results indicated that using acrylamide-β-cyclodextrin as a co-functional monomer improved both the adsorption capacity and active sites stability of the imprinted polymers. The solid-phase extraction using the polymers as packing materials were subsequently applied for the separation of tea saponins in raw Camellia oleifera press extract, and targets were obtained with a purity reaching 89%.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-13T03:50:31.841636-05:
      DOI: 10.1002/jssc.201600834
  • Ultrafiltration-LC–MS combined with semi-preparative high-performance
           liquid chromatography for the simultaneous screening and isolation of
           lactate dehydrogenase inhibitors from Belamcanda chinensis

    • Authors: Senlin Li; Sainan Li, Ying Tang, Chunming Liu, Lina Chen, Yuchi Zhang
      Abstract: Stroke represents the fourth leading cause of death in the USA and the second leading cause of death worldwide. Lactate dehydrogenase inhibitors are widely used in the treatment of ischemic stroke and natural products are considered a promising source of novel lactate dehydrogenase inhibitors. In this study, we used PC12 cells to determine the protective effect of extracts from the herb Belamcanda chinensis following toxic challenge. Using ultrafiltration high-performance liquid chromatography coupled with photo-diode array detection and electrospray ionization mass spectrometry, we screened and identified isoflavonoids from Belamcanda chinensis extracts. Semi-preparative high-performance liquid chromatography was then applied to separate and isolate the active constituents. Using these methods, we identified six major compounds in Belamcanda chinensis as lactate dehydrogenase inhibitors: tectoridin, iristectorin A, iridin, tectorigenin, irigenin, and irisflorentin, which were then isolated to>92% purity. This is the first report that Belamcanda chinensis extracts contain potent lactate dehydrogenase inhibitors. Our results demonstrate that the systematic isolation of bioactive components from Belamcanda chinensis guided by ultrafiltration high-performance liquid chromatography coupled with photo-diode array detection and electrospray ionization mass spectrometry represents a feasible and efficient technique that could be extended for the identification and isolation of other enzyme inhibitors.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-13T03:50:28.856546-05:
      DOI: 10.1002/jssc.201600703
  • Tablet-effervescence-assisted dissolved carbon flotation for the
           extraction of four triazole fungicides in water by gas chromatography with
           mass spectrometry

    • Authors: Qizhen Wei; Zhiyu Song, Jing Nie, Hailun Xia, Fujiang Chen, Zuguang Li, Mawrong Lee
      Abstract: A pretreatment method named tablet-effervescence-assisted dissolved carbon flotation was introduced for the determination of four triazole fungicides in environmental water. In this method, the use of effervescent tablet composed of nontoxic sodium carbonate and sodium dihydrogen phosphate could generate CO2 in situ to assist the dispersion of extraction solvent and to accelerate mass transfer of target analytes. In addition, the simple phase separation simply based on the rising of low-density organic solvent from the aqueous phase was applied rather than the application of apparatus, which demonstrated the potential for on-site extraction in the field. The experimental variables, including the composition of effervescent tablets, amount of effervescent tablets, types and volume of extraction solvent, were investigated. Under the optimized conditions, the method showed good linearity for myclobutanil, tebuconazole, epoxiconazole and difenoconazole in the range of 1–100 μg·L−1 . The limits of detection and the limits of quantification were within the range of 0.15–0.26 and 0.49–0.86 μg·L−1, respectively. The obtained correlation coefficients varied from 0.997 to 0.999, and suitable enrichment factors were 422–589. The recoveries were 82.5–112.9% with relative standard deviations of 4.7–13.5%.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-13T02:01:16.786086-05:
      DOI: 10.1002/jssc.201600619
  • Recent applications of hydrophilic interaction liquid chromatography in
           pharmaceutical analysis

    • Authors: Qian Zhang; Feng-Qing Yang, Liya Ge, Yuan-Jia Hu, Zhi-Ning Xia
      Abstract: Hydrophilic interaction liquid chromatography, an alternative liquid chromatography mode, is of particular interest in separating hydrophilic and polar ionic compounds. Compared with traditional liquid chromatography techniques, hydrophilic interaction liquid chromatography offers specific advantages mainly including: (1) relatively green and water-soluble mobile phase composition, which enhances the solubility of hydrophilic and polar ionic compounds; (2) no need for ion-pairing reagents and high content of organic solvent, which benefits mass spectrometry detection; (3) high orthogonality to reverse-phase liquid chromatography, well adapted to two-dimensional liquid chromatography for complicated samples. Therefore, hydrophilic interaction liquid chromatography has been rapidly developed in many areas over the past decades. This review summarizes the recent progress (from 2012 to July 2016) of hydrophilic interaction liquid chromatography in pharmaceutical analysis, with the focus on detecting chemical drugs in various matrices, charactering active compounds of natural products and assessing biotherapeutics through typical structure unit. Moreover, the retention mechanism and behavior of analytes in hydrophilic interaction liquid chromatography as well as some novel hydrophilic interaction liquid chromatography columns used for pharmaceutical analysis are also described.
      PubDate: 2016-10-13T01:06:05.726442-05:
      DOI: 10.1002/jssc.201600843
  • Advances in the development and applications of organic–silica
           hybrid monoliths

    • Authors: Zuzana Zajickova
      Abstract: This review will concentrate on recent progress (since 2013) toward preparation of organic–silica hybrid monoliths and their latest applications as extraction and separation media largely focusing on capillary liquid chromatography and capillary electrochromatography. Main emphasis will be given to advancement of approaches relying on the sol–gel chemistry of tetra- and tri-alkoxysilanes, sol–gel chemistry of alkoxysilanes and free-radical copolymerization with organic monomers, and free radical and ring-opening copolymerization of polyhedral oligomeric silsesquioxanes with organic monomers. Hybrid molecularly-imprinted polymer monoliths and hybrid monoliths made with non-silica-based precursors or in combination with metal alkoxides will be included as well.
      PubDate: 2016-10-12T10:46:58.906496-05:
      DOI: 10.1002/jssc.201600774
  • Rapid characterization of the chemical constituents of Cortex Fraxini by
           homogenate extraction followed by UHPLC coupled with Fourier transform ion
           cyclotron resonance mass spectrometry and GC–MS

    • Authors: Yinan Wang; Fei Han, Aihua Song, Miao Wang, Min Zhao, Chunjie Zhao
      Abstract: Cortex Fraxini is an important traditional Chinese medicine. In this work, a rapid and reliable homogenate extraction method was applied for the fast extraction for Cortex Fraxini, and the method was optimized by response surface methodology. Ultra high performance liquid chromatography combined with Fourier transform ion cyclotron resonance mass spectrometry and gas chromatography with mass spectrometry were established for the separation and characterization of the constituents of Cortex Fraxini. Liquid chromatography separation was conducted on a C18 column (150 mm × 2.1 mm, 1.8 μm), and gas chromatography separation was performed on a capillary with a 5% phenyl-methylpolysiloxane stationary phase (30 m × 0.25 mm × 0.25 mm) by injection of silylated samples. According to the results, 33 chemical compounds were characterized by liquid chromatography with mass spectrometry, and 11 chemical compounds were characterized by gas chromatography with mass spectrometry, and coumarins were the major components characterized by both gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. The proposed homogenate extraction was an efficient and rapid method, and coumarins, phenylethanoid glycosides, iridoid glycosides, phenylpropanoids, and lignans were the main constituents of Cortex Fraxini. This work laid the foundation for further study of Cortex Fraxini and will be helpful for the rapid extraction and characterization of ingredients in other traditional Chinese medicines.
      PubDate: 2016-10-12T10:46:46.459845-05:
      DOI: 10.1002/jssc.201600851
  • Study of solvent effects on the stability constant and ionic mobility of
           the dibenzo-18-crown-6 complex with potassium ion by affinity capillary

    • Authors: Renáta Konášová; Jana Jaklová Dytrtová, Václav Kašička
      Abstract: The effect of solvent on the strength of noncovalent interactions and ionic mobility of the dibenzo-18-crown-6 complex with K+ in water/organic solvents was investigated by using affinity capillary electrophoresis. The proportion of organic solvent (methanol, ethanol, propan-2-ol, and acetonitrile) in the mixtures ranged from 0 to 100 vol.%. The stability constant, KKL, and actual ionic mobility of the dibenzo-18-crown-6-K+ complex were determined by the nonlinear regression analysis of the dependence of the effective electrophoretic mobility of dibenzo-18-crown-6 on the concentration of K+ (added as KCl) in the background electrolyte (25 mM lithium acetate, pH 5.5, in the above mixed hydro–organic solvents). Competitive interaction of the dibenzo-18-crown-6 with Li+ was observed and quantified in mixtures containing more than 60 vol.% of the organic solvent. However, the stability constant of the dibenzo-18-crown-6-Li+ complex was in all cases lower than 0.5 % of KKL. The log KKL increased approximately linearly in the range 1.62–4.98 with the increasing molar fraction of organic solvent in the above mixed solvents and with similar slopes for all four organic solvents used in this study. The ionic mobilities of the dibenzo-18-crown-6-K+ complex were in the range (6.1–43.4) × 10−9 m2 V−1 s−1.
      PubDate: 2016-10-12T08:16:07.706236-05:
      DOI: 10.1002/jssc.201600830
  • High-performance liquid chromatography coupled with tandem mass
           spectrometry technology in the analysis of Chinese Medicine Formulas: A
           bibliometric analysis (1997–2015)

    • Authors: Xi-Ran He; Chun-Guang Li, Xiao-Shu Zhu, Yuan-Qing Li, Mariam Jarouche, Alan Bensoussan, Ping-Ping Li
      Abstract: There is a recognized challenge in analyzing traditional Chinese medicine formulas because of their complex chemical compositions. The application of modern analytical techniques such as high-performance liquid chromatography coupled with a tandem mass spectrometry has improved the characterization of various compounds from traditional Chinese medicine formulas significantly. This study aims to conduct a bibliometric analysis to recognize the overall trend of high-performance liquid chromatography coupled with tandem mass spectrometry approaches in the analysis of traditional Chinese medicine formulas, its significance and possible underlying interactions between individual herbs in these formulas. Electronic databases were searched systematically, and the identified studies were collected and analyzed using Microsoft Access 2010, Graph Pad 5.0 software and Ucinet software package. 338 publications between 1997 and 2015 were identified, and analyzed in terms of annual growth and accumulated publications, top journals, forms of traditional Chinese medicine preparations and highly studied formulas and single herbs, as well as social network analysis of single herbs. There is a significant increase trend in using high-performance liquid chromatography coupled with tandem mass spectrometry related techniques in analysis of commonly used forms of traditional Chinese medicine formulas in the last three years. Stringent quality control is of great significance for the modernization and globalization of traditional Chinese medicine, and this bibliometric analysis provided the first and comprehensive summary within this field.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T07:55:51.030362-05:
      DOI: 10.1002/jssc.201600784
  • Graphene-based pipette tip solid-phase extraction with ultra-high
           performance liquid chromatography and tandem mass spectrometry for the
           analysis of carbamate pesticide residues in fruit juice

    • Authors: Zhihong Shi; Qi Li, Dan Xu, Qingru Huai, Hongyi Zhang
      Abstract: Graphene-based pipette tip solid-phase extraction was combined with ultra-high performance liquid chromatography and tandem mass spectrometry for the determination of carbamate pesticide residues in fruit juice samples. Four milligrams of graphene was used as sorbent material to pack a 1000 μL pipette tip for the extraction of pirimicarb, propoxur, isoprocarb, fenobucarb, and diethofencarb from 3 mL of fruit juice sample. The whole extraction process was finished in 12 min, and the volume of eluent used was only 1.5 mL. Under the optimized conditions, good linear relationship (R> 0.999) and lower limits of detection (0.0022–0.033 ng/mL) were achieved. The recoveries at three spiked levels ranged from 80.90 to 124.60% with relative standard deviations less than 4.88%. Compared with commercially available sorbents including propylsulfonic acid silica, graphitized carbon black, and C18, graphene was superior in extraction efficiency. The proposed method is simple, rapid, sensitive, selective, and solvent saving.
      PubDate: 2016-10-12T06:26:41.097015-05:
      DOI: 10.1002/jssc.201600498
  • Toward a comprehensive microextraction/determination unit: A chip silicon
           rubber polyaniline-based system and its direct coupling with gas
           chromatography and mass spectrometry

    • Authors: Habib Bagheri; Misagh Allahdadlalouni, Cyrus Zamani
      Abstract: An inexpensive silicon rubber-based chip was constructed by fabricating a triangle-shaped microcanal with a 135 μm width and 234 μm depth by laser ablation technique. The fabricated groove was sealed by a thin glass cover while two pieces of stainless-steel tubing were connected to each side of the canal. Then, a thin polyaniline film was synthesized on the walls of the canal by chemical oxidation using a syringe pump to deliver the relevant reagents. The microfluidic system was eventually connected to a gas chromatography-mass spectrometry. To evaluate the capability of the constructed microfluidic system, it was implemented to the analysis of submilliliter volumes of environmental samples spiked with the trace amounts of some pesticide residues. To show the applicability of the hyphenated system, the extraction/determination of triazines was implemented while only 500 μL sample with the limits of detection ranged from 0.2 to 0.5 ng/mL could be easily achieved. In addition, the influential extraction parameters such as sample volume, flow rate, and sample pH were optimized. Under the optimized conditions, the relative standard deviation values for double-distillated water sample spiked with the selected triazines at 250 ng/mL were 6.5–12.5% (n = 3).
      PubDate: 2016-10-12T06:26:38.953014-05:
      DOI: 10.1002/jssc.201600500
  • Determination and removal of sulfonamides and quinolones from
           environmental water samples using magnetic adsorbents

    • Authors: Hao Wu; Yating Shi, Xiaozhen Guo, Shuangli Zhao, Juanli Du, Hongping Jia, Lina He, Liming Du
      Abstract: In this study, the magnetic materials known as polymerized ionic liquid@3-(trimethoxysilyl)propyl methacrylate@Fe3O4 nanoparticles were synthesized and utilized as potential adsorbents. First, these nanoparticles were applied to the analysis of sulfonamides and quinolones present in different water samples using magnetic solid phase extraction and high-performance liquid chromatography. Under optimized conditions, the developed method showed excellent detection sensitivity, with limits of detection (S/N = 3) and quantification limits (S/N = 10) within 0.2–1.0 and 0.8–3.4 μg/L, respectively. The spiked recoveries of the SAs and QNs in environmental water samples ranged from 83.5 to 103.0%, with RSDs of less than 4.5%.In addition, the adsorbents effectively removed sulfamethoxazole and ofloxacin present in existing aquatic environments. The adsorption kinetics and isotherms of sulfamethoxazole and ofloxacin on the magnetic adsorbents were studied to assess removal performance. The results indicate that the adsorption process follows a pseudo-second-order mechanism, which reveals that the sorption mechanism is the rate-limiting step and produces high qmax values (sulfamethoxazole = 70.35 mg/g and ofloxacin = 48.95 mg/g), thus demonstrating the enormous adsorption capacity of these magnetic adsorbents.
      PubDate: 2016-10-12T06:26:28.39687-05:0
      DOI: 10.1002/jssc.201600631
  • Determination of selected fatty acids in dried sweat spot using gas
           chromatography with flame ionization detection

    • Authors: Roman Kanďár; Petra Drábková, Lenka Andrlová, Adam Kostelník, Alexander Čegan
      Abstract: A method is described for the determination of fatty acids in dried sweat spot and plasma samples using gas chromatography with flame ionization detection. Plasma and dried sweat spot samples were obtained from a group of blood donors. The sweat was collected from each volunteer during exercise. Sweat was spotted onto collection paper containing butylated hydroxytoluene. Fatty acids were derivatized with acetyl chloride in methanol to form methyl esters of fatty acids. The fatty acids in dried sweat spot samples treated with butylated hydroxytoluene and stored at –20°C were stable for 3 months. Our results indicate that sweat contains, among fatty acids with short chain, also fatty acids with long chain and unsaturated fatty acids. Linear relationships between percentage content of selected fatty acids in dried sweat spot and plasma were observed.
      PubDate: 2016-10-12T06:26:19.488017-05:
      DOI: 10.1002/jssc.201600513
  • Determination of arsenic species in solid matrices utilizing supercritical
           fluid extraction coupled with gas chromatography after derivatization with
           thioglycolic acid n-butyl ester

    • Authors: Zhifeng Wang; Zhaojie Cui
      Abstract: A method using derivatization and supercritical fluid extraction coupled with gas chromatography was developed for the analysis of dimethylarsinate, monomethylarsonate and inorganic arsenic simultaneously in solid matrices. Thioglycolic acid n-butyl ester was used as a novel derivatizing reagent. A systematic discussion was made to investigate the effects of pressure, temperature, flow rate of the supercritical CO2, extraction time, concentration of the modifier and microemulsion on extraction efficiency. The application for real environmental samples was also studied. Results showed that thioglycolic acid n-butyl ester was an effective derivatizing reagent that could be applied for arsenic speciation. Using methanol as modifier of the supercritical CO2 can raise the extraction efficiency, which can be further enhanced by adding a microemulsion that contains Triton X-405. The optimum extraction conditions were: 25 MPa, 90°C, static extraction for 10 min, dynamic extraction for 25 min with a flow rate of 2.0 mL min−1 of supercritical CO2 modified by 5% v/v methanol and microemulsion. The detection limits of dimethylarsinate, monomethylarsonate and inorganic arsenic in solid matrices were 0.12, 0.26 and 1.1 mg kg−1, respectively. The optimized method was sensitive, convenient and reliable for the extraction and analysis of different arsenic species in solid samples.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T05:01:46.136577-05:
      DOI: 10.1002/jssc.201600510
  • Capillary electrochromatography of proteins and peptides (2006-2015)

    • Authors: Ivan Mikšík
      Abstract: This review summarizes the development and the applications of capillary electrochromatographic techniques pertinent to the analysis of proteins and peptides, which took place over the last ten years (2006–middle 2016). This “hybrid” technique is useful for the analysis of a broad spectrum of proteins and peptides and is an approach that is complementary to the liquid chromatographic and the capillary electrophoretic analysis. All modes of capillary electrochromatography are described here, which includes particle packed columns, monolithic stationary phases and open-tubular capillary electrochromatography.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T04:56:14.52253-05:0
      DOI: 10.1002/jssc.201600908
  • Hybrid molecularly imprinted polymers modified by deep eutectic solvents
           and ionic liquids with three templates for the rapid simultaneous
           purification of rutin, scoparone and quercetin from Herba Artemisiae

    • Authors: Guizhen Li; Wha Seung Ahn, Kyung Ho Row
      Abstract: Different kinds of deep eutectic solvents based on choline chloride and ionic liquids based on 1-methylimidazole were used to modify hybrid molecularly imprinted polymers with the monomer γ-aminopropyltriethoxysilane-methacrylic and three templates (rutin, scoparone, and quercetin). The materials were adopted as solid-phase extraction packing agents, and were characterized by FTIR spectroscopy and field emission scanning electron microscopy. The hybrid molecularly imprinted polymers modified by deep eutectic solvents had high recoveries and a strong recognition of rutin, scoparone, and quercetin in Herba Artemisiae Scopariae than those modified by ionic liquids. In the procedure of solid-phase extraction, deep eutectic solvents-2-hybrid molecularly imprinted polymers were obtained with the best recoveries with rutin (92.27%), scoparone (87.51%), and quercetin (80.02%), and the actual extraction yields of rutin (5.6 mg·g−1), scoparone (2.3 mg·g−1), and quercetin (3.4 mg·g−1). Overall, the proposed approach with the high affinity of hybrid molecularly imprinted polymers might offer a novel method for the purification of complex samples.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T01:21:45.790194-05:
      DOI: 10.1002/jssc.201600892
  • Rapid selective accelerated solvent extraction and simultaneous
           determination of herbicide atrazine and its metabolites in fruit by ultra
           high performance liquid chromatography

    • Authors: Licong Jia; Ming Su, Xingqiang Wu, Hanwen Sun
      Abstract: A selective accelerated solvent extraction procedure achieved one step extraction and clean up for analysis of herbicide atrazine and its metabolites in fruit. Using a BEH C18 analytical column and the gradient mode with 2 mM ammonium acetate aqueous solution/acetonitrile as a mobile phase achieved effective chromatographic separation of the five analytes within 4 min. The calibration curves were linear over two orders of magnitude of concentration with correlation coefficients (r) of 0.9996‒0.9999. The method limit of quantification was 1, 2, 1.5, 3, and 2 μg/kg for atrazine, desethylatrazine, desisopropylatrazine, desethyldesisopropylatrazine, and hydroxyatrazine, respectively, in the case of atrazine it is at least two orders of magnitude lower than the maximum residue limit (0.25 mg/kg). The intra-day and inter-day precisions of the five analytes were in the range of 2.1–3.5 and 3.1–4.8 %, respectively. The recoveries of the five analytes at three spiked levels varied from 85.9 to 107% with a relative standard deviation of 1.8–4.9% for pear and apple samples. The ultra high performance liquid chromatography with diode array detection method was proved to be fast, inexpensive, selective, sensitive, and accurate for the quantification of the analytes in pear and apple samples.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T00:51:04.706724-05:
      DOI: 10.1002/jssc.201600883
  • Polymer-based Monolithic Column with an Incorporated Chiral
           Metal–Organic Framework for the Enantioseparation of Methyl Phenyl
           Sulfoxide Using Nano-Liquid Chromatography

    • Authors: Xin Wang; Alexandros Lamprou, Frantisek Svec, Yu Bai, Huwei Liu
      Abstract: A new approach to the preparation of enantioselective porous polymer monolithic columns with incorporated chiral metal–organic framework for nano-liquid chromatography has been developed. While no enantioseparation was achieved with monolithic poly(4-vinylpyridine-co-ethylene dimethacrylate) column, excellent separations of both enantiomers of (±)-methyl phenyl sulfoxide were achieved with its counterpart prepared after admixing the metal–organic framework [Zn2(benzene dicarboxylate)(l-lactic acid)(dmf)](DMF), which is synthesized from zinc nitrate, l-lactic acid, and benzene dicarboxylic acid in the polymerization mixture. These novel monolithic columns combined the selectivity of the chiral framework with the excellent hydrodynamic properties of polymer monoliths, may provide a great impact on future studies in the field of chiral analysis by liquid chromatography.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-12T00:50:55.587203-05:
      DOI: 10.1002/jssc.201600810
  • Simultaneous quantitation of 14 active components in Yinchenhao decoction
           by using ultra high performance liquid chromatography with diode array
           detection: Method development and ingredient analysis of different
           commonly prepared samples

    • Authors: YaXiong Yi; Yong Zhang, Yue Ding, Lu Lu, Tong Zhang, Yuan Zhao, XiaoJun Xu, YuXin Zhang
      Abstract: We developed a novel quantitative analysis method based on ultra high performance liquid chromatography coupled with diode array detection for the simultaneous determination of the 14 main active components in Yinchenhao decoction. All components were separated on an Agilent SB-C18 column by using a gradient solvent system of acetonitrile/0.1% phosphoric acid solution at a flow rate of 0.4 mL/min for 35 min. Subsequently, linearity, precision, repeatability, and accuracy tests were implemented to validate the method. Furthermore, the method has been applied for compositional difference analysis of 14 components in eight normal-extraction Yinchenhao decoction samples, accompanied by hierarchical clustering analysis and similarity analysis. The result that all samples were divided into three groups based on different contents of components demonstrated that extraction methods of decocting, refluxing, ultrasonication and extraction solvents of water or ethanol affected component differentiation, and should be related to its clinical applications. The results also indicated that the sample prepared by patients in the family by using water extraction employing a casserole was almost same to that prepared using a stainless-steel kettle, which is mostly used in pharmaceutical factories. This research would help patients to select the best and most convenient method for preparing Yinchenhao decoction.
      PubDate: 2016-10-10T07:36:16.304822-05:
      DOI: 10.1002/jssc.201600284
  • Competitive effect of glucose–fructose adsorption in a fixed-bed
           chromatographic column

    • Authors: Preuk Tangpromphan; Amaraporn Kaewchada, Attasak Jaree
      Abstract: A continuous operation separation system such as a simulated moving-bed process requires adsorption data with precise equilibrium and kinetic model parameters in a single chromatographic column. The adsorption of glucose and fructose in a fixed-bed chromatographic column was investigated to determine the competition effect of each resulting from their initial molar ratios. The model parameters including bed porosity and axial dispersion coefficient were determined using the moment analysis method. The equilibrium isotherm parameters were estimated by experiment at various molar ratios and initial sugar concentrations. The parameters obtained were then used for the simulation of dynamic breakthrough curves of glucose and fructose. The equilibrium isotherms revealed that the linear adsorption pattern provided good prediction for each molar ratio using the Henry equation. In addition, the modified Langmuir model was proposed to account for the competitive adsorption, due to the cooperative competition effect whereby glucose was promoted to the active site by fructose at a higher extent than vice versa. A positive relationship between the experimental and numerical data of the adsorption time profiles was also observed.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-10T04:50:42.297113-05:
      DOI: 10.1002/jssc.201600572
  • Analysis of melamine and analogues in complex matrices: Advances and

    • Authors: Tingting Wang; Junfeng Ma, Yihui Chen, Ying Li, Lihua Zhang, Yukui Zhang
      Abstract: Analysis of melamine and its analogues is of increasing research interest recently. Owing to their high nitrogen content and low price, they were deliberately added to artificially enhance protein concentration in a number of different types of human and animal food sources. In addition, environmental water might also be contaminated by melamine due to its use in the chemical industry and the degradation of the pesticide cyromazine. Herein we provide a detailed overview of recently developed materials and techniques for the analysis of melamine and its analogues in complex matrices, especially in dairy products (e.g., milk and powdered milk) and environmental water.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-10T04:50:40.39342-05:0
      DOI: 10.1002/jssc.201600854
  • Investigation of the chemical markers for experiential quality evaluation
           of crude aconite by UHPLC–Q-TOF-MS

    • Authors: Ding-kun Zhang; Xue Han, Rui-yu Li, Ming Niu, Qin Dong, Ming Yang, Jia-bo Wang, Xiao-he Xiao
      Abstract: Many foods and herbs are experientially classified into different commodity grades in commercial circulation. Regarding the hypertoxic herb aconite, large samples are considered to be of better quality. However, this experiential classification lacks a scientific basis. In this study, we focused on the quality diversity among different grades and studied it using the minimum lethal dose assay and a novel ultra high performance liquid chromatography coupled with time-of-flight mass spectrometry method. Toxicity assay result suggested grade I aconite had the lowest toxicity (p < 0.05). Using this method with partial least squares-discriminant analysis, we discovered nine chemomarkers, including neoline, songorine, fuziline, mesaconitine, talatizidine, dexyaconitine, talatisamine, hypaconitine, and fuzitine. Considering their toxicity and activity, we found the levels of toxic ingredients hypaconitine, dexyaconitine, and mesaconitine in grade I were lower than those in grade II (p < 0.01), while the levels of efficacy ingredients songorine, talatisamine, and neoline were the highest in grade I (p < 0.01). Further study demonstrated that the quality variation was associated with plant tissue development and toxic ingredient distribution law. Our results provide scientific evidence for the experiential quality evaluation of aconite, and it will be of great utility for other foods and herbs.
      PubDate: 2016-10-10T04:35:39.534531-05:
      DOI: 10.1002/jssc.201600567
  • Multivariate analysis of the volatile components in tobacco based on
           infrared-assisted extraction coupled to headspace solid-phase
           microextraction and gas chromatography-mass spectrometry

    • Authors: Yanqin Yang; Yuanjiang Pan, Guojun Zhou, Guohai Chu, Jian Jiang, Kailong Yuan, Qian Xia, Changhe Cheng
      Abstract: A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics.
      PubDate: 2016-10-10T04:31:07.578653-05:
      DOI: 10.1002/jssc.201600503
  • Polydimethylsiloxane-coated partitioning sample collection device for the
           precise quantification of polycyclic aromatic hydrocarbons in air

    • Authors: Ikuo Ueta; Moe Onikata, Koji Fujimura, Tomotaka Yoshimura, Shoji Narukami, Suguru Mochizuki, Tomohiro Sasaki, Tsuneaki Maeda
      Abstract: A novel partitioning collection device comprising a glass cartridge packed with poly(dimethylsiloxane)-coated macroporous silica particles was developed for the precise quantification of polycyclic aromatic hydrocarbons in air. The analyte collection and elution performances achieved using different amounts of poly(dimethylsiloxane) coating were quantitatively evaluated. The sample retention power increased with increasing the coating, and more than 250 L of air could be collected without analyte breakthrough at a sampling temperature of 35°C. During the air collection, the moisture in the air was not retained on the particles due to the hydrophobic surface of the sorbent. A complete and rapid elution of the collected analytes from the device was accomplished by the passage of only 10 mL of acetone with ultrasonication for 1 min. The proposed method was successfully applied for the determination of airborne polycyclic aromatic hydrocarbons in tunnel air.
      PubDate: 2016-10-10T04:31:01.701785-05:
      DOI: 10.1002/jssc.201600752
  • Comparative analysis of the main bioactive components of Xin-Sheng-Hua
           granule and its single herbs by ultrahigh performance liquid
           chromatography with tandem mass spectrometry

    • Authors: Hanqing Pang; Jun Wang, Yuping Tang, Huiqin Xu, Liang Wu, Yi Jin, Zhenhua Zhu, Sheng Guo, Xuqin Shi, Shengliang Huang, Dazheng Sun, Jin-ao Duan
      Abstract: Xin-Sheng-Hua granule, a representative formula for postpartum hemorrhage, has been used clinically to treat postpartum diseases. Its main bioactive components comprise aromatic acids, phthalides, alkaloids, flavonoids, and gingerols among others. To investigate the changes in main bioactive constituents in its seven single herbs before and after compatibility, a rapid, simple, and sensitive method was developed for comparative analysis of 27 main bioactive components by using ultrahigh-performance liquid chromatography with triple quadrupole electrospray tandem mass spectrometry for the first time. The sufficient separation of 27 target constituents was achieved on a Thermo Scientific Hypersil GOLD column (100 mm × 3 mm, 1.9 μm) within 20 min under the optimized chromatographic conditions. Compared with the theoretical content, the observed content of each analyte showed remarkable differences in Xin-Sheng-Hua granule except thymine, p-coumaric acid, senkyunolide I, senkyunolide H, and ligustilide; the total contents of 27 components increased significantly, and the content variation degrees for the different components were gingerols> flavonoids> aromatic acids> alkaloids> phthalides. The results could provide a good reference for the quality control of Xin-Sheng-Hua granule and might be helpful to interpret the drug interactions based on variation of bioactive components in formulae.
      PubDate: 2016-10-06T01:48:23.22866-05:0
      DOI: 10.1002/jssc.201600606
  • Preconcentration and determination of ceftazidime in real samples using
           dispersive liquid–liquid microextraction and high-performance liquid
           chromatography with the aid of experimental design

    • Authors: Rasoul Razmi; Behrouz Shahpari, Eslam Pourbasheer, Mohammad Hasan Boustanifar, Zhila Azari, Amin Ebadi
      Abstract: A rapid and simple method for the extraction and preconcentration of ceftazidime in aqueous samples has been developed using dispersive liquid–liquid microextraction followed by high-performance liquid chromatography analysis. The extraction parameters, such as the volume of extraction solvent and disperser solvent, salt effect, sample volume, centrifuge rate, centrifuge time, extraction time, and temperature in the dispersive liquid–liquid microextraction process, were studied and optimized with the experimental design methods. Firstly, for the preliminary screening of the parameters the taguchi design was used and then, the fractional factorial design was used for significant factors optimization. At the optimum conditions, the calibration curves for ceftazidime indicated good linearity over the range of 0.001–10 μg/mL with correlation coefficients higher than the 0.98, and the limits of detection were 0.13 and 0.17 ng/mL, for water and urine samples, respectively. The proposed method successfully employed to determine ceftazidime in water and urine samples and good agreement between the experimental data and predictive values has been achieved.
      PubDate: 2016-10-06T01:47:29.48468-05:0
      DOI: 10.1002/jssc.201600639
  • Development of a dispersive liquid–liquid microextraction method using a
           lighter-than-water ionic liquid for the analysis of polycyclic aromatic
           hydrocarbons in water

    • Authors: Giselle S. Medina; Mario Reta
      Abstract: A dispersive liquid–liquid microextraction method using a lighter-than-water phosphonium-based ionic liquid for the extraction of 16 polycyclic aromatic hydrocarbons from water samples has been developed. The extracted compounds were analyzed by liquid chromatography coupled to fluorescence/diode array detectors. The effects of several experimental parameters on the extraction efficiency, such as type and volume of ionic liquid and disperser solvent, type and concentration of salt in the aqueous phase and extraction time, were investigated and optimized. Three phosphonium-based ionic liquids were assayed, obtaining larger extraction efficiencies when trihexyl-(tetradecyl)phosphonium bromide was used. The optimized methodology requires a few microliters of a lighter-than-water phosphonium-based ionic liquid, which allows an easy separation of the extraction solvent phase. The obtained limits of detection were between 0.02 and 0.56 μg/L, enrichment factors between 109 and 228, recoveries between 60 and 108%, trueness between 0.4 and 9.9% and reproducibility values between 3 and 12% were obtained. These figures of merit combined with the simplicity, rapidity and low cost of the analytical methodology indicate that this is a viable and convenient alternative to the methods reported in the literature. The developed method was used to analyze polycyclic aromatic hydrocarbons in river water samples.
      PubDate: 2016-10-06T01:47:13.967019-05:
      DOI: 10.1002/jssc.201600758
  • Trilinear analysis of thin-layer chromatography retention of 35 model
           compounds chromatographed on nine adsorbents with 20 pure solvents

    • Authors: Łukasz Komsta; Robert Skibiński, Natalia Bezpalko, Aleksandra Mielniczek, Barbara Stępkowska
      Abstract: The RF value dataset of 35 model compounds, chromatographed with 20 pure solvents as the mobile phase each on nine adsorbents: RP2, RP8, RP18, alumina, cellulose, CN, DIOL, NH2, and silica, was subjected to trilinear analysis with parallel factor analysis. The two-factor optimal model explained 87% of total information in this complex dataset. The first obtained score (trend) represents two features: the presence of hydrogen bonding and heteroatoms of solute and the mean elution force of the solvent. The second trend represents molecule size, aromaticity, and number of carbons, interconnected with presence of chlorine in mobile phase. The correlation between the scores and molecular descriptors were checked to interpret these trends quantitatively. The scores of adsorbents were slightly intercorrelated, showing NH2, alumina, and cellulose as outliers from main adsorbents cloud. The obtained results suggest that molecular size and aromaticity, connected with chlorine atoms in mobile phase, is the second source of retention variability.
      PubDate: 2016-10-06T01:47:02.095935-05:
      DOI: 10.1002/jssc.201600705
  • Magnetic molecularly imprinted composite for the selective solid-phase
           extraction of p-aminosalicylic acid followed by high-performance liquid
           chromatography with ultraviolet detection

    • Authors: Hasan Bagheri; Karam Molaei, Ali Akbar Asgharinezhad, Homeira Ebrahimzadeh, Mojtaba Shamsipur
      Abstract: A new method for the selective extraction of p-aminosalicylic acid from aqueous and urine samples has been developed using magnetic molecularly imprinted polymer nanoparticles before determination by high-performance liquid chromatography. The Fe3O4 nanoparticles were first prepared through the chemical coprecipitation of Fe2+ and Fe3+ and then coated with a vinyl shell. Subsequently, a layer of molecularly imprinted polymers was grafted onto the vinyl-modified magnetic nanoparticles by precipitation polymerization. FTIR spectroscopy, scanning electron microscopy, vibrating sample magnetometry, and thermogravimetric analysis were applied to characterize the sorbent properties. Moreover, the predominant parameters affecting the magnetic solid phase extraction such as sample pH, sorption and elution times, the amount of sorbent, and composition and volume of eluent were investigated thoroughly. The maximum sorption capacity of the imprinted polymer toward p-aminosalicylic acid was 70.9 mg/g, which is 4.5 times higher than that of the magnetic nonimprinted polymer. The magnetic molecularly imprinted polymernanoparticles were applied for the selective extraction of p-aminosalicylic acid from aqueous and urine samples and satisfactory results were achieved. The results illustrate that magnetic molecularly imprinted polymer nanoparticles have a great potential in the extraction of p-aminosalicylic acid from environmental and biological matrices.
      PubDate: 2016-10-06T01:45:55.746358-05:
      DOI: 10.1002/jssc.201600865
  • Facile preparation of polydopamine-coated imprinted polymers on the
           surface of SiO2 for estrone capture in milk samples

    • Authors: Penglei Zheng; Bilin Zhang, Zhimin Luo, Wei Du, Pengqi Guo, Yulan Zhou, Ruimiao Chang, Chun Chang, Qiang Fu
      Abstract: Estrone molecularly imprinted polymers were synthesized through the self-polymerization of dopamine on the surface of silica gels, which had the characteristics of mild polymerization conditions, simple reaction procedure and good specific recognition ability for estrone. The estrone molecularly imprinted polymers were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, thermogravimetric analysis, elemental analysis and nitrogen adsorption–desorption tests. The characterization confirmed that the imprinted polymers were successfully grafted on the surface of silica gels. Through investigating the adsorption performance, the prepared estrone molecularly imprinted polymers exhibited high adsorption capacity, fast mass transfer, as well as excellent selectivity towards estrone. The estrone molecularly imprinted polymers as the solid-phase extraction adsorbent coupled with high-performance liquid chromatography was developed to determine estrone from the milk samples. The developed estrone molecularly imprinted polymer solid-phase extraction with high-performance liquid chromatography method exhibited satisfactory specificity, precision, accuracy and good linearity relationship in the range of 0.2–20 μg/mL. The developed method is simple, fast, effective and high specificity method and it provides a new method to detect the residues of estrone in animal foods.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T23:51:07.154965-05:
      DOI: 10.1002/jssc.201600611
  • Comprehensive study of the macropore and mesopore size distributions in
           polymer monoliths using complementary physical characterization techniques
           and liquid chromatography

    • Authors: Sam Wouters; Tom Hauffman, Marjo C. Mittelmeijer-Hazeleger, Gadi Rothenberg, Gert Desmet, Gino V. Baron, Sebastiaan Eeltink
      Abstract: Poly(styrene-co-divinylbenzene) monolithic stationary phases with two different domain sizes were synthesized by a thermally initiated free-radical copolymerization in capillary columns. The morphology was investigated at the meso- and macroscopic level using complementary physical characterization techniques aiming at better understanding the effect of column structure on separation performance. Varying the porogenic solvent ratio yielded materials with a mode pore size of 200 nm and 1.5 μm, respectively. Subsequently, nano-liquid chromatography experiments were performed on 200 μm i.d. × 200 mm columns using unretained markers, linking structure inhomogeneity to eddy dispersion. Although small-domain-size monoliths feature a relatively narrow macropore-size distribution, their homogeneity is compromised by the presence of a small number of large macropores, which induces a significant eddy-dispersion contribution to band broadening. The small-domain size monolith also has a relatively steep mass-transfer term, compared to a monolith containing larger globules and macropores. Structural inhomogeneity was also studied at the mesoscopic level using gas-adsorption techniques combined with the non-local-density-function-theory. This model allows to accurately determine the mesopore properties in the dry state. The styrene-based monolith with small domain size has a distinctive trimodal mesopore distribution with pores of 5, 15 and 25 nm, whereas the monolith with larger feature sizes only contains mesopores around 5 nm in size.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T23:51:02.130205-05:
      DOI: 10.1002/jssc.201600896
  • Rapid and sensitive determination of major polyphenolic components in
           Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction

    • Authors: Atul S. Rathore; L. Sathiyanarayanan, Shreekant Deshpande, Kakasaheb R. Mahadik
      Abstract: A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. Ultra performance liquid chromatography-hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r2> 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T23:50:57.652477-05:
      DOI: 10.1002/jssc.201600685
  • Trace determination of organophosphate esters in environmental water
           samples with an ionogel-based nanoconfined ionic liquid fiber coating for
           solid-phase microextraction with gas chromatography and flame photometric

    • Authors: Long Pang; Rong Pang, Liming Ge, Liqing Zheng, Jihong Zhao, Hongzhong Zhang
      Abstract: Organophosphate esters, widely used as flame retardants and plasticizers, are regarded as a class of emerging pollutants. In this work, a novel approach was developed for the fabrication of a solid-phase microextraction fiber by using hybrid silica-based materials with immobilized ionic liquids with sol–gel technology, and the prepared solid-phase microextraction fiber was then coupled with gas chromatography and flame photometric detection for the analysis of six organophosphate esters. The high loading of 1-hexadecyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide was confined within the hybrid network. The developed solid-phase microextraction fiber possesses a coating thickness of ∼35 μm with good thermal stability and long lifetime. The parameters affecting the extraction efficiency such as extraction time, temperature, pH, and ionic strength of the sample solution were optimized. Under the optimized conditions, the limits of detection were in the range of 0.04−0.95 μg L−1, and the precision of the method assessed with repeatability and reproducibility of (RSD%) ˂13 and ˂29%, respectively. The proposed method was successfully applied to determine the six organophosphate esters in three real water samples, with recoveries in the range of 64.8−125.4% at two different spiking concentration levels. As a result, the proposed method demonstrated its potential for application in trace determination of organophosphate esters in actual water samples.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T23:50:47.528672-05:
      DOI: 10.1002/jssc.201600662
  • Analysis of proteins and peptides by electromigration methods in

    • Authors: Sille Štěpánová; Václav Kašička
      Abstract: This review presents the developments and applications of microchip electromigration methods in the separation and analysis of peptides and proteins in the period 2011–mid 2016. The developments in sample preparation and preconcentration, microchannel material and surface treatment are described. Separations by various microchip electromigration methods (zone electrophoresis in free and sieving media, affinity electrophoresis, isotachophoresis, isoelectric focusing, electrokinetic chromatography and electrochromatography) are demonstrated. Advances in detection methods are reported and novel applications in the areas of proteomics and peptidomics, quality control of peptide and protein pharmaceuticals, analysis of proteins and peptides in biomatrices, and determination of physicochemical parameters are shown.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T06:21:27.263184-05:
      DOI: 10.1002/jssc.201600962
  • Method Development for Separating Organic Carbonates by Ion-moderated
           high-performance liquid chromatography

    • Authors: Anuja Bhalkikar; Chris M. Marin, Chin Li Cheung
      Abstract: An ion-moderated partition high-performance liquid chromatography method was developed for the separation and identification of common organic carbonates. The separation of organic carbonates was achieved on an ion exclusion column with an exchangeable hydrogen ion. An isocratic, aqueous mobile phase was used for elution and detection was performed with a refractive index detector. The developed method was validated for specificity, linearity, limits of detection and quantification, precision and accuracy. All calibration curves showed excellent linear regression (R2> 0.9990) within the testing range. The limits of detection were 3.8–30.8 ppm for the analyzed carbonates. Improvements in the peak resolution of the chromatograms were achieved by decreasing the high-performance liquid chromatography column temperature. Addition of the organic modifier, acetonitrile, to the eluent was found to have insignificant effects on the peak resolution. The developed method was demonstrated for analyzing organic carbonate components in the electrolyte system of a commercial lithium ion battery.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-05T06:21:06.645786-05:
      DOI: 10.1002/jssc.201600743
  • Liquid chromatography with tandem mass spectrometry method for the
           simultaneous determination of multiple sweet mogrosides in the fruits of
           Siraitia grosvenorii and its marketed sweeteners

    • Authors: Zuliang Luo; Hongwu Shi, Kailun Zhang, Xijun Qin, Yuhua Guo, Xiaojun Ma
      Abstract: A high-performance liquid chromatography with electrospray ionization tandem mass spectrometry method has been developed and validated for the simultaneous quantification of eight major sweet mogrosides in different batches of the fruits of Siraitia grosvenorii and its marketed sweeteners. The sample preparation procedure and chromatographic and mass spectrographic conditions were optimized. Chromatographic separation was achieved on a reversed-phase Poroshell 120 SB C18 column in 10.0 min with gradient elution with acetonitrile and water, both of which contained 0.1% formic acid. The multiple reaction monitoring scanning mode was employed for quantification in the negative ion mode. The developed method was validated with acceptable linearity (r2 = 0.9984–0.9998) over a wide concentration range, precision (relative standard deviations = 1.09–3.91%), stability (relative standard deviations = 1.21–3.01%), and recovery in the range of 91.22–106.58% (relative standard deviations ≤ 3.79%) under optimum conditions. The proposed method was demonstrated to be simple, rapid, specific, and reliable and was successfully applied for the quality control of the fruits of S. grosvenorii and its marketed sweeteners.
      PubDate: 2016-10-05T04:35:54.240399-05:
      DOI: 10.1002/jssc.201600563
  • Evaluation of a new carbon/zirconia-based sorbent for the cleanup of food
           extracts in multiclass analysis of pesticides and environmental

    • Authors: Lijun Han; Yelena Sapozhnikova, Jessie Matarrita
      Abstract: A novel carbon/zirconia-based material, SupelTM QuE Verde, was evaluated in a filter-vial dispersive solid-phase extraction cleanup of pork, salmon, kale, and avocado extracts for the residual analysis of 65 pesticides and 52 environmental contaminants (flame retardants, polychlorinated biphenyls, polybrominated diphenyl ethers and polycyclic aromatic hydrocarbons) using low-pressure gas chromatography with tandem mass spectrometry. An amount of 180 mg sorbent per 0.6 mL extract in filter-vial dispersive solid-phase extraction cleanup was found the optimum in terms of achieving satisfactory removal of co-extractives and recoveries of analytes, especially for structurally planar compounds. For analytes partially retained by Verde, normalization to an internal standard resulted in 62–107% recoveries. Addition of Verde to primary secondary amine and C18 in cleanup resulted in 38% more removal of gas-chromatography-amenable co-extractives in avocado, 30% in kale, 39% in salmon, and 50% in pork. The removal efficiency of co-extracted chlorophyll was 93% for kale and 64% for avocado based on ultraviolet-visible absorbance. The developed method was validated at three spiking levels (10, 25, and 100 ng/g), and 70–120% recoveries with ≤20% relative standard deviation were achieved for 96 (83%) out of 117 analytes in pork, 79 (69%) in salmon, 71 (62%) in kale, and 75 (65%) in avocado.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-04T22:20:47.758622-05:
      DOI: 10.1002/jssc.201600920
  • Gadolinium oxide: Exclusive selectivity and sensitivity in the enrichment
           of phosphorylated biomolecules

    • Authors: Fahmida Jabeen; Muhammad Najam-ul-Haq, Muhammad Naeem Ashiq, Matthias Rainer, Christian W. Huck, Guenther K. Bonn
      Abstract: Selectivity and sensitivity define the dynamic applicability of separation and enrichment techniques. Owing to proteome complexity, numbers of separation media have been introduced in phosphoproteomics. Complex samples are pretreated to make the low-abundance molecules detectable by mass spectrometry. Gadolinium oxide nanoparticles, offering mono- and bi-dentate interactions, are optimized to capture the phosphopeptides. Selectivity of 1:11 000 is achieved for digested β-casein phosphopeptides in bovine serum albumin digest background using gadolinium oxide nanoparticles. The limit of detection goes down to 1 attomole. With the optimized sample preparation protocol, gadolinium oxide nanoparticles enrich phosphopeptides of κ-casein (Ser148 and Ser170) from digested milk sample, fibrinogen alpha chain phosphopeptide (Ser609) along with four hydrolytic products of Ser22-modified phosphopeptides from serum.
      PubDate: 2016-10-04T06:56:54.554335-05:
      DOI: 10.1002/jssc.201600651
  • Development of an online solid-phase extraction with liquid chromatography
           method based on polymer monoliths for the determination of dopamine

    • Authors: Simona Janků; Martina Komendová, Jiří Urban
      Abstract: Porous polymer monoliths have been used to develop an online solid-phase extraction with liquid chromatography method for determination of dopamine in urine as well as for a continuous monitoring of dopamine in flowing system. A polymerization mixture containing 4-vinylphenylboronic acid monomer has been used to prepare a trapping column based on specific ring formation reaction with dopamine cis-diol functionality. Additionally, a monolithic stationary phase with zwitterion functionality has been used to prepare capillary column for the separation of dopamine.Experimental conditions including molarity, pH, and flow rate of the loading buffer together with a valve switching time have been optimized to provide the highest recovery for dopamine. Experimental setup has been used to determine dopamine in a urine. By using both calibration curve and standard addition method, the dopamine level was determined to be 1.19 and 1.28 mg/L, respectively.Further, we have used experimental design to optimize coupling of two extraction monolithic loops to separation capillary column with monolithic phase for a comprehensive monitoring of dopamine. After multivariate analysis, sample loading flow-rate and a flow-rate of flushing buffer were selected as the most significant variables. Optimized experimental setup was applied to continuously monitor dopamine degradation.
      PubDate: 2016-10-04T06:21:35.482661-05:
      DOI: 10.1002/jssc.201600818
  • Recent progress of chiral stationary phases for separation of enantiomers
           in gas chromatography

    • Authors: Sheng-Ming Xie; Li-Ming Yuan
      Abstract: Chromatography techniques based on chiral stationary phases are widely used for the separation of enantiomers. In particular, gas chromatography has developed rapidly in recent years due to its merits such as fast analysis speed, lower consumption of stationary phases and analytes, higher column efficiency, making it a better choice for chiral separation in diverse industries. This article summarizes recent progress of novel chiral stationary phases based on cyclofructan derivatives and chiral porous materials including chiral metal–organic frameworks, chiral porous organic frameworks, chiral inorganic mesoporous materials, and chiral porous organic cages in gas chromatography, covering original research papers published since 2010. The chiral recognition properties and mechanisms of separation toward enantiomers are also introduced.
      PubDate: 2016-10-04T06:21:18.570848-05:
      DOI: 10.1002/jssc.201600808
  • Fluid manipulation on the micro-scale: Basics of fluid behavior in

    • Authors: Jakub Novotný; František Foret
      Abstract: Fluid manipulation on the micro-scale (microfluidics) is bringing new potential applications in a number of fields, including, chemistry, biology and medicine. At sub-millimeter channel scale, some phenomena, unimportant at the macroscale, become an important force to consider when designing a microfluidics system. For example, the decrease in fluid mass causes the effects of viscosity to overcome the influence of inertia. Turbulent flow cannot be achieved at any realistic fluid velocity, making mixing a challenging task. The only phenomenon capable of blending liquids at microscale is diffusion and liquid streams can be flowed side-by-side for tens of minutes before they completely fuse together. The decrease in the channel size also leads to an increased surface-to-volume ratio, which increases the importance of surface effects, including adsorption, capillary action and surface wetting and/or electric double layer formation with related electrokinetic phenomena. While rivers cannot flow uphill, a stream of liquid can easily flow up against gravity inside a capillary. Similarly, the formation of electric double layer near the charged surface of a micro-channel or capillary can be applied for electrokinetic actuating. This review summarizes selected physical phenomena related to liquid based (water solutions) microfluidics as described in recent research.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-04T01:32:48.534166-05:
      DOI: 10.1002/jssc.201600905
  • Glass slides functionalized by 1-carboxyethyl-3-methylimidazolium chloride
           for the determination of triazine herbicides in rice using
           high-performance liquid chromatography

    • Authors: Xinpei Li; Shigang Wei, Ying Sun, Qun Sun, Li Liang, Zhang Bo, Huilan Piao, Daqian Song, Xinghua Wang
      Abstract: A novel and simple supported ionic-liquid-based solid-phase extraction method for the determination of triazine herbicides in rice was developed in this work. Glass slides were functionalized by an ionic liquid, 1-carboxyethyl-3-methylimidazolium chloride, and were used for the simultaneous extraction of seven triazine herbicides in rice samples. The effects of the type of extraction solvent, the extraction time, the type and volume of loading solvent, and the type of eluting solvent on the extraction efficiency were investigated and optimized. Under the optimum operation conditions, the limits of detection for seven triazine herbicides in rice samples obtained by high performance liquid chromatography were 3.16–5.42 ng g−1, which were lower than the maximum residue levels established by various organizations. The linear correlation coefficients were higher than 0.9975 in the concentration range of 0.015–1.08 μg g−1 for seven triazine herbicides. The recoveries of seven triazine herbicides at the two concentration levels of 0.15 and 0.45 μg g−1 are between 82.47 and 104.21%, with relative standard deviations of 0.69–9.19%. The intra- and inter-day (n = 5) precisions for all triazine herbicides at the spiked level of 0.30 μg g−1 were 1.72–11.71%.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-03T05:25:37.12846-05:0
      DOI: 10.1002/jssc.201600861
  • Development and validation of a capillary electrophoresis method for the
           characterization of sulfoethyl cellulose

    • Authors: Henrik Harnisch; Jens Hühner, Christian Neusüß, Andreas Koschella, Thomas Heinze, Gerhard K. E. Scriba
      Abstract: To characterize sulfoethyl cellulose samples, a capillary electrophoresis method was developed and validated. Sulfoethyl cellulose was hydrolyzed, and the resulting d-glucose derivatives were analyzed after reductive amination with 4-aminobenzoic acid using 150 mM boric acid, pH 9.5, as background electrolyte at 20°C and a voltage of 28 kV. Peak identification was derived from capillary electrophoresis with mass spectrometry using 25 mM ammonia adjusted to pH 6.2 by acetic acid as electrolyte. Besides mono-, di- and tri-sulfoethyl-d-glucose, small amounts of disaccharides could be identified resulting from incomplete hydrolysis. The linearity of the borate buffer-based capillary electrophoresis method was evaluated using d-glucose in the concentration range of 3.9–97.5 μg/mL, while limits of detection and quantification derived from the signal-to-noise ratio of 3 and 10 were 0.4 ± 0.1 and 1.2 ± 0.3 μg/mL, respectively. Reproducibility and intermediate precision were determined using a hydrolyzed sulfoethyl cellulose sample and ranged between 0.2 and 8.8% for migration times and between 0.3 and 10.4% for peak area. The method was applied to the analysis of the degree of substitution of synthetic sulfoethyl cellulose samples obtained by variation of the synthetic process and compared to data obtained by elemental analysis.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-03T02:55:37.618196-05:
      DOI: 10.1002/jssc.201600687
  • Investigation of multivalent interactions between conjugate of quantum
           dots with c-Myc peptide tag and the anti-c-Myc antibody by capillary
           electrophoresis with fluorescence detection

    • Authors: Jianhao Wang; Li Yang, Li Liu, Hao Wu, Jianpeng Wang, Pengju Jiang, Xiyuan Jiang, Lin Qiu
      Abstract: Herein, we report an assay for detecting the binding of a multivalent peptide and antibody within a capillary with the use of fluorescence coupled capillary electrophoresis. Quantum dots and a c-Myc tag containing peptide EQKLISEEDLG4H6 were injected sequentially and formed a multivalent quantum dot-EQKLISEEDLG4H6 assembly within the capillary. The efficiency of the quantum dot-peptide self-assembly was affected by the peptide/quantum dot molar ratio, sampling time, and interval time. Finally, the binding of the monoclonal anti-c-Myc antibody and the multivalent quantum dot-EQKLISEEDLG4H6 ligand was studied using an in-capillary assay. The microscopic dissociation constant for the self-assembly of monoclonal anti-c-Myc antibody and quantum dot-EQKLISEEDLG4H6 was determined to be 14.1 μM with a stoichiometry of the peptide-antibody complex of 1.7 determined after fitting this to the Hill equation. This method can be further extended in order to detect a wide range of biomolecule–biomolecule binding interactions.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-03T02:50:33.971153-05:
      DOI: 10.1002/jssc.201600931
  • Solid-phase microextraction of ultra-trace amounts of tramadol from human
           urine by using a carbon nanotube/flower shaped zinc oxide hollow fiber

    • Authors: Maryam Abbasian; Mahdi Balali-Mood, Sayeed Ahmad Mozaffari, Hossein Salar Amoli
      Abstract: A new method is successfully developed for the separation and determination of a very low amount of tramadol in urine using functionalized multiwalled carbon nanotubes/flower shaped zinc oxide before solid-phase microextraction combined with gas chromatography. Under ultrasonic agitation, a sol of multi-walled carbon nanotubes and flower shaped zinc oxide were forced into and trapped within the pore structure of the polypropylene and the sol solution immobilized into the hollow fiber. Flower shaped zinc oxide was synthesized and characterized by Fourier transform infrared spectroscopy. The morphology of the surface of fabricated solid-phase microextraction was investigated by scanning electron microscopy and X-ray diffraction. The parameters affecting the extraction efficiencies were investigated and optimized. Under the optimized conditions, the method shows linearity in a wide range of 0.12 to 7680 ng mL−1, and a low detection limit (S/N = 3) of 0.03 ng mL−1. The precision of the method was determined and a relative standard deviation of 3.87% was obtained. This method was successfully applied for the separation and determination of tramadol in urine samples. The relative recovery percentage obtained for the spiked urine sample at 1000 ng mL−1 was 94.2%.This article is protected by copyright. All rights reserved
      PubDate: 2016-10-02T23:20:34.920731-05:
      DOI: 10.1002/jssc.201600729
  • Supercritical fluid chromatography for lipid analysis in foodstuffs

    • Authors: Paola Donato; Veronica Inferrera, Danilo Sciarrone, Luigi Mondello
      Abstract: The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes.This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO2, to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions.A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-30T21:51:01.340415-05:
      DOI: 10.1002/jssc.201600936
  • Screening of lipase inhibitors in folium mori with lipase-linked magnetic
           microspheres by high-performance liquid chromatography and evaluation in
           diabetic mice

    • Authors: Rui Ma; Hongbo Weng, Jianying Liang
      Abstract: A new method for the screening of compounds with hypoglycemic effect from traditional Chinese medicines employing high-performance liquid chromatography and lipase-linked magnetic microspheres has been proposed. We hypothesized that the interaction of traditional Chinese medicine extracts with lipase-linked magnetic microspheres should decrease the concentration of compounds with hypoglycemic effect. Using this approach, the potential lipase inhibitors in Folium Mori extract were found out. Firstly, lipase was immobilized on magnetic microspheres by chemical method. Then, by comparing the chromatograms of samples before and after the interaction with lipase-linked magnetic microspheres, seven compounds of Folium Mori extract were identified. It was found that protocatechuic acid, chlorogenic acid, protocatechualdehyde, rutin, isoquercitrin, astragalin and dicaffeoylquinic acid B had evident combination with lipase-linked magnetic microspheres. Their hypoglycemic effects were verified in streptozocin-induced diabetic mice. In the present study, astragalin was verified to improve the glucose tolerance and low the level of glucose in streptozocin-induced diabetic mice, which indicated the astragalin might be a new high efficient lipase inhibitor. Based on the significant results, this method could be a convenient approach to screen the potential lipase inhibitors from traditional Chinese medicines. Meanwhile it also could be expanded to screen out other active compounds in traditional Chinese medicines.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-30T04:50:43.611111-05:
      DOI: 10.1002/jssc.201600924
  • Rapid and efficient enantioseparation of (S)-amlodipine by
           surface-imprinted core–shell polymer microspheres

    • Authors: Shenzhi Lai; Chunyan Chen, Xiaoli Ouyang, Yanru Qin, Changqun Cai, Xiaoming Chen
      Abstract: We present a protocol for the preparation of surface-imprinted polymer microspheres by core–shell precipitation polymerization for the enantioseparation of (S)-amlodipine. In this work, submicron mesoporous silica microspheres were prepared with gemini cationic surfactant as soft template. Molecularly imprinted polymers were coated on the silica supports with a low level of crosslinking, and the thickness of the thin-walled imprinted shell was about 45 nm. The material showed fast binding kinetics for (S)-amlodipine (within only 20 min for complete equilibrium), and the saturation adsorption capacity reached 309.2 mg/g, indicating the good accessibility of binding sites and improved mass transfer for target molecule. The imprinted microspheres exhibited an appreciable enantiomeric excess of (S)-amlodipine of 11.3% when used as glass chromatography column for the enantioseparation of (S)-amlodipine from amlodipine besylate without extra chiral additives. The surface-imprinted materials display potentially amplification for industrial enantioseparation of (S)-amlodipine.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-28T08:35:56.415521-05:
      DOI: 10.1002/jssc.201600850
  • Sensitive determination of pyrrolizidine alkaloids in Tussilago farfara L.
           by field-amplified, sample-stacking, sweeping micellar electrokinetic

    • Authors: Kun Cao; Yi Xu, Xiuni Mu, Qing Zhang, Renjie Wang, Junjiang Lv, Zixuan Liu
      Abstract: Pyrrolizidine alkaloids are the toxic components in Tussilago farfara L. Due to the lack of standard substances for quantitative analysis and traces of pyrrolizidine alkaloids in total alkaloids, the full quality control of Tussilago farfara L has been limited. In this study we aimed to solve the difficulty of determination of pyrrolizidine alkaloids and identify more components in the total alkaloids. An on-line pre-concentration method has been applied to improve determining sensitivity of pyrrolizidine alkaloids in Tussilago farfara L. in which included field-amplified sample stacking and sweeping in micellar electrokinetic capillary chromatography. The main parameters that affected separation and stacking efficiency were investigated in details. Under the optimal conditions, the sensitivity enhancement factors obtained by the developed method for the analytes were from 15- to 12-fold, the limits of detection of senkirkine and senecionine were 2∼5 μg·L−1. Senkirkine and senecionine have been detected in alkaloids (c) of Tussilago farfara L, along ferulic acid methyl ester and methyl caffeate. The developed method was also applied to the analysis of acid extraction (a) of Tussilago farfara L, and senkirkine could be detected directly. The results indicated that the developed method is feasible for the analysis of pyrrolizidine alkaloids in Tussilago farfara L with good recoveries.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-27T10:37:09.807557-05:
      DOI: 10.1002/jssc.201600762
  • Simultaneous quantification of triterpenoid saponins in rat plasma by
           UHPLC–MS/MS and its application to a pharmacokinetic study after oral
           total saponin of Aralia elata leaves

    • Authors: Yichun Sun; Juan Xue, Baimei Li, Xiaoting Lin, Zhibin Wang, Hai Jiang, Hongwei Zhang, Qiuhong Wang, Haixue Kuang
      Abstract: A rapid, sensitive, and reliable analytical ultra performance liquid chromatography with tandem mass spectrometry method was developed for the simultaneous determination of Aralia-saponin IV, 3-O-β-d-glucopyranosyl-(13)-β-d-glucopyranosyl-(13)-β-d-glucopyranosyl oleanolic acid 28-O-β-d-glucopyranoside, Aralia-saponin A and Aralia-saponin B after the oral administration of total saponin of Aralia elata leaves in rat plasma. Plasma samples were pretreated by protein precipitation with methanol. The analysis was performed on an ACQUITY UPLC HSS T3 column. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode using an electrospray ionization source with negative ionization mode. Under the experimental conditions, the calibration curves of four analytes had good linearity values (r> 0.991). The intra- and inter-day precision values of the four analytes were ≤ 11.6%, and the accuracy was between –6.2 and 4.2%.The extraction recoveries of four triterpenoid saponins were in the range of 84.06–91.66% (RSD < 10.5%), and all values of the matrix effect were more than 90.30%. The developed analytical method was successfully applied to pharmacokinetic study on simultaneous determination of the four triterpenoid saponins in rat plasma after oral administration of total saponin of Aralia elata leaves, which helps guiding clinical usage of Aralia elata leaves.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-27T05:22:12.869407-05:
      DOI: 10.1002/jssc.201600801
  • Effervescence-assisted dispersive solid-phase extraction using
           ionic-liquid-modified magnetic β-cyclodextrin/attapulgite coupled with
           high-performance liquid chromatography for fungicide detection in honey
           and juice

    • Authors: Xiaoling Wu; Miyi Yang, Haozhe Zeng, Xuefei Xi, Sanbing Zhang, Runhua Lu, Haixiang Gao, Wenfeng Zhou
      Abstract: In this study, a simple effervescence-assisted dispersive solid-phase extraction method was developed to detect fungicides in honey and juice. Most significantly, an innovative ionic-liquid-modified magnetic β-cyclodextrin/attapulgite sorbent was used because its large specific surface area enhanced the extraction capacity and also led to facile separation. A one-factor-at-a-time approach and orthogonal design were employed to optimize the experimental parameters. Under the optimized conditions, the entire extraction procedure was completed within 3 min. In addition, the calibration curves exhibited good linearity, and high enrichment factors were achieved for pure water and honey samples. For the honey samples, the extraction efficiencies for the target fungicides ranged from 77.0 to 94.3% with relative standard deviations of 2.3–5.44%. The detection and quantitation limits were in the ranges of 0.07–0.38 and 0.23–1.27 μg·L−1, respectively. Finally, the developed technique was successfully applied to real samples, and satisfactory results were achieved. This analytical technique is cost-effective, environmentally friendly, and time-saving.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-27T03:52:07.751692-05:
      DOI: 10.1002/jssc.201600596
  • Spiral counter-current chromatography: Design, development, application,
           and challenges

    • Authors: Xin-Yi Huang; Xiao-Ming Sun, Dong Pei, Duo-Long Di
      Abstract: Depending on the rapid growth in the radial gradient of the centrifugal force, spiral counter-current chromatography can greatly improve the retention of stationary phase, especially for the aqueous two-phase systems with ultra-polar and high viscosity that are not well retained in the conventional multilayer coils counter-current chromatography. As a result, it is an attractive and alternative technology that is suited for separation of hydrophilic compounds and has led to many exciting progress in recent years. This review presents the recent advances and applications of spiral counter-current chromatography, including its major benefits and limitations, some novel methods to improve the separation efficiency and its applications in separation of real samples. In addition, the remaining challenges and future perspectives on development of spiral counter-current chromatography also are proposed in this article.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-26T03:15:27.209472-05:
      DOI: 10.1002/jssc.201600927
  • Manipulating adenoviral vector ion-exchange chromatography: Hexon versus

    • Authors: Jelena Ruščić; Andreja Ambriović-Ristov, Dragomira Majhen, Sandra Kolundžija, Miloš Barut, Karim Benihoud, Mladen Krajačić
      Abstract: The serotype specificity of adenovirus ion-exchange chromatography has previously been studied using standard particle-based columns, and the hexon protein has been reported to determine retention time. In this study, we have submitted Adenovirus type 5 recombinants to anion-exchange chromatography using methacrylate monolithic supports. Our experiments with hexon-modified adenoviral vectors show more precisely that the retention time is affected by the substitution of amino acids in hypervariable region 5, which lies within the hexon DE1 loop. By exploring the recombinants modified in the fiber protein, we have proven the previously predicted chromatographic potential of this surface constituent. Modifications that preserve the net charge of the hexon protein, or those that cause only a small charge difference in the fiber protein, in addition to shortening the fiber shaft, did not change the chromatographic behavior of the adenovirus particles. However, modifications that include the deletion of just two negatively charged amino acids in the hexon protein, or the introduction of a heterologous fiber protein, derived from another serotype, revealed recognizable changes in anion-exchange chromatography. This could be useful in facilitating chromatography-approach purification by creating targeted capsid modifications, thereby shifting adenovirus particles away from particular interfering substances present in the crude lysate.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-23T07:55:21.282975-05:
      DOI: 10.1002/jssc.201600829
  • Bioassay-guided isolation of an active compound with Protein Tyrosine
           Phosphatase 1B Inhibitory Activity from Sargassum fusiforme by high-speed
           counter-current chromatography

    • Authors: Miao Wang; Dongyu Gu, Xinfeng Guo, Haoquan Li, Yi Wang, Hong Guo, Yi Yang, Jing Tian
      Abstract: A rapid and efficient method using high-speed counter-current chromatography was established for the bioassay-guided separation of an active compound with protein tyrosine phosphatase 1B inhibitory activity from Sargassum fusiforme. Under the bioassay guidance, the ethyl acetate extract with the best IC50 value of 0.37±0.07 μg/mL exhibited a potential protein tyrosine phosphatase 1B inhibitory activity, which was further separated by high-speed counter-current chromatography. The separation was performed with a two-phase solvent system composed of n-hexane/methanol/water (5:4:1, v/v). As a result, dibutyl phthalate (19.7 mg) with the purity of 97.3% was obtained from 200 mg of the ethyl acetate extract. Its IC50 was 14.05±0.06 μM, which was further explained by molecular docking. The result of molecular docking showed that dibutyl phthalate enfolded in the catalytic site of protein tyrosine phosphatase 1B. The main force between dibutyl phthalate and protein tyrosine phosphatase 1B was the hydrogen bond interacted with Gln266. In addition, hydrogen bond, van der Waals force and hydrophobic interacted with the amino acids (Ala217, Ile219, and Gly220) were also responsible for the stable protein-ligand complex.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-23T03:50:21.838803-05:
      DOI: 10.1002/jssc.201600691
  • Development of a novel stirrer-liquid/solid microextraction method for the
           separation and enrichment of trace levels of active compounds in
           traditional Chinese medicine

    • Authors: Caiyun Wang; Xuan Chen, Shuang Hu, Xiaohong Bai
      Abstract: In this paper, a novel stirrer-liquid/solid microextraction method was developed and introduced for the separation and enrichment of trace levels of curcumin, bisdemethoxycurcumin and demethoxycurcumin in Rhizoma Curcumae Longae, Radix Curcumae and Rhizoma Curcumae before their analysis by high-performance liquid chromatography with ultraviolet detection. In the proposed approach, a magnetic stirrer was immersed in decanol to coat its surface completely with decanol, which was used as an extraction platform. The stirrer coated with decanol is not only able to agitate the sample solution to constantly update the sample on the stirrer surface but also it can adsorb and extract the target analytes. Some effective parameters, including suitable superficial area of stirrer, extraction solvent, sample phase pH, NaCl concentration, stirring rate, extraction time, sample phase volume, were analyzed and selected. Under the optimal conditions, the linearities are 0.0044–2.20 μg/mL, detection limits are 0.3–0.6 ng/mL, and the extraction content per unit length and enrichment factors of the target analytes are 6.24–9.71 mm−1 and 589–917, respectively. Also, the stirrer-liquid/solid microextraction mechanism for the extraction and enrichment of the target analytes was analyzed and expounded. The results showed that stirrer-liquid/solid microextraction is a simple, rapid sample pretreatment approach with a high enrichment factor.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-23T01:55:58.046751-05:
      DOI: 10.1002/jssc.201600605
  • Screening and identifying antioxidants from Oplopanax elatus using
           2,2ʹ-diphenyl-1-picrylhydrazyl with off-line two-dimensional HPLC coupled
           with diode array detection and tandem time-of-flight mass spectrometry

    • Authors: Li Shao; Ming-Kun Nie, Man-Yun Chen, Jing Wang, Chong-Zhi Wang, Wei-Hua Huang, Chun-Su Yuan, Hong-Hao Zhou
      Abstract: The root of Oplopanax elatus (Nakai) Nakai has a well-known history of use for the treatment of diseases such as neurasthenia, cardiovascular disorders and cancer by the native people in northeast China. It is important to screen and identify the bioactive molecules from its root rapidly. Hereby, an off-line two-dimensional high performance liquid chromatography coupled with diode array detection and tandem time-of-flight mass spectrometry together with 2,2ʹ-diphenyl-1-picrylhydrazyl was established to screen antioxidants from the root of O. elatus. A Waters cyanogen column (150 × 3.9 mm, i.d., 4 μm) was used for the first dimensional liquid chromatography, while a Hypersil BDS-C18 column (250 × 4.6 mm, i.d., 5 μm) was installed for the second dimension liquid chromatographic analysis. Twenty-eight compounds had been tentatively identified from the methanol extract of the air-dried root of O. elatus including six polyynes, and eight phenolic derivatives screened with antioxidant activity. The developed method could be expedient for screening and identifying antioxidants from O. elatus.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-14T04:40:47.375276-05:
      DOI: 10.1002/jssc.201600838
  • Preparation of chiral oxazolinyl-functionalized β-cyclodextrin-bonded
           stationary phases and their enantioseparation performance in
           high-performance liquid chromatography

    • Authors: Lan Li; Man Zhang, Yuting Wang, Wenhong Zhou, Zhiming Zhou
      Abstract: A simple procedure for the synthesis of three new oxazolinyl-substituted β-cyclodextrins (6-deoxy-6-R-(–)-4-phenyl-4,5-dihydrooxazolinyl-β-cyclodextrin, 6-deoxy-6-S-(–)-4-phenyl-4,5-dihydrooxazolinyl-β-cyclodextrin, and 6-deoxy-6-S-(–)-(4-pyridin-1-ium-4-methyl-benzenesulphonate)-4,5-dihy-drooxazolinyl-β-cyclodextrin) and their covalent bonding to silica are reported. The ability of these chiral stationary phase columns for separating compounds is also presented and discussed. Twenty-eight compounds were examined in the polar-organic mobile phase mode, and 11 β-nitroethanols were tested in the reversed-phase mode. Excellent enantioseparations were achieved for most of the analytes, even for several challenging compounds. The rigid and flexible structures of mono-substituted chiral groups and the fragments around the rim of the β-cyclodextrin cavity played an important role in the separation process. Factors such as π–π stacking, dipole–dipole interactions, ion-pairing, and steric hindrance effects were found to affect the chromatographic performance. Moreover, the buffer composition, and percentages of organic modifiers in the mobile phase, were investigated and compared. The mechanisms involved in the separation were postulated based on the chromatographic data.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-09T02:21:27.685612-05:
      DOI: 10.1002/jssc.201600609
  • Application of multi-walled carbon nanotubes for the preconcentration and
           determination of organochlorine pesticides in water samples by gas
           chromatography with mass spectrometry

    • Authors: Abdollah Taghani; Naaser Goudarzi, Ghadamali Bagherian
      Abstract: A fast, sensitive, and convenient technique consisting of a miniaturized solid-phase extraction method named microextraction in packed syringe coupled with gas chromatography and mass spectrometry was developed for the preconcentration and determination of some pesticides, including hexachlorobenzene, heptachlor, alachlor, aldrine, and metolachlore, in natural water samples. Carboxyl-purified multi-walled carbon nanotubes were used as a sorbent in microextraction in packed syringe. Based on this technique, 6.0 mg of multi-walled carbon nanotubes was inserted in the syringe between two polypropylene frits. The analytes would be adsorbed on the solid phase, and would subsequently be eluted using organic solvents. The influence of some important parameters involved including the solution pH, type and volume of the organic desorption solvent, and amount of the multi-walled carbon nanotubes sorbent on the extraction efficiency of the selected pesticides were investigated. The proposed method showed a good linearity in the range of 0.1–25.0 ng mL‒1 and low limits of detection in the range of 0.02–0.19 ng mL‒1 using the selected ion-monitoring mode. Reproducibility of the method was in the range of 3.3–8.5% for the studied pesticides. Also to evaluate the matrix effect, the developed method was applied to the preconcentration and determination of the selected pesticides in different water samples.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-08T03:50:21.278429-05:
      DOI: 10.1002/jssc.201600555
  • Multi-class method for the quantification 92 veterinary anti-microbial
           drugs in livestock excreta, wastewater, and surface water by liquid
           chromatography with tandem mass spectrometry

    • Authors: Jinfang Gao; Yonghui Cui, Yanfei Tao, Lingli Huang, Dapeng Peng, Shuyu Xie, Xu wang, Zhenli Liu, Dongmei Chen, Zonghui Yuan
      Abstract: A simple multi-residue method was developed for detecting and quantifying 92 veterinary anti-microbial drugs from eight classes (β-lactams, quinolones, sulfonamides, tetracyclines, lincomycins, macrolides, chloramphenicols, and pleuromutilin) in livestock excreta and water by liquid chromatography with tandem mass spectrometry. The feces samples were extracted by ultrasound-assisted extraction with a mixture of acetonitrile/water (80:20, v/v) and edetate disodium, followed by a clean-up using solid-phase extraction with amino cartridge. Water samples were purified with hydrophilic-lipophilic balance solid-phase extraction column. Urine samples were extracted with acetonitrile and edetate disodium. Detection of veterinary anti-microbial drugs was achieved by liquid chromatography with tandem mass spectrometry using both positive and negative electrospray ionization mode. The recovery of veterinary anti-microbial drugs in feces, urine and water samples were 75–99, 85–110, and 85–101% and associated relative standard deviations were less than 15, 10, and 8% respectively. The limits of quantification in feces, urine, and water samples were 0.5–1, 0.5–1, and 0.01–0.05 μg/L, respectively. This method was applied to determine real samples obtained from local farms, and provides reliable quantification and identification results of 92 veterinary anti-microbial drugs in livestock excreta and water.This article is protected by copyright. All rights reserved
      PubDate: 2016-09-04T23:50:51.507179-05:
      DOI: 10.1002/jssc.201600531
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