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Chiral separation of lansoprazole and rabeprazole by capillary electrophoresis using dual cyclodextrin systems

Published: Jul 16, 2019

Author(s): Lajos Attila Papp, Gabriel Hancu, Árpád Gyéresi, Hajnal Kelemen, Zoltán‐István Szabó, Béla Noszál, Pavel Dubský, Gergő Tóth

Journal: ELECTROPHORESIS

Abstract Novel capillary electrophoresis methods using CDs as chiral selectors were developed and validated for the chiral separation of lansoprazole and rabeprazole, two proton pump inhibitors. Fourteen different neutral and anionic CDs were screened at pH 4 and 7 in the preliminary analysis. Sulfobutyl‐ether‐β‐CD with a degree of substitution of 6.5 and 10 at neutral pH proved to be the most suitable chiral selector for both compounds. Various dual CD systems were also compared, and the...

Read More thumbnail image: Chiral separation of lansoprazole and rabeprazole by capillary electrophoresis using dual cyclodextrin systems

Characterization of therapeutic antibody fragmentation using automated capillary western blotting as an orthogonal analytical technique

Published: Jul 16, 2019

Author(s): Yunxiao Zhu, Deepti Ahluwalia, Yingchen Chen, Madesh Belakavadi, Amit Katiyar, Tapan K. Das

Journal: ELECTROPHORESIS

Abstract Fragmentation in protein‐based molecules continues to be a challenge during manufacturing and storage, and requires an appropriate control strategy to ensure purity and integrity of the drug product. Electrophoretic and chromatographic methods are commonly used for monitoring the fragments. However, size‐exclusion chromatography often suffers from low resolution of low molecular weight fragments. Electrophoretic methods like CE‐SDS are not compatible with enriching fragments for...

Read More thumbnail image: Characterization of therapeutic antibody fragmentation using automated capillary western blotting as an orthogonal analytical technique

Accurate discrimination of Gastrodia elata from different geographical origins using high‐performance liquid chromatography fingerprint combined with boosting partial least‐squares discriminant analysis

Published: Jul 16, 2019

Author(s): Shanshan Sun, Yancheng Li, Lijun Zhu, Haiyan Ma, Lupan Li, Yufeng Liu

Journal: Journal of Separation Science

Abstract Gastrodia elata from different geographical origins varies in quality and pharmacological activity. This study focused on the classification and identification of Gastrodia elata from six producing areas using high‐performance liquid chromatography fingerprint combined with boosting partial least‐squares discriminant analysis. Before recognition analysis, a principal component analysis was applied to ascertain the discrimination possibility with high‐performance liquid chromatography...

Read More thumbnail image: Accurate discrimination of Gastrodia elata from different geographical origins using highperformance liquid chromatography fingerprint combined with boosting partial leastsquares discriminant analysis

Effects of cyclonic plasma deposited organosilicon nano‐coating on 316 stainless steel and its surface characterization

Published: Jul 15, 2019

Author(s): Li‐Yu Wu, Yu‐Lin Kuo, Kuang‐Hui Chang, Ting‐Hao Chen, Chou‐Yuan Cheng, Yu‐Shuan Liu, Chun Huang

Journal: Surface and Interface Analysis

Cyclonic atmospheric pressure plasma is developed to synthesize the organosilicon nano‐coating on 316 L stainless steel surface with hexamethyldisilazane (HMDSN) and HMDSN/N2 monomers. The modified 316 L stainless steel surface characteristics of cyclonic plasma deposited organosilicon nano‐coating were evaluated by the static contact angle measurement, FTIR, SEM, AFM, and XPS detections. The chemical analysis with FTIR and XPS depicts that cyclonic plasma deposited nano‐coating obtains the...

Read More thumbnail image: Effects of cyclonic plasma deposited organosilicon nanocoating on 316 stainless steel and its surface characterization

Summary of ISO/TC 201 Standard: ISO 22415—Surface chemical analysis—Secondary ion mass spectrometry—Method for determining yield volume in argon cluster sputter depth profiling of organic materials

Published: Jul 15, 2019

Author(s): Alexander G. Shard, Rasmus Havelund, Martin P. Seah, Charles A. Clifford

Journal: Surface and Interface Analysis

The International Standard ISO 22415 provides methods to measure sputtering yield volumes of organic test materials using argon cluster ions. The test materials should consist of thin films of known thicknesses between 50 and 1000 nm. The format of the test materials, the measurement of sputtering ion dose, sputtered depth, and reporting requirements for sputtering yield volumes are described.

Read More thumbnail image: Summary of ISOTC 201 Standard ISO 22415Surface chemical analysisSecondary ion mass spectrometryMethod for determining yield volume in argon cluster sputter depth profiling of organic materials

Development of rapid and high‐throughput LC–MS/MS method for quantification of olprinone in rabbit plasma

Published: Jul 15, 2019

Author(s): Martin Kertys, Petra Kosutova, Daniela Mokra, Juraj Mokry

Journal: Biomedical Chromatography

Abstract A simple, highly sensitive and rapid method for quantification of olprinone (phosphodiesterase 3 inhibitor) in rabbit plasma using liquid chromatography–tandem mass spectrometry with electrospray was developed. An aliquot of 50 μL of plasma sample was cleaned up and extracted using Ostro™ 96‐well plate followed by dilution. Chromatographic separation of olprinone and olprinone‐d3 was carried out on a CORTECS® T3 column within 3 min. Detection was achieved using a triple quadrupole...

Read More thumbnail image: Development of rapid and highthroughput LCMSMS method for quantification of olprinone in rabbit plasma

Simultaneous determination of 19 constituents in Cimicifugae Rhizoma by HPLC–DAD and screening for antioxidants through DPPH free radical scavenging assay

Published: Jul 15, 2019

Author(s): Xueni Niu, Rulan Qin, Yudan Zhao, Ling Han, Jincai Lu, Chongning Lv

Journal: Biomedical Chromatography

Abstract Cimicifugae Rhizoma (sheng ma) is a well‐known traditional Chinese medicine, which has been demonstrated to possess anti‐inflammatory, antipyretic and analgesic activities. In the present study, a simple and efficient HPLC–DAD (high‐performance liquid chromatography coupled with diode array detection) method was developed and validated for simultaneous quantification of 19 chemical components (including 16 phenolic acids, one coumarin and two alkaloids) in Cimicifugae Rhizoma. The...

Read More thumbnail image: Simultaneous determination of 19 constituents in Cimicifugae Rhizoma by HPLCDAD and screening for antioxidants through DPPH free radical scavenging assay

Hydrophobic deep eutectic solvent‐based dispersive liquid–liquid microextraction for the simultaneous enantiomeric analysis of five β‐agonists in the environmental samples

Published: Jul 15, 2019

Author(s): Yongjing Liu, Wen Xu, Hua Zhang, Wei Xu

Journal: ELECTROPHORESIS

Abstract In this study, a simple and effective method was developed for the enantiomeric analysis of five β‐agonists (terbutaline, clorprenaline, tulobuterol, clenbuterol, and salbutamol) in water samples using deep eutectic solvent (DES) based dispersive liquid–liquid microextraction and chiral LC‐MS. In such a framework, different kinds of hydrophobic DESs were tailored to examine their extraction ability for five β‐agonists from aqueous sample. After an initial screening, the primary...

Read More thumbnail image: Hydrophobic deep eutectic solventbased dispersive liquidliquid microextraction for the simultaneous enantiomeric analysis of five agonists in the environmental samples

Liquid chromatography tandem mass spectrometry with triple stage fragmentation for highly selective analysis and pharmacokinetics of alarelin in rat plasma

Published: Jul 15, 2019

Author(s): Zhi Zhang, Runzhi Li, Shihao Liu, Lei Yin, Tongtong Xu, John Paul Fawcett, Jingkai Gu

Journal: Journal of Separation Science

Abstract Alarelin, a gonadotropin‐releasing hormone analogue, is widely used in China for the treatment of endometriosis and uterine leiomyoma. In order to investigate its pharmacokinetic behavior and support the preclinical application of new formulations, we have developed a novel and highly selective bioanalytical method to determine alarelin in rat plasma based on liquid chromatography tandem mass spectrometry with triple stage fragmentation. After sample preparation by protein...

Read More thumbnail image: Liquid chromatography tandem mass spectrometry with triple stage fragmentation for highly selective analysis and pharmacokinetics of alarelin in rat plasma

Online preconcentration and determination of chondroitin sulfate, dermatan sulfate and hyaluronic acid in biological and cosmetic samples using capillary electrophoresis

Published: Jul 15, 2019

Author(s): Kanokporn Chindaphan, Kanet Wongravee, Thumnoon Nhujak, Thasinas Dissayabutra, Monpichar Srisa‐Art

Journal: Journal of Separation Science

Abstract Capillary electrophoresis with large‐volume sample stacking using an electroosmotic flow pump was developed for the determination of chondroitin sulfate, dermatan sulfate, and hyaluronic acid. Central composite design was used to simultaneously optimize the parameters for capillary electrophoresis separation. The optimized capillary electrophoresis conditions were 200 mM sodium dihydrogen phosphate, 200 mM butylamine, and 0.5% w/v polyethylene glycol as a background electrolyte, pH 4...

Read More thumbnail image: Online preconcentration and determination of chondroitin sulfate dermatan sulfate and hyaluronic acid in biological and cosmetic samples using capillary electrophoresis

Chemical characterization of leaves and calli extracts of Rosmarinus officinalis by UHPLC‐MS

Published: Jul 15, 2019

Author(s): Martha Berenice Pérez‐Mendoza, Laura Llorens‐Escobar, Pablo Emilio Vanegas‐Espinoza, Alejandro Cifuentes, Elena Ibáñez, Alma Angélica Del Villar‐Martínez

Journal: ELECTROPHORESIS

Abstract Rosmarinus officinalis L. (Lamiaceae) is an aromatic plant widely popular mainly due to its uses in traditional medicine as an anti‐inflammatory, diuretic and antimicrobial, as well as in the prevention and treatment of diseases. These biological activities are mainly related to the presence of phenolic and terpenic compounds. This work reports a chemical profile analysis of extracts from leaves and calli of rosemary obtained by both pressurized liquid extraction and maceration....

Read More thumbnail image: Chemical characterization of leaves and calli extracts of Rosmarinus officinalis by UHPLCMS

An efficient high‐speed countercurrent chromatography method for preparative separation of javanicin from Fusarium solani, a fungus isolated from the fruiting body of the mushroom Trametes trogii

Published: Jul 15, 2019

Author(s): Ruyi Guo, Xu Cai, Qian Li, Yun Huang, Benke Chen, Ping Guan, Jintian Tang, Xianwei Zou

Journal: Biomedical Chromatography

Abstract To develop an efficient method for large preparation of javanicin from Fusarium solani, a rapid and simple method by high‐speed countercurrent chromatography was established based on average polarity (P′ values) and partition coefficients (K values) of crude samples. A suitable solvent system for high‐speed countercurrent chromatography was selected from many possible biphasic solvent systems. HSCCC was successfully applied to separate and purify javanicin, the main bioactive...

Read More thumbnail image: An efficient highspeed countercurrent chromatography method for preparative separation of javanicin from Fusarium solani a fungus isolated from the fruiting body of the mushroom Trametes trogii

Quantitative analysis of multicomponents by a single marker and quality evaluation of Venenum Bufonis from different geographical origins

Published: Jul 15, 2019

Author(s): Ke‐ke Cui, Yue‐ting Cao, Jia‐feng Shao, Zheng‐yu Lu, Long‐hu Wang

Journal: Biomedical Chromatography

Abstract Bufadienolides are the main bioactive components of Venenum Bufonis (VB) and have been widely used to treat different types of human cancers for decades. The bufadienolide content in VB varies significantly in materials from different geographical origins. In this work, a new strategy for the quality assessment of VB was developed through quantitative analysis of multi‐components by single marker (QAMS). Cinobufagin was selected as the internal reference substance; seven...

Read More thumbnail image: Quantitative analysis of multicomponents by a single marker and quality evaluation of Venenum Bufonis from different geographical origins

A novel and sensitive UPLC–MS/MS method to determine mequitazine in rat plasma and urine: Validation and its application to pharmacokinetic studies

Published: Jul 15, 2019

Author(s): Seung‐Hyun Jeong, Ji‐Hun Jang, Yong‐Bok Lee

Journal: Biomedical Chromatography

Abstract The aim of this study was to develop an analytical method to determine mequitazine in rat plasma and urine. Mequitazine was separated by UPLC–MS/MS equipped with a Kinetex core–shell C18 column (50 × 2.1 mm, 1.7 μm) using 0.1% (v/v) aqueous formic acid and acetonitrile containing 0.1% (v/v) formic acid as a mobile phase by gradient elution at a flow rate of 0.3 mL/min. Quantitation of this analysis was performed on a triple quadrupole mass spectrometer employing electrospray...

Read More thumbnail image: A novel and sensitive UPLCMSMS method to determine mequitazine in rat plasma and urine Validation and its application to pharmacokinetic studies

MR signal changes in superparamagnetic iron oxide nanoparticle‐labeled macrophages in response to X irradiation

Published: Jul 15, 2019

Author(s): Masayuki Yamaguchi, Kazunobu Ohnuki, Kenji Hotta, Hirofumi Fujii

Journal: NMR in Biomedicine

To investigate whether MR signals associated with macrophages labeled with superparamagnetic iron oxide nanoparticles (SPIONs) change in response to X irradiation, we performed in vitro MRI of SPION‐labeled macrophage‐like J774A.1 cells that were subsequently X irradiated. We labeled the cells with ferucarbotran at a concentration of 10 μg iron/mL in culture medium for 16 h and subsequently performed X irradiation at doses of 0, 2, 10, or 20 Gy using a low‐energy X‐ray unit. On Days 3 and 6,...

Read More thumbnail image: MR signal changes in superparamagnetic iron oxide nanoparticlelabeled macrophages in response to X irradiation

A method for multiparametric statistical quantification of the heterogeneity of free Na+ concentration by 19F MR spectroscopy: Proof of principle in silico and in vitro

Published: Jul 12, 2019

Author(s): Norbert W. Lutz, Monique Bernard

Journal: NMR in Biomedicine

Sodium(I) (Na+) is one of the most important cations in mammalian tissues. Since Na+ plays a key role in basic cell function, noninvasive methods for measuring intracellular concentrations of free sodium ions in biological tissue have been developed on the basis of 19F NMR spectroscopy. However, intracellular Na+ levels are often not uniform throughout a tissue volume (or voxel) being measured. In such cases, [Na+] heterogeneity is not reflected in results obtained by the classical technique,...

Read More thumbnail image: A method for multiparametric statistical quantification of the heterogeneity of free Na concentration by 19F MR spectroscopy Proof of principle in silico and in vitro

Development and validation of a simple and sensitive high‐resolution LC/MS method for determination of PF‐04620110 in dog plasma: Application to a pharmacokinetic study

Published: Jul 11, 2019

Author(s): Fan He, Wei Zheng, Yongzhuang Chen, Chengke Mo, Yilu Chen

Journal: Biomedical Chromatography

Abstract In this study, a more sensitive and reliable quantitative method based on ultra‐high performance liquid chromatography coupled with Q‐Exactive‐Orbitrap‐MS in full‐mass scan was developed and validated for the determination of PF‐04620110 in dog plasma. After protein precipitation with acetonitrile, the sample separations were carried out on an Acquity BEH C18 column with 1 mm ammonium acetate in water and acetonitrile containing 0.1% acetic acid as mobile phase, at a flow rate of...

Read More thumbnail image: Development and validation of a simple and sensitive highresolution LCMS method for determination of PF04620110 in dog plasma Application to a pharmacokinetic study

Enantioseparation of 5‐chloro‐2‐{2‐[3,4‐dihydroisoquinoline‐2(1H)‐yl]ethyl}‐2‐methyl‐2,3‐dihydro‐1H‐inden‐1‐one (SYA 40247), a high‐affinity 5‐HT7 receptor ligand, by HPLC–PDA using amylose tris‐(3, 5‐ dimethylphenylcarbamate) as a chiral stationary phase

Published: Jul 11, 2019

Author(s): Edem K. Onyameh, Barbara A. Bricker, Edward Ofori, Seth Y. Ablordeppey

Journal: Biomedical Chromatography

Abstract In previous structure–activity relationship studies to identify new and selective 5‐HT7 receptor (5‐HT7R) ligands, we identified the chiral compound, 5‐chloro‐2‐{2‐[3,4‐dihydroisoquinoline‐2(1H)‐yl]ethyl}‐2‐methyl‐2,3‐dihydro‐1H‐inden‐1‐one (SYA 40247), with high‐affinity binding to the 5‐HT7R. Thus, it was of interest to separate the enantiomers in order to evaluate their affinity at the 5‐HT7R. To achieve this separation, a normal‐phase analytical method using HPLC–PDA and a 4.6...

Read More thumbnail image: Enantioseparation of 5chloro2234dihydroisoquinoline21Hylethyl2methyl23dihydro1Hinden1one SYA 40247 a highaffinity 5HT7 receptor ligand by HPLCPDA using amylose tris3 5 dimethylphenylcarbamate as a chiral stationary phase

Comparative pharmacokinetic study of four major bioactive components after oral administration of Zhi‐Zi‐Hou‐Po decoction in normal and corticosterone‐induced depressive rats

Published: Jul 11, 2019

Author(s): Yongtao Bai, Lihua Song, Yongheng Zhang, Guoliang Dai, Weidong Zhang, Shanshan Song, Hong Sun, Wen Jing, Meijuan Xu, Wenzheng Ju

Journal: Biomedical Chromatography

Abstract A highly selective and efficient LC–MS/MS method was developed to determine the plasma concentration of magnolol, hesperidin, neohesperidin and geniposide following oral administration of Zhi‐Zi‐Hou‐Po decoction in normal and depressed rats. Plasma samples were pretreated by protein precipitation with methanol. Chromatographic separation was performed on an XTerra® MS C18 column using a gradient elution with a mobile phase composed of acetonitrile–0.1% aqueous formic acid. The...

Read More thumbnail image: Comparative pharmacokinetic study of four major bioactive components after oral administration of ZhiZiHouPo decoction in normal and corticosteroneinduced depressive rats

Enantioseparation of N‐acetyl‐glutamine enantiomers by LC–MS/MS and its application to a plasma protein binding study

Published: Jul 11, 2019

Author(s): Lei Gao, Yunwen Xue, Zunjian Zhang, Yuan Tian

Journal: Biomedical Chromatography

Abstract A novel chiral method was developed and validated to determine N‐acetyl‐glutamine (NAG) enantiomers by liquid chromatography–tandem mass spectrometry (LC–MS/MS). Enantioseparation was achieved on a Chiralpak QD‐AX column (150 × 4.6 mm i.d., 5 μm) using methanol–water (50 mm ammonium formate, pH 4.3; 70:30, v/v) at a flow rate of 500 μL/min. The detection was operated with an electrospray ionization source interface in positive mode. The ion transition for NAG enantiomers was m/z...

Read More thumbnail image: Enantioseparation of Nacetylglutamine enantiomers by LCMSMS and its application to a plasma protein binding study
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