JournalTOCs

Journal of Chromatographic Science
Journal Prestige (SJR): 0.36

Citation Impact (citeScore): 1
Number of Followers: 15

Hybrid journal (It can contain Open Access articles)
ISSN (Print) 0021-9665 - ISSN (Online) 1945-239X
Published by Oxford University Press

[419 journals]

Determination of Phthalates in Marine Sediments Using Ultrasonic
Extraction Followed by Dispersive Solid-Phase Extraction and Gas
Chromatography–Mass Spectrometry
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  Authors: Hu H; Li T, Bao J, et al.
  Pages: 207 - 216
  Abstract: AbstractA simple, rapid and novel method has been developed and validated for determination of 16 phthalates in marine sediment samples by gas chromatography coupled to mass spectrometry. Freeze dried samples were first ultrasonic extraction by n-hexane:methylene chloride (1:1, v/v) and n-hexane:ethyl acetate (1:1, v/v) and followed by dispersive solid-phase extraction cleanup. The linearity of this method ranged from 1 to 1,000 μg/L, with regression coefficients ranging between 0.9993 and 0.9999. The limits of detection were in ng/g level, ranging between 0.1 and 0.25 ng/g (dry weight). The concentration of the total phthalates in marine sediment samples from Waters of Dongji (Zhoushan, China), Yueqing Bay (Wenzhou, China) and Coastal Waters of Yuhuan (Taizhou, China) ranged from 235.4 to 608.7 μg/kg with diisobutyl phthalate, dibutyl phthalate and di(2-ethylhexyl) phthalate being the major species, which constitutes of 94.6 and 98.1% of the total phthalates. The recoveries of spiked 16 phthalates at different concentration levels in sediment sample 3 of Waters of Dongji (Zhoushan, China) and sediment sample 3 of Yueqing bay (Wenzhou, China) were in the range of 78–117% and 83–114%, respectively, with relative standard deviations of 2.4–6.8% and 3.4–7.5% (n = 5), respectively. The performance of the proposed method was also compared with traditional Soxhlet extraction and column chromatography cleanup on the same genuine sediment samples and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of phthalates in different marine sediment samples.
  PubDate: Tue, 22 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab080
  Issue No: Vol. 60, No. 3 (2021)
Application of ICH Guidelines for Studying the Degradation Behavior of
Rocuronium Bromide Coupled with Stability-Indicating RP-LC Method
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  Authors: El Houssini O; Abd El-Rahman M, Fahem D, et al.
  Pages: 217 - 223
  Abstract: AbstractNon-depolarizing neuromuscular blocking agent Rocuronium bromide was quantified in drug substance and drug product using reversed-phase liquid chromatographic method. Forced degradation studies were conducted for Rocuronium bromide in drug substance under acidic (2MHCl), basic (2MNaOH), oxidative (3% H2O2), thermal (135°C) and photolytic (254 nm) stress conditions. An Agilent H12 C18 column was used for separation using diammonium hydrogen phosphate buffer (pH 8; 0.04M)- acetonitrile (50:50; v/v) as mobile phase at flow rate of 1 mL/min. The quantification was done using UV detection at 210 nm. The limit of quantification and detection was 11.1 and 3.66 μg/mL, respectively, and the recovery percentage was 99% in drug substance and drug product. ICH guidelines were adopted for method validation. The proposed LC method monitored the degradation profile for Rocuronium bromide under various stress conditions and provided a specific LC method for its routine analysis. Besides, the MS data were used to identify all Rocuronium bromide degradation products and the possible degradation pathway was designated.
  PubDate: Sat, 12 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab065
  Issue No: Vol. 60, No. 3 (2021)
Simultaneous Determination of Iridoid Glycosides, Phenylpropanoid
Glycosides, Organic Acids, Nucleosides and Amino Acids in Scrophulariae
Radix Processed by Different Processing Methods by HPLC-QTRAP-MS/MS
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  Authors: Wang S; Wang Q, Yin X, et al.
  Pages: 232 - 242
  Abstract: AbstractScrophulariae Radix is one of the widely used traditional Chinese medicines. In this study, a high-performance liquid chromatography coupled with triple quadrupole-linear ion trap mass spectrometry method was established for the simultaneous determination of multiple bioactive constituents including four iridoid glycosides, two phenylpropanoid glycosides, six organic acids, 11 nucleosides and 16 amino acids in Scrophulariae Radix. The validated method was used to analyze nine Scrophulariae Radix samples processed by different processing methods. In addition, Grey relational analysis and DTOPSIS were used to evaluate the samples according to the content of 39 ayalytes. The results showed that the quality of Scrophulariae Radix processed by cutting into slices, sun drying and “sweating” methods were better. All the results proved that the developed method was available and could be used to evaluate the quality of Scrophulariae Radix.
  PubDate: Tue, 08 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab056
  Issue No: Vol. 60, No. 3 (2021)
Preparation and application of
3-(methylene-bis(1′,4′-phenylene)dicarbamate-2,3-bis(3,5-dimethylphenylcarbamate)-amylose)-2-hydroxylpropoxy-propylsilyl-appended
silica particles as chiral stationary phase for HPLC
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  Authors: Xu L; Wang H, Yi J, et al.
  Pages: 243 - 249
  Abstract: Abstract3-(Methylene-bis(1′,4′-phenylene) dicarbamate-2,3-bis(3,5-dimethylphenylcarbamate)-amylose)-2-hydroxylpropoxy-propylsilyl-appended silica particles (DMP-AM-HPS), a new type of 2, 3-regioselectively substituted amylose-immobilized chiral stationary phase (CSP) for high-performance liquid chromatography (HPLC), have been prepared by treatment of 3-(2,3-dihydroxyl-propoxy)-propylsilyl silica particles with 2,3-bis(3,5-dimethylphenylcarbamate)-amylose and 4,4′-diphenylmethane diisocyanate. The chemical characterization of the bonded particles DMP-AM-HPS has been carried out by elemental analysis and Fourier transform infrared spectroscopic analysis. The chromatographic performance of the DMP-AM-HPS has been evaluated in HPLC under multi-mode conditions including normal phase, reversed phase, and polar organic mobile phase conditions. The DMP-AM-HPS phase has exhibited excellent selectivity in separating enantiomers of a wide range of chiral drug compounds. The result also suggests that unsubstituted C6 hydroxyl groups in the regioselectively substituted amylose not only have important contributions to chiral recognitions and chromatographic separations, but also allow the DMP-AM-HPS to be used as a new type of amylose-immobilized CSP under multi-mode mobile phase conditions in HPLC.
  PubDate: Wed, 23 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab073
  Issue No: Vol. 60, No. 3 (2021)
Evaluation of Chiral Liquid Chromatographic Method for Separation and
Quantification of Isomers of Brivaracetam
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  Authors: Choppari T; Gunnam S, Chennuru L, et al.
  Pages: 250 - 259
  Abstract: AbstractA selective, sensitive and robust chiral analytical method was developed for the quantification of Brivaracetam (BRV) and its three isomers. Systematic chiral chromatographic elution process was executed in different modes on chiral columns of polysaccharide based to attain the finest condition. The analytical method was developed by utilizing immobilized polysaccharide chiral column (CHIRALPAK IG-U) with reversed phase under isocratic condition containing acetonitrile and 10 mM ammonium bicarbonate in the proportion of 40:60 (v/v). The mobile phase flow rate and column temperature were monitored at 0.3 mLmin−1 and 25°C with a resolution of more than 2.0. The eluted components from the column were processed at 212 nm UV detection. The limit of detection and limit of quantification values of BRV, 2R, 4S-Isomer, 2R, 4R-Isomer and 2S, 4S-Isomers were found to be 0.0066/0.02, 0.0035/0.0107, 0.0036/0.0109 and 0.005/0.0152 µgml−1 respectively. Precision, linearity, accuracy and robustness were conducted according to ICH guidelines and the findings were within the acceptable limits. The proposed analytical method was found to be precise, accurate and specific for the quantification of enantiomer and its diastereomers for drug product and drug substance of BRV.
  PubDate: Sat, 26 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab075
  Issue No: Vol. 60, No. 3 (2021)
A Clean, Sustainable and Stability-Indicating Method for the
Quantification of Ceftriaxone Sodium in Pharmaceutical Product by HPLC
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  Authors: da Trindade M; Kogawa A, Salgado H.
  Pages: 260 - 266
  Abstract: AbstractCeftriaxone sodium is a widely used antimicrobial, which is only available as a lyophilized powder. The presence of methods for evaluating the quality of this product is very important and helps to ensure its effectiveness, in addition to contributing to the fight against bacterial resistance. Therefore, a clean and sustainable high-performance liquid chromatography (HPLC) method has been developed for evaluating ceftriaxone stability in pharmaceutical product. A Zorbax SB C18 (150 × 4.6 mm, 5 μm) column was maintained at 25°C; the mobile phase consisted of purified water acidified with 0.2% orthophosphoric acid and ethanol (87: 13, v/v) at a flow rate of 0.9 mL min−1. The detection wavelength was set at 260 nm. The method was linear over a concentration range of 20–120 μg mL−1, precise with relative standard deviations <2%, robust in the event of minor changes to the original method conditions, accurate with recovery between 98% and 102% and specific to degradation products. The retention time for ceftriaxone sodium was ~4.6 minutes. This work shows an ecologically correct option by HPLC method for the evaluation of ceftriaxone sodium in pharmaceutical product, as well as its stability, which addresses the requirements of the current green and sustainable analytical chemistry.
  PubDate: Tue, 15 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab078
  Issue No: Vol. 60, No. 3 (2021)
HPTLC Method for the Ultrasensitive Detection of Triamterene in Plasma
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  Authors: Khorshed A; Elsutohy M, Mohamed A, et al.
  Pages: 267 - 273
  Abstract: AbstractA high-performance thin-layer chromatographic (HPTLC) method has developed for the selective detection of a diuretic drug, triamterene (TRIAM), in pure form, tablets and human plasma. The method was based on chromatographic separation of TRIAM using HPTLC plates, precoated with silica gel, and a mobile phase consisted of ethyl acetate: dimethylformamide: ammonia (7.0: 2.7: 0.3, by volume). The native fluorescence signal of TRIAM was detected at 440 nm and used to quantify TRIAM using the proposed method, improving the method sensitivity to ~250-folds in comparison to that reported in previous HPTLC studies. The developed method enabled the detection of TRIAM in pure drug and biological samples (human plasma) within linear concentrations ranged from 0.8 to 60 ng/band or 1.0 to 60 ng/band for pure drug and plasma samples, respectively. Furthermore, the method was validated according to the official guidelines to permit its applicability in quality control and clinical laboratories.
  PubDate: Mon, 14 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab076
  Issue No: Vol. 60, No. 3 (2021)
Quantitation of Cabozantinib in Human Plasma by LC–MS/MS
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  Authors: Jones R; Holleran J, Parise R, et al.
  Pages: 274 - 279
  Abstract: AbstractTo support a phase III randomized trial of the multi-targeted tyrosine kinase inhibitor cabozantinib in neuroendocrine tumors, we developed a high-performance liquid chromatography mass spectrometry method to quantitate cabozantinib in 50 μL of human plasma. After acetonitrile protein precipitation, chromatographic separation was achieved with a Phenomenex synergy polar reverse phase (4 μm, 2 × 50 mm) column and a gradient of 0.1% formic acid in acetonitrile and 0.1% formic acid in water over a 5-min run time. Detection was performed on a Quattromicro quadrupole mass spectrometer with electrospray, positive-mode ionization. The assay was linear over the concentration range 50–5000 ng/mL and proved to be accurate (103.4–105.4%) and precise (<5.0%CV). Hemolysis (10% RBC) and use of heparin as anticoagulant did not impact quantitation. Recovery from plasma varied between 103.0–107.7% and matrix effect was −47.5 to −41.3%. Plasma freeze–thaw stability (97.7–104.9%), stability for 3 months at −80°C (103.4–111.4%), and stability for 4 h at room temperature (100.1–104.9%) were all acceptable. Incurred sample reanalysis of (N = 64) passed: 100% samples within 20% difference, −0.7% median difference and 1.1% median absolute difference. External validation showed a bias of less than 1.1%. This assay will help further define the clinical pharmacokinetics of cabozantinib.
  PubDate: Wed, 07 Jul 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab090
  Issue No: Vol. 60, No. 3 (2021)
Rapid Determination of 6-Methyl-5-hepten-2-one in Fruit with LLE-GC-MS
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  Authors: Zhou Z; Wang X, Cui X, et al.
  Pages: 280 - 286
  Abstract: AbstractThe volatile compound 6-methyl-5-hepten-2-one (MHO) is an important chemical intermediate and flavor component derived from carotenoid during fruit metabolism, which is important factor impacting consumer-liking. Fruit has complex matrix and is difficult to be purified during MHO analysis. A rapid liquid–liquid extraction-gas chromatography–mass spectrometry (LLE-GC–MS) method was developed for effective determination of MHO in fruit in this study. The calibration curves for MHO showed high linearity in the range of 100–2000 ng/ml with internal standard method. The limit of detection (LOD), limit of quantification (LOQ) were both <100 ng/ml. Real samples of tomato cultivar fruit were analyzed and RSD of biological replicates varied in the range of 2.01% to 12.59%. MHO showed varied content in different tomato fruit tissues of the selected cultivars, in addition to the variation between cultivars. Furthermore, the possible fragmentation patterns were proposed for the main characteristic ions of MHO and internal standard, based on isolation of the fragment ions after the precursor ion underwent splitting at the electron impact ion source. Compared with reported solid-phase microextraction (SPME)-GC–MS method, the validated method was more rapid, precise, accurate and low cost for MHO quantitation.
  PubDate: Wed, 30 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab071
  Issue No: Vol. 60, No. 3 (2021)
Determination of Phthalate Esters in Cosmetics and Baby Care Products by a
Biosorbent Based on Lawsone Capped Chitosan and Followed by Liquid
Chromatography
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  Authors: Samadi F; Es’haghi Z.
  Pages: 287 - 297
  Abstract: AbstractThis research presents a green synthetic pathway for the preparation of a new biosorbent and eco-friendly extraction process of three phthalate esters: dimethyl phthalate, di-butyl phthalate and benzyl butyl phthalate, from cosmetics and baby care products. Dispersive solid-phase extraction was used based on a new core-shell biomass/sorbent; chitosan-loaded lawsone. The proposed method provides fortunate trapping of phthalate esters in a one-step extraction. Under the optimized extraction conditions, the current work was presented low detection limits (0.03–0.15 ng. g−1), limits of quantification (0.1–0.5 ng·g−1) and reasonable linearity (0.1–10 000 ng. g−1). The applicability of the method was estimated by recovery experiments at different spiking levels (n = 5) for phthalate esters in the real samples.
  PubDate: Fri, 11 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab062
  Issue No: Vol. 60, No. 3 (2021)
Determination of 15 + 1 European Priority Polycyclic Aromatic
Hydrocarbons in Smoked Meat Products by Saponification/Solid-Phase
Extraction and Gas Chromatography–Mass Spectrometry
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  Authors: Zhang L; Wu P, Zhou H, et al.
  Pages: 298 - 307
  Abstract: AbstractA method for the determination of 15 + 1 European priority polycyclic aromatic hydrocarbons (EUPAHs) in smoked meat samples by saponification/solid-phase extraction and gas chromatography–mass spectrometry has been developed. Both saponification and solid-phase extraction conditions were optimized, which lead to shorter sample preparation time and excellent sensitivity and selectivity. The optimal saponification condition for the lipid extract of 5.00 g smoked food sample was 5 mL KOH (1.5 mol/L)–ethanol at 70°C for 5 min, and the shorter alkaline treatment time avoided the loss of volatile EUPAHs such as Benzo[c]fluorene. All the EUPAHs showed good linearity in the range between 5.0 and 50.0 ng/mL with correlation coefficients between 0.997 and 1.00. The estimated LODs for the EUPAHs were 0.15–0.30 μg/kg, while the LOQs were 0.50–1.0 μg/kg. The three spiking levels of EUPAHs were 1.0, 2.0 and 5.0 μg/kg, and the average recovery was between 75.2 and 99.6%, while the RSD were 2.3–12.4%. This sensitive and rapid method was successfully applied to smoked meat samples from Zhejiang Province of China, and the results revealed the presence of 13 EUPAHs. Benzo[a]pyrene (BaP) was found in 19 out of 20 samples, with concentration ranging from 0.51 to 4.57 μg/kg. The sum of concentrations of PAH4 (summation of benzo(a)pyrene, chrysene, benzo(a)anthracene, and benzo(b)fluoranthene) were 2.40–53.56 μg/kg.
  PubDate: Thu, 24 Jun 2021 00:00:00 GMT
  DOI: 10.1093/chromsci/bmab087
  Issue No: Vol. 60, No. 3 (2021)