|
Chromatographia
Journal Prestige (SJR): 0.514  Citation Impact (citeScore): 1 Number of Followers: 21  Hybrid journal (It can contain Open Access articles)ISSN (Print) 1612-1112 - ISSN (Online) 0009-5893 Published by Springer-Verlag  [2468 journals]
|
- Handbook of Bioanalytics
-
Free pre-print version: Loading...
PubDate: 2023-05-18
-
- Development of Hyphenated Techniques and Network Identification Approaches
for Biotransformational Evaluation of Promising Antitubercular N-pyrrolyl
hydrazide-hydrazone in Isolated Rat Hepatocytes-
Free pre-print version: Loading...
Abstract: Novel, rapid and precise RP-HPLC–DAD method was developed, validated and successfully applied for determination of metabolic changes of ethyl 5-(4-bromophenyl)-1-(3-(2-(2-hydroxybenzylidene)hydrazinyl)-3-oxopropyl)-2-methyl-1H-pyrrole-3-carboxylate (12b) in isolated rat hepatocytes. The analytes were detected by a simple DAD detector at 279 nm wavelength. A single-step extraction method was implemented to enable fast purification and extraction from cellular culture, resulting in a complete recovery. Thereafter, the method was adequately transferred to a LC–MS system for identification of unknown products. Additionally, network metabolism evaluation was performed to predict the structures of major metabolites with their isotope mass through BioTransformer 3.0. The data from the LC–MS analysis and the online server were compared for comprehensive identification. The results indicated formation of four metabolic products, obtained through processes of hydrolysis (12 and b), hydroxylation in the structure 12b (M1) and O-dealkylation (M2).
PubDate: 2023-05-04
-
- Leveraging Superficially Porous Particle Technology to Develop
High-Throughput HPLC Methods for Small-Molecule Drug Discovery-
Free pre-print version: Loading...
Abstract: Superficially porous particle (SPP) columns have gained considerable momentum over fully porous particle (FPP) columns among many chromatographers. However, despite several advantages, the SPP columns are not always been used effectively with traditional HPLC. The present study explores the possibility of reducing the runtime of HPLC methods using SPP column technology without compromising the efficiency of high-throughput analysis using conventional HPLC systems. An optimized method was developed by exploiting the advantages of SPP column technology and its effectiveness demonstrated in two separate SPP columns, Kinetex EVO C18 and Accucore C18. By altering method parameters such as flow rate, gradient time, and photodiode array (PDA) detector acquisition rate, we showed that an optimized method is more efficient than the regular method. The experimental results showed significant improvement in peak capacity, peak symmetry, theoretical plate numbers, and peak resolution for the SPP column within a short runtime of 7 min. We demonstrated that the present optimized method helped to reduce runtime by 50% and provide ~ 31% net organic solvent savings, exhibiting a greener approach to methods and method development.
PubDate: 2023-05-04
-
- A Metal Organic Framework + Ionic Liquid Pseudophase System as a Gas
Chromatography Stationary Phase-
Free pre-print version: Loading...
Abstract: Ionic liquids (ILs) containing colloidal metal organic frameworks (MOFs) have been used as gas chromatography stationary phases to provide distinct separation properties. The behavior of four different organic frameworks in 18 ionic liquids was investigated. Metal organic frameworks flocculated, degraded, or formed colloidal dispersions in ionic liquids. The newly developed stationary phase consisted of colloidal ZIF-8 uniformly dispersed in an imidazolium-based dicationic ionic liquid which provided the first separation of permanent gases via hybrid gas–liquid chromatography. In addition, various groups of alkanes, ketones, alcohols, ethers, and Rohrschneider-McReynolds compounds were separated on this newly developed hybrid stationary phase. Equations for the three-phase model were derived to determine the behavior of solutes with this pseudophase system. Using this model, the distribution constants between all three phases were calculated. It was shown that the metal organic framework had a significant effect on solute partitioning to the stationary phase.
PubDate: 2023-05-02
-
- Preparation of C-Terminal Epitope Imprinted Particles for Recognition of
Cytochrome c Assisted with γ-Cyclodextrin by Host-Guest Interaction-
Free pre-print version: Loading...
Abstract: A kind of epitope surface imprinted particles was synthesized to selectively recognize cytochrome c (Cyt c) by a novel strategy assisted with γ-cyclodextrin (γ-CD) by host-guest interaction. C-terminal epitope nonapeptide of Cyt c was chosen as the template. γ-CD was immobilized on the surface of the silica as an encapsulated molecule to capture the template and improve the corresponding spatial orientation by the host-guest interaction for the peptide and target protein recognition. After γ-CD and epitope modified, the surface imprinted polymer assisted with the host-guest interaction was synthesized via monomers and cross-linkers by radical polymerization strategy. After the peptide removal, the epitope surface imprinted particles were obtained. The performance of Cyt c recognition in bovine serum sample by the imprinted polymers was calculated by HPLC. The modified imprinted polymers prepared achieved the best binding capability of 2.89 mg g−1 AE-9 with the IF = 4.07 and 37.58 mg g−1 Cyt c with the IF = 3.38, and it also realized an efficiency and selectivity protein recognition. Additionally, the imprinted particles assisting by γ-CD have good reusability with 89.89% of the original after five sorption-elution cycles and a better recognized ability (IF = 3.38) than those without γ-CD assisting (IF = 1.44). These results indicated that this epitope imprinted method assisted with the host-guest recognition interaction by γ-CD exhibited well specific recognition abilities towards the target protein Cyt c and potential application for Cyt c recognition in biological sample. Graphical
PubDate: 2023-04-27
-
- Fast RP-HPLC Method for Analysis of Glucosinolates and Phenolics in
Moringa stenopetala Leaf Powder Preparations-
Free pre-print version: Loading...
Abstract: Moringa stenopetala (M. stenopetala) leaf powder is extensively used as food, for preparation of nutraceuticals and herbal medicines in many developing countries. Glucosinolates and phenolics are known to be important bioactive constituents of these preparations. In this study, a selective and fast RP-HPLC method was developed and validated for simultaneous determination of intact glucosinolates and phenolics in M. stenopetala leaf powders. The developed method was linear with a coefficient of determination (r2) ≥ 0.998, precision ≤ 1.5%, and recovery values close to 100%. The method was also sensitive with detection and quantification limits below 1.5 µg/mL and 5 µg/mL, respectively. Besides the use of external standards, quantitative analysis of multicomponents by a single marker (QAMS) was developed and applied to commercial Moringa samples. The correlation coefficient (r ≥ 0.9993) between the QAMS and the external standard method proved the consistency and the strength of the relationship between the two methods. Rutin was used as single marker for the determination of five bioactive components in M. stenopetala leaf samples. Furthermore, a radar plot was used to differentiate samples collected from different geographical origin. Analysis results of the commercial samples revealed that rutin was found to be the constituent with the highest concentration (varying from 6.6 mg/g to 18.8 mg/g) among the phenolics while glucomoringin (0.2–4.2 mg/g) was the most common glucosinolate.
PubDate: 2023-04-26
-
- Recent Trends in Suppressor Techniques for Ion Chromatography
-
Free pre-print version: Loading...
Abstract: This review summarizes the progress in suppressor over the period from 1981 to 2022, with an emphasis on the last ten years. Although quite well investigated for decades, suppression techniques, along with their crucial roles in emerging analysis areas, have presented significantly scientific challenges. Apart from the intrinsic characters of vital components used, the design of system and the suppression mechanism are extremely important to improve the performance of suppressor for ion chromatography. Early packed-column suppressor must be regenerated off-line using an acid or base solution and had too large delay volume to possess sufficient suppression capacity. The trend is shifting toward the development of convenient, sustainable and high-performance suppressors in several ways: (i) the substantial improvement in the electrolytically or chemically regenerated suppression techniques; (ii) the miniaturization of conventional suppressors and the use of innovative designs to reduce the void volume and the overall band dispersion; and (iii) the application of ion reflux to suppressor for reducing the generation of waste. The topical review mainly focuses on the development and special applications of suppressors, spacing from the design and performance of suppressors, buffer generation, analyte enrichment and matrix isolation. Furthermore, the current challenges and future prospects regarding suppressors are discussed. Graphical
PubDate: 2023-04-25
-
- Congress, Conferences, and Workshops
-
Free pre-print version: Loading...
PubDate: 2023-04-20
-
- Low-Temperature Cleanup Followed by Dispersive Solid-Phase Extraction for
Determination of Nine Polar Plant Growth Regulators in Herbal Matrices
Using Liquid Chromatography–Tandem Mass Spectrometry-
Free pre-print version: Loading...
Abstract: Polar plant growth regulators, used alone or doped in fertilizers, are most effective and widely utilized plant growth regulators (PGRs) in agriculture, which play important roles in mediating the yield and quality of crops and foodstuffs. The application scope has been extended to herbal medicines in the past 2 decades and relevant study is inadequate. The aim of this study is to establish a QuPPe-based extraction method containing low-temperature and d-SPE cleanup procedure followed by the detection on a selective multiresidue ultrahigh-performance liquid chromatography − triple quadrupole tandem mass spectrometry (UHPLC–QqQ–MS/MS) in three herbal matrices. This simple, accurate, versatile and robust method was verified according to the validation criteria of the SANTE/12682/2019 guideline document. The analytical range was from 2.5 to 200 μg/L, and the average recoveries were in the range of 64.6−117.8% (n = 6). The optimized method was applied to 135 herbal medicines thereof. Result showed that the detection frequency of chlormequat was the highest in the investigated PGRs, with the positive rate of 15.6%. Improvement of the detection method for polar PGRs will enrich the coverage of PGRs, which is conducive to safeguard public health and ensure drug safety.
PubDate: 2023-04-13
-
- Application of UPLC-MS/MS Method for Analysis of Apigenin, Apigenin
7-Glucoside and Chlorogenic Acid in Goat Serum-
Free pre-print version: Loading...
Abstract: UPLC-MS/MS method was developed for determination of bioactive compounds including chlorogenic acid (CA), apigenin (AP) and apigenin 7-glucoside (AP7G) in goat serum. The analytes were separated on Kinetex C18 analytical column and a mobile phase consisting 0.1% formic acid in water and methanol with gradient elution. Detection of analytes was performed using a triple quadrupole mass spectrometer with electrospray ionization in positive mode. The lower limit of quantitation was 0.5 ng mL–1 for AP and AP7G and 2.5 ng mL–1 for CA. The inter- and intra-day precision of the method expressed as relative standard deviation was in the range of 1.22–14.5%. The accuracy of the method expressed as the relative error was in the range of 0.147–14.6%. The extraction recoveries of the compounds were 76.2–89.5%. The validated method was successfully applied for analysis of the compounds in the serum of sixty goats, half of which were fed with fodder with the addition of an herbal mixture. The higher concentration values of all analyzed compounds were reported in the serum of the animals fed with herbs compared to the control group receiving standard fodder.
PubDate: 2023-04-12
-
- Solid-Phase Extraction and Simultaneous Fluorescence Detection of
Cis-Diol-Containing Biomolecules Based on a Novel Boronate Affinity
Material-
Free pre-print version: Loading...
Abstract: Boronate affinity materials have been widely studied in separation science, chemical sensing, drug delivery and nanomedicine due to their unique recognition mechanism towards cis-diol-containing biomolecules (cis-diols). In this paper, a new phenylboronic acid (PBA)-functionalized silica particle was prepared by one-pot synthetic strategy based on a PBA-coupled silane reagent, which was synthesized using 1,3,5-benzenetricarboxaldehyde as a spacer arm to covalently link 3-aminophenylboronic acid and 3-aminopropyltriethoxysiliane. Such PBA-functionalized silica particles displayed wrinkle shape with large surface area of 192 m2 g−1, resulting in its high binding capacities of 480 µmol g−1 for catechol and 63 µmol g−1 for adenosine. Moreover, the PBA-functionalized silica particles could rapidly extract the cis-diols in 10 min with a high binding recovery of 83–92%, much higher than its control polymers (1 ~ 47%). In addition to the good extraction performances, the PBA-functionalized silica particles also exhibited fluorescence responses to the cis-diols using two different excitation lights at 300 nm and 470 nm, giving emission lights at 379 nm and 631 nm, respectively, whose fluorescence-responsive mechanism was preliminarily studied. In summary, the developed boronate affinity silica particles can be used not only for the solid-phase extraction of cis-diols, but also to report the recognition events through the fluorescence signals, providing an idea to develop multi-functional boronate affinity materials for simultaneous enrichment and detection of cis-diols in biological samples.
PubDate: 2023-04-12
-
- Research Progress on Extraction and Analytical Methods for Saxitoxin and
Its Congeners-
Free pre-print version: Loading...
Abstract: Saxitoxin is a potent neurotoxin commonly found in shellfish, produced by dinoflagellate and cyanobacterial blooms in seawater or fresh water. This review dissects the conventional liquid–liquid extraction (LLE) and solid-phase extraction (SPE) and the emerging microscale sample preparation method, followed by their achievements in the preconcentration of saxitoxin-group toxins from different matrices. Despite the tedious and multi-step procedures, LLE and SPE remain the most applied techniques in detecting saxitoxin due to their high sensitivity and selectivity. Nevertheless, microscale sample preparation offers potential as a green technique, especially in the development of advanced adsorbents for better sensitivity.
PubDate: 2023-04-08
-
- Chemical Characterization and Bioactivity Analysis of Polysaccharides
Extracted from Ginkgo Folium Residue with Different Solvents-
Free pre-print version: Loading...
Abstract: Ginkgo Folium residues contain a large number of polysaccharide substances that need to be exploited to achieve a deeper utilization of the resource. In this paper, the effects of hot water, acid, alkali, salt, ultrasonic-assisted extraction, and enzyme-assisted extraction on the chemical composition and biological activity of polysaccharides as major components of Ginkgo Folium residues are compared horizontally. Chemical composition analysis showed that all of the six polysaccharides obtained by different methods were acidic heteropolysaccharides. Ultrasonication broke the glycosidic bonds compared to the samples extracted with water. Both in acidic and alkaline extraction environments, the glycosidic bonds were broken, which greatly reduced the relative molecular weight of the polysaccharides. The Maillard reaction may have occurred in the alkali-extracted samples. The FT-IR spectrum of the salt-extracted sample was significantly different from the other samples, probably due to the consumption of hydroxyl groups during the extraction of polysaccharides by ammonium oxalate. The antioxidant results showed that the antioxidant capacity of alkaline medium was significantly higher than other samples. Acid and salt-extracted samples also have high antioxidant activity. Preliminary in vitro anti-inflammatory activity screening showed that the alkaline extraction method has some anti-inflammatory potential. The polysaccharides of Ginkgo Folium were extracted in different ways that could significantly inhibit LPS-induced NO secretion in RAW264.7 cells. These results provide a reference for extracting and applying polysaccharides from Ginkgo Folium residues.
PubDate: 2023-04-04
-
- High-Temperature Two-Dimensional Gas Chromatography with Flow Modulator
for Analyzing Complex Objects of Catalytic Processing-
Free pre-print version: Loading...
Abstract: This paper is dedicated to the development of the method of high-temperature two-dimensional gas chromatography (HT-GC × GC) using a flow modulator for the analysis of a number of complex high-boiling samples. A method has been developed that allows to analyze complex samples with a temperature up to 360 °C using a combination of non-polar and mid-polar columns. We have achieved separations of such complex mixtures as products of thermal cracking of slack wax, vacuum gas oil (VGO) and the products of its processing, a product of catalytic processing of sludge sediments pyrolysate and products of polyethylene pyrolysis. The method makes it possible to achieve good resolution in the previously listed samples between the groups of aromatic and aliphatic hydrocarbons. In addition, the group of aliphatic hydrocarbons was resolved into separate constituent classes: alkanes, alkenes, alkadienes, and cycloalkanes. A good resolution was reached for sludge pyrolysis samples between the groups of polar compounds and aromatic and aliphatic hydrocarbons. Comparisons with other standardized methods illustrate the high potential of high-temperature two-dimensional gas chromatography for the analysis of high-boiling mixtures.
PubDate: 2023-03-22
DOI: 10.1007/s10337-022-04210-7
-
- Accurate Quantitation of the Phenyl Group in Methylphenylsilicone Oils by
GPC-UV-
Free pre-print version: Loading...
Abstract: Phenyl content is a crucial quality indicator for phenyl silicone oils, but the current 1H NMR method for determining it is still unreliable because of the possibility of interference from methylphenylcyclosiloxane or solvents such as toluene and xylene. Here, a novel method for the determination of the phenyl content in phenyl silicone oils for has been developed using gel permeation chromatography–ultraviolet detection (GPC-UV) analysis. Under optimized parameters, the standard curve has been established in the linear range of 5–1000 μg mL−1 with a squared correlation coefficient of more than 0.999, and a quantification limit of 0.972 μg mL−1 has been obtained. Potential interference-causing substances, such as methylphenylcyclosiloxane, toluene or xylene, and various silicone oils can be readily ruled out using the GPC-UV method. The phenyl content in 9 samples of phenyl silicone oil that were readily available was determined with a recovery in the range of 84.63–106.74%. The amount (0.613 mg g−1) of phenyl in sample H1 by GPC-UV was in good agreement with that (0.603 mg g−1) by the 1H NMR analysis.
PubDate: 2023-03-17
DOI: 10.1007/s10337-023-04248-1
-
- Capillary Electrophoresis Method for Simultaneous Quantification of
Hypocholesterolemic Drugs in Binary Mixture Formulation: Fast, Green, and
Cost-Effective Alternative to HPLC-
Free pre-print version: Loading...
Abstract: A fast and sustainable environment-friendly micellar electrokinetic chromatography coupled with a diode array detector was investigated and validated in accordance with ICH requirements for the simultaneous quantification of ezetimibe and simvastatin in a tablet binary mixture formulation. Drugs’ separation from their internal standard and degradation products was achieved using the optimized electrophoretic conditions: 50 µm i.d. × 30 cm fused-silica capillary, background electrolyte composed of 20 mmol L−1 sodium tetraborate buffer solution (pH 9, adjusted with o-phosphoric acid), 30 mmol L−1 sodium dodecyl sulfate, 12% acetonitrile; with detection at 238 nm and voltage of + 30 kV. Drugs were separated in less than 6 min. The method was linear with determination coefficients 0.9956 and 0.9920 for ezetimibe and simvastatin, respectively; and precise (intra-day 1.05% and 0.38%; inter-day 1.20% and 0.69%) for ezetimibe and simvastatin, respectively. Accuracy was tested through recovery and mean values (101.0 ± 0.77% for ezetimibe and 100.4 ± 0.35% for simvastatin) were obtained. The proposed method is the first that determined ezetimibe and simvastatin in presence of their degradation products. This method can be successfully used in quality control laboratories as an alternative to HPLC technique for the simultaneous quantification of ezetimibe and simvastatin in their combined drug products and could also be used as a stability-indicating method. The proposed method greenness profile was confirmed using Green Analytical Procedure Index and Analytical GREEnness tools with a final score of 11 and 0.81, respectively. Graphical abstract
PubDate: 2023-03-15
DOI: 10.1007/s10337-023-04243-6
-
- Congress, Conferences, and Workshops
-
Free pre-print version: Loading...
PubDate: 2023-03-11
DOI: 10.1007/s10337-023-04247-2
-
- A New Reverse Phase High-Performance Liquid Chromatography (RP-HPLC)
Method for Determination of Kinetin Riboside (Plant Hormone) in
Dequalinium Chloride Based Self-assembled Vesicles: Development,
Validation, and Force Degradation Study-
Free pre-print version: Loading...
Abstract: The analytical procedure remains the fundamental part of formulation development in terms of quantification of the drug in the formulation. The purpose of the current study was to develop accurate, sensitive and rapid high performance liquid chromatography (RP-HPLC) method for the quantitation of kinetin riboside (KR) in KR-loaded dequalinium based vesicles, also known as DQAsomes. The chromatographic analysis was performed on C18 column with detection wavelength of 269 nm for KR and 310 nm for dequalinium chloride (DQA). The mobile phase consisted of 0.01 M potassium phosphate buffer and methanol in gradient system. The method was further validated according to the guidelines set by ICH. The developed chromatographic method was found to be linear from 10 to 250 µg/mL with r2 value of 0.9995. All other validation parameters including accuracy, precision, robustness, etc. were well within the acceptable limits. The current research also encompasses force degradation studies to understand the impact of different stressing conditions on the stability of drugs in the formulation. KR-loaded DQAsomes were formulated by modified film hydration method and characterized for particle size (215.32 ± 3.54 nm), size distribution (0.12 ± 0.004) and zeta potential (39.4 ± 3.04 mV). The developed and validated method was further applied to evaluate KR entrapment and loading from KR-loaded DQAsomes along with in vitro cumulative KR release from the formulation. This research would further act as a foundation for the quantification of the drug in other dequalinium-containing formulations. Graphical
PubDate: 2023-03-07
DOI: 10.1007/s10337-023-04246-3
-
- Development of an On-Line Two-dimensional Normal Phase Liquid
Chromatography System for Analysis of Weakly Polar Samples-
Free pre-print version: Loading...
Abstract: In this study, a novel on-line two-dimensional (2D) normal phase × normal phase liquid chromatography (NPLC × NPLC) was developed for the separation of weakly polar samples. The 2D NPLC was integrated by a unique designed solvent evaporation (SE) interface, including a 6-port 2-position valve and a 10-port 2-position valve in conjunction with two silica gel-packed enrichment columns. The enrichment columns played a pivotal role in evaporating normal phase (NP) solvent from the first dimensional NPLC under vacuum and elevated temperature condition. The working parameters of the interface were evaluated comprehensively. To demonstrate the resolving powerful 2D system, we analyzed three natural-sourced weakly polar compounds from the extracts of toad venom, dammar resin, and propolis. To this end, we studied the effects of mobile phase combinations, the second dimensional column length for separation of the extracts from toad venom, and propolis, respectively. In general, we have found that excellent separation can be obtained with diversity of NP solvent combinations and longer NPLC column (150 mm long). Moreover, compared with the generally used 2D reversed-phase liquid chromatography (RPLC × RPLC), the NPLC × NPLC method exhibited better separation orthogonality. In conclusion, the new NPLC × NPLC separation method provides potential advantages for analysis of weakly polar samples.
PubDate: 2023-03-05
DOI: 10.1007/s10337-022-04230-3
-
- Magnetic Solid-Phase Extraction Pretreatment Method for Quantitative
Analysis of 12 Steroids in Human Serum Based on LC–MS/MS-
Free pre-print version: Loading...
Abstract: Accurate quantification of steroid hormones based on LC–MS/MS is of great significance for the diagnosis of endocrine diseases and the study of metabolomics. However, the current liquid–liquid extraction (LLE) and solid-phase extraction (SPE) are difficult to be further accepted in the pretreatment of clinical samples. Therefore, we carefully developed and optimized a novel method for the treatment of human serum samples by magnetic solid-phase extraction (MSPE). Several necessary tests for 12 steroids, such as LLOQ, matrix effect, recovery and precision, have verified the repeatability and practicability of the method. The comparison with LLE proves that the environment-friendly MSPE has the significance of further popularization in the treatment of clinical samples. Focusing on the future, the study opens the door for the automatic preprocessing of human serum samples based on MSPE, including but not limited to the quantitative analysis of steroid hormones.
PubDate: 2023-03-02
DOI: 10.1007/s10337-023-04244-5
-
