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Determination of cycloserine in microdialysis samples using liquid chromatography–tandem mass spectrometry with benzoyl chloride derivatization

Published: Jan 29, 2018

Author(s): Wenjing Zhang, Sihui Wan, Lizhi Chen, Xuebin Wang, Zhuo Wang, Yi Huang

Journal: Biomedical Chromatography

Abstract A new method for the analysis of cycloserine (4‐amino‐3‐isoxazolidinone, CYC) in rat microdialysis samples has been developed. This method consists of derivatizing the CYC with benzoyl chloride, which transforms primary amines into highly stable derivatives. An attractive feature of this method was that the derivatization reaction is straightforward and can be completed within 10 min. The formed derivative, in contrast to...

Read More thumbnail image: Determination of cycloserine in microdialysis samples using liquid chromatographytandem mass spectrometry with benzoyl chloride derivatization

Development and validation of LC‐MS/MS method for simultaneous determination of sofosbuvir and daclatasvir in human Plasma: Application to pharmacokinetic study

Published: Jan 29, 2018

Author(s): Ola M. Abdallah, Ahmed M. Abdel‐Megied, Amira S. Gouda

Journal: Biomedical Chromatography

Abstract A simple and highly sensitive liquid chromatography–tandem mass spectrometry (LC‐MS/MS) bioanalytical method was developed and fully validated for the first time for the simultaneous determination of newly discovered antiviral drugs, namely sofosbuvir (SOF) and daclatasvir (DAC) in human plasma. Tadalafil (TAD) was used as internal standard (IS). SOF, DAC and TAD (IS) were extracted from plasma using liquid–liquid...

Read More thumbnail image: Development and validation of LCMSMS method for simultaneous determination of sofosbuvir and daclatasvir in human Plasma Application to pharmacokinetic study

Purification of angiotensin‐converting enzyme from human plasma and investigation of the effect of some active ingredients isolated from Nigella sativa L. extract on the enzyme activity

Published: Jan 29, 2018

Author(s): Zehra Basi, Vedat Turkoglu

Journal: Biomedical Chromatography

Abstract In the present study, one‐step purification of angiotensin‐converting enzyme (ACE, peptidyldipeptidase A, EC 3.4.15.1), responsible for regulation of blood pressure, was achieved using affinity chromatography from human plasma. The enzyme was purified 12,860‐fold with a specific activtiy of 5080 EU/mg protein. Optimum temperature and pH were determined for the enzyme as 35–40°C and pH 7.4–7.5, respectively. The purity of...

Read More thumbnail image: Purification of angiotensinconverting enzyme from human plasma and investigation of the effect of some active ingredients isolated from Nigella sativa L_ extract on the enzyme activity

Simultaneous quantification of T4, T3, rT3, 3,5‐T2 and 3,3′‐T2 in larval zebrafish ( Danio rerio ) as a model to study exposure to polychlorinated biphenyls

Published: Jan 29, 2018

Author(s): Xiaopeng Chen, Kyla M. Walter, Galen W. Miller, Pamela J. Lein, Birgit Puschner

Journal: Biomedical Chromatography

Abstract Environmental toxicants that interfere with thyroid hormone (TH) signaling can impact growth and development in animals and humans. Zebrafish represent a model to study chemically induced TH disruption, prompting the need for sensitive detection of THs. Simultaneous quantification of 3,3′,5‐triiodo‐l‐thyronine (T3), thyroxine (T4), 3,3′,5′‐triiodo‐l‐thyronine (rT3), 3,5‐diiodo‐l‐thyronine (3,5‐T2) and 3,3′‐diiodo‐l‐thyronine (3,3′‐T2)...

Read More thumbnail image: Simultaneous quantification of T4 T3 rT3 35T2 and 33T2 in larval zebrafish  Danio rerio  as a model to study exposure to polychlorinated biphenyls

Characterization and application of a lanthanide‐based metal–organic framework in the development and validation of a matrix solid‐phase dispersion procedure for pesticide extraction on peppers (Capsicum annuum L.) with gas chromatography–mass spectrometry

Published: Jan 26, 2018

Author(s): Alysson Santos Barreto, Paula de Cássia da Silva Andrade, Jéssica Meira Farias, Adalberto Menezes Filho, Gilberto Fernandes de Sá, Severino Alves Júnior

Journal: Journal of Separation Science

Abstract The metal–organic framework [(La0.9Sm0.1)2(DPA)3(H2O)3]∞ was synthetized and characterized by X‐ray diffractometry, differential thermogravimetric analysis, and infrared spectroscopy. The material was tested for the development and validation of a matrix solid‐phase dispersion procedure for extraction of atrazine, bifenthrin, bromuconazole, clofentezine, fenbuconazole, flumetralin, procymidone, and pirimicarb, from peppers, ...

Read More thumbnail image: Characterization and application of a lanthanidebased metalorganic framework in the development and validation of a matrix solidphase dispersion procedure for pesticide extraction on peppers Capsicum annuum L_ with gas chromatographymass spectrometry

Comparison of commercial organic polymer‐based and silica‐based monolithic columns using mixtures of analytes differing in size and chemistry

Published: Jan 26, 2018

Author(s): Olga Vyviurska, Yongqin Lv, Benjamin F. Mann, Frantisek Svec

Journal: Journal of Separation Science

Abstract Commercially available silica‐based monolithic columns Chromolith RP‐8e, Chromolith RP‐18, and Chromolith HR RP‐18, and polymer‐based monolithic columns ProSwift RP‐1S, ProSwift RP‐2H, and ProSwift RP‐3U varying in pore size and bonded phase have been tested for the fast separation of selected sets of analytes. These mixtures of analytes included small molecules (uracil, caffeine, 1‐phenylethanol, butyl paraben, and...

Read More thumbnail image: Comparison of commercial organic polymerbased and silicabased monolithic columns using mixtures of analytes differing in size and chemistry

Dispersion‐assisted quick and simultaneous extraction of 30 pesticides from alcoholic and non‐alcoholic drinks with the aid of experimental design

Published: Jan 26, 2018

Author(s): Rakesh Roshan Jha, Nivedita Singh, Rupender Kumari, Devendra Kumar Patel

Journal: Journal of Separation Science

Abstract The presence of pesticides in food items and beverages is a big threat to humankind, and their quantitative estimation with high precision and accuracy is always a challenge for analytical chemists. Hence, a simple and rapid method is proposed for the simultaneous determination of 30 pesticides in beverages (alcoholic and non‐alcoholic drinks). The proposed method hyphenated with triple quadrupole liquid chromatography mass...

Read More thumbnail image: Dispersionassisted quick and simultaneous extraction of 30 pesticides from alcoholic and nonalcoholic drinks with the aid of experimental design

Determination and dissipation of afidopyropen and its metabolite in wheat and soil using QuEChERS–UHPLC–MS/MS

Published: Jan 26, 2018

Author(s): Yajie Chen, Mingcheng Guo, Xingang Liu, Jun Xu, Fengshou Dong, Xiaohu Wu, Baotong Li, Yongquan Zheng

Journal: Journal of Separation Science

Abstract The dissipations of afidopyropen and its metabolite in wheat plant and soil were determined using a quick, easy, cheap, effective, rugged, and safe method with ultra‐high performance liquid chromatography and tandem mass spectrometry under a field ecosystem. The limits of quantification were estimated for both target compounds as 0.001 mg/kg. The recoveries of afidopyropen and its metabolite ranged from 94 to 114%...

Read More thumbnail image: Determination and dissipation of afidopyropen and its metabolite in wheat and soil using QuEChERSUHPLCMSMS

Rapid characterization of the absorbed chemical constituents of Tangzhiqing formula following oral administration using UHPLC–Q‐TOF‐MS

Published: Jan 26, 2018

Author(s): Xiao‐Lei Wu, Ming‐Jiang Wu, Xin‐Ze Chen, Hong‐Min Zhang, Li‐Qin Ding, Fu‐Ying Tian, Xiao‐Meng Fu, Feng Qiu, De‐Qin Zhang

Journal: Journal of Separation Science

Abstract Tangzhiqing formula, a Chinese herbal formula, is used for the treatment of type II diabetes and prediabetes. Although its effectiveness has been certified by clinical use, its absorbed chemical constituents are not comprehensively represented. Thence, in order to reveal potential bioactive components and metabolism of Tangzhiqing formula, an ultra‐high performance liquid chromatography with quadrupole time‐of‐flight mass...

Read More thumbnail image: Rapid characterization of the absorbed chemical constituents of Tangzhiqing formula following oral administration using UHPLCQTOFMS

In situ derivatization and hollow‐fiber liquid‐phase microextraction to determine sulfonamides in water using UHPLC with fluorescence detection

Published: Jan 26, 2018

Author(s): Lihua Yang, Yang Shi, Jinjin Li, Tiangang Luan

Journal: Journal of Separation Science

Abstract A sensitive method for determining sulfonamides in water was developed and validated through in situ derivatization and hollow‐fiber liquid‐phase microextraction with ultra‐high performance liquid chromatography and fluorescence detection. The target sulfonamides were sulfadiazine, sulfacetamide, sulfamerazine, sulfamethazine, sulfamethoxypyridazine, sulfachloropyridazine, sulfamethoxazole, and sulfisoxazole. Following in...

Read More thumbnail image: In situ derivatization and hollowfiber liquidphase microextraction to determine sulfonamides in water using UHPLC with fluorescence detection

Magnetic iron(III)‐based framework composites for the magnetic solid‐phase extraction of fungicides from environmental water samples

Published: Jan 26, 2018

Author(s): Yan‐Feng Huang, Qiao‐Huan Liu, Kang Li, Ying Li, Na Chang

Journal: Journal of Separation Science

Abstract We adopted a facile hydrofluoric acid‐free hydro‐/solvothermal method for the preparation of four magnetic iron(III)‐based framework composites (MIL‐101@Fe3O4‐COOH, MIL‐101‐NH2@Fe3O4‐COOH, MIL‐53@Fe3O4‐COOH, and MIL‐53‐NH2@Fe3O4‐COOH). The obtained four magnetic iron(III)‐based framework composites were applied to magnetic separation and enrichment of the fungicides (prochloraz, myclobutanil, tebuconazole, and iprodione) from...

Read More thumbnail image: Magnetic ironIIIbased framework composites for the magnetic solidphase extraction of fungicides from environmental water samples

Cellulose tris‐(3,5‐dimethylphenylcarbamate)‐based chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography: comparison with HPLC

Published: Jan 26, 2018

Author(s): Květa Kalíková, Monika Martínková, Martin G. Schmid, Eva Tesařová

Journal: Journal of Separation Science

Abstract A cellulose tris‐(3,5‐dimethylphenylcarbamate)‐based chiral stationary phase was studied as a tool for the enantioselective separation of 21 selected analytes with different pharmaceutical and physicochemical properties. The enantioseparations were performed using supercritical fluid chromatography. The effect of the mobile phase composition was studied. Four different additives (diethylamine, triethylamine, isopropylamine,...

Read More thumbnail image: Cellulose tris35dimethylphenylcarbamatebased chiral stationary phase for the enantioseparation of drugs in supercritical fluid chromatography comparison with HPLC

Determination of 3‐chloro‐1,2‐propanediol in polyamideamine epichlorohydrin resin solution by reaction‐based headspace gas chromatography

Published: Jan 26, 2018

Author(s): Ning Yan, Xiao‐Fang Wan, Xin‐Sheng Chai, Run‐Quan Chen

Journal: Journal of Separation Science

Abstract We report on a headspace gas chromatographic method for determining the content of 3‐chloro‐1,2‐propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3‐chloro‐1,2‐propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the...

Read More thumbnail image: Determination of 3chloro12propanediol in polyamideamine epichlorohydrin resin solution by reactionbased headspace gas chromatography

Snapshot‐CEST: Optimizing spiral‐centric‐reordered gradient echo acquisition for fast and robust 3D CEST MRI at 9.4 T

Published: Jan 26, 2018

Author(s): Moritz Zaiss, Philipp Ehses, Klaus Scheffler

Journal: NMR in Biomedicine

Gradient echo (GRE)‐based acquisition provides a robust readout method for chemical exchange saturation transfer (CEST) at ultrahigh field (UHF). To develop a snapshot‐CEST approach, the transient GRE signal and point spread function were investigated in detail, leading to optimized measurement parameters and reordering schemes for fast and robust volumetric CEST imaging. Simulation of the transient GRE signal was used to determine the...

Read More thumbnail image: SnapshotCEST Optimizing spiralcentricreordered gradient echo acquisition for fast and robust 3D CEST MRI at 9_4T

Efficient preparative separation of β‐cypermethrin stereoisomers by supercritical fluid chromatography with a two‐step combined strategy

Published: Jan 25, 2018

Author(s): Yilun Yan, Jun Fan, Yecai Lai, Jianfeng He, Dong Guo, Hui Zhang, Weiguang Zhang

Journal: Journal of Separation Science

Abstract An efficient two‐step method has been developed for the separation of β‐cypermethrin stereoisomers by supercritical fluid chromatography with polysaccharide chiral stationary phases. With respect to retention, selectivity, and resolution of β‐cypermethrin, the effects of chiral stationary phases, cosolvents, mobile phases, and column temperature have been studied in detail. Through a two‐step separation, β‐cypermethrin was...

Read More thumbnail image: Efficient preparative separation of cypermethrin stereoisomers by supercritical fluid chromatography with a twostep combined strategy

Hypercrosslinked particles for the extraction of sweeteners using dispersive solid‐phase extraction from environmental samples

Published: Jan 25, 2018

Author(s): Sameer S. Lakade, Qing Zhou, Aimin Li, Francesc Borrull, Núria Fontanals, Rosa M. Marcé

Journal: Journal of Separation Science

Abstract This work presents a new extraction material, namely, Q‐100, based on hypercrosslinked magnetic particles, which was tested in dispersive solid‐phase extraction for a group of sweeteners from environmental samples. The hypercrosslinked Q‐100 magnetic particles had the advantage of suitable pore size distribution and high surface area, and showed good retention behavior toward sweeteners. Different dispersive solid‐phase...

Read More thumbnail image: Hypercrosslinked particles for the extraction of sweeteners using dispersive solidphase extraction from environmental samples

Simultaneous enantioselective determination of six pesticides in aqueous environmental samples by chiral liquid chromatography with tandem mass spectrometry

Published: Jan 25, 2018

Author(s): Pengfei Zhao, Shuo Lei, Mingming Xing, Shihang Xiong, Xingjie Guo

Journal: Journal of Separation Science

Abstract A robust and sensitive method was developed for the enantiomeric analysis of six chiral pesticides (including metalaxyl, epoxiconazole, myclobutanil, hexaconazole, napropamide, and isocarbophos) in aquatic environmental samples. The optimized chromatographic conditions for the quantification of all the 12 enantiomers were performed with Chiralcel OD‐RH column using mobile phase consisting of 0.1% aqueous formic acid and...

Read More thumbnail image: Simultaneous enantioselective determination of six pesticides in aqueous environmental samples by chiral liquid chromatography with tandem mass spectrometry

A homochiral porous organic cage with large cavity and pore windows for the efficient gas chromatography separation of enantiomers and positional isomers

Published: Jan 25, 2018

Author(s): Jun‐Hui Zhang, Sheng‐Ming Xie, Bang‐Jin Wang, Pin‐Gang He, Li‐Ming Yuan

Journal: Journal of Separation Science

Abstract Porous organic cages composed of discrete cage molecules have attracted considerable recent attention as gas adsorption materials and separation media. In this study, we report a homochiral porous organic cage CC5 with a large cavity and pore windows as a novel stationary phase for high‐resolution gas chromatographic separations. The capillary column was prepared by a static coating method. A large number of racemic...

Read More thumbnail image: A homochiral porous organic cage with large cavity and pore windows for the efficient gas chromatography separation of enantiomers and positional isomers

Air‐assisted dispersive liquid–liquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenone‐type UV filters from aqueous samples

Published: Jan 25, 2018

Author(s): Dandan Ge, Yi Zhang, Yixiu Dai, Shumin Yang

Journal: Journal of Separation Science

Abstract Deep eutectic solvents are considered as new and green solvents that can be widely used in analytical chemistry such as microextraction. In the present work, a new dl‐menthol‐based hydrophobic deep eutectic solvent was synthesized and used as extraction solvents in an air‐assisted dispersive liquid–liquid microextraction method for preconcentration and extraction of benzophenone‐type UV filters from aqueous samples followed...

Read More thumbnail image: Airassisted dispersive liquidliquid microextraction based on a new hydrophobic deep eutectic solvent for the preconcentration of benzophenonetype UV filters from aqueous samples

Quality evaluation of Eucommiae Cortex processed by different methods and “sweating” conditions based on simultaneous determination of multiple bioactive constituents combined with gray relational analysis

Published: Jan 25, 2018

Author(s): Ying Yan, Hao Cai, Hui Zhao, Cuihua Chen, Lisi Zou, Xunhong Liu, Chuan Chai, Shengnan Wang, Yujiao Hua

Journal: Journal of Separation Science

Abstract Eucommiae Cortex is a classical traditional Chinese medicine, which needs to be processed by “sweating” methods. To select the suitable processing method and “sweating” processing condition for Eucommiae Cortex, in this study, the quality of Eucommiae Cortex was evaluated based on simultaneous determination of multiple bioactive constituents combined with gray relational analysis. The contents of lignans, iridoids,...

Read More thumbnail image: Quality evaluation of Eucommiae Cortex processed by different methods and sweating conditions based on simultaneous determination of multiple bioactive constituents combined with gray relational analysis
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