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Preparative enantioseparation of loxoprofen precursor by recycling countercurrent chromatography with hydroxypropyl‐β‐cyclodextrin as a chiral selector

Published: May 22, 2018

Author(s): Hui Zhang, Xujun Qiu, Liqiong Lv, Wenyu Sun, Chaoyue Wang, Jizhong Yan, Shengqiang Tong

Journal: Journal of Separation Science

Abstract Recycling countercurrent chromatography was successfully applied to the resolution of 2‐(4‐bromomethylphenyl)propionic acid, a key synthetic intermediate for synthesis of nonsteroidal anti‐inflammatory drug loxoprofen, using hydroxypropyl‐β‐cyclodextrin as chiral selector. The two‐phase solvent system composed of n‐hexane/n‐butyl acetate/0.1 mol/L citrate buffer solution with pH 2.4 (8:2:10, v/v/v) was selected....

Read More thumbnail image: Preparative enantioseparation of loxoprofen precursor by recycling countercurrent chromatography with hydroxypropylcyclodextrin as a chiral selector

Multi‐similarity measurement driven ensemble just‐in‐time learning for soft sensing of industrial processes

Published: May 22, 2018

Author(s): Xiaofeng Yuan, Jiao Zhou, Yalin Wang, Chunhua Yang

Journal: Journal of Chemometrics

Abstract Just‐in‐time learning (JITL) technique has been widely used for adaptive soft sensing of nonlinear processes. It builds online local model with the most relevant samples from historical dataset whenever a query sample comes. Hence, the prediction performance greatly depends on the similarity measurement for relevant sample selection. Different similarity measurements have been developed for sample selection in the past...

Read More thumbnail image: Multisimilarity measurement driven ensemble justintime learning for soft sensing of industrial processes

Development of new extraction method based on liquid–liquid–liquid extraction followed by dispersive liquid–liquid microextraction for extraction of three tricyclic antidepressants in plasma samples

Published: May 21, 2018

Author(s): Mir Ali Farajzadeh, Maryam Abbaspour

Journal: Biomedical Chromatography

Abstract In the present study, a new extraction method based on a three–phase system, liquid–liquid–liquid extraction, followed by dispersive liquid–liquid microextraction has been developed and validated for the extraction and preconcentration of three commonly prescribed tricyclic antidepressant drugs – amitriptyline, imipramine, and clomipramine – in human plasma prior to their analysis by gas chromatography–flame ionization...

Read More thumbnail image: Development of new extraction method based on liquidliquidliquid extraction followed by dispersive liquidliquid microextraction for extraction of three tricyclic antidepressants in plasma samples

LC–MS/MS method for the simultaneous determination of tenofovir, emtricitabine, elvitegravir and rilpivirine in dried blood spots

Published: May 21, 2018

Author(s): Pavan Kumar Prathipati, Subhra Mandal, Christopher J. Destache

Journal: Biomedical Chromatography

Abstract A simple, short, and rugged LC–MS/MS method for the simultaneous determination of tenofovir, emtricitabine, elvitegravir and rilpivirine was developed and validated. Dried blood spots were prepared with 25 μL of spiked whole blood. A 3 mm punch was extracted with methanol containing labeled internal standards. Ten microliters was injected into the LC–MS/MS using isocratic mobile phase composed of 0.1% formic acid in...

Read More thumbnail image: LCMSMS method for the simultaneous determination of tenofovir emtricitabine elvitegravir and rilpivirine in dried blood spots

Liquid chromatographic–tandem mass spectrometry assay for the quantification of MDT‐637 in human nasal wash

Published: May 21, 2018

Author(s): Shane C. Karnik, Robert Cook, Steve H. Gorman, Ray Bakhtiar

Journal: Biomedical Chromatography

Abstract MDT‐637 is a new chemical entity that shows potent and selective antiviral activity against respiratory syncytial virus. As part of the new drug development program, a method for quantitating MDT‐637 in nasal wash collected from human subjects was required. This article describes the method development and validation and application of a bioanalytical assay for MDT‐637 in human nasal wash using liquid chromatography–tandem...

Read More thumbnail image: Liquid chromatographictandem mass spectrometry assay for the quantification of MDT637 in human nasal wash

Determination of armepavine in mouse blood by UPLC‐MS/MS and its application to pharmacokinetic study

Published: May 21, 2018

Author(s): Peiwu Geng, Jun Luo, Ziwei Weng, Zhehua Fan, Bin Zhang, Jianshe Ma, Xianqin Wang, Meiling Zhang

Journal: Biomedical Chromatography

Abstract The purpose of this study was to develop an ultra‐performance liquid chromatography with tandem mass spectrometry (UPLC‐MS/MS) method to determine armepavine in mouse blood. Nuciferine was used as internal standard. Chromatographic separation was performed on a UPLC BEH (2.1 × 50 mm, 1.7 μm) column with a gradient elution of acetonitrile and 10 mmol/L ammonium acetate solution (containing 0.1% formic acid). The quantitative...

Read More thumbnail image: Determination of armepavine in mouse blood by UPLCMSMS and its application to pharmacokinetic study

Quality evaluation of six bioactive constituents in goji berry based on capillary electrophoresis field amplified sample stacking

Published: May 21, 2018

Author(s): Wei‐Feng Wang, Jun‐Li Yang, Yan‐Ping Shi

Journal: ELECTROPHORESIS

Abstract Goji berry, fruits of the plant Lycium barbarum L., has long been used as traditional medicine and functional food in China. In this work, a simple and easy‐operation on‐line concentration capillary electrophoresis (CE) for detection flavonoids in goji berry was developed by coupling of field amplified sample stacking (FASS) with an electroosmotic (EOF) pump driving water removal process. Due to the EOF pump and electrokinetic ...

Read More thumbnail image: Quality evaluation of six bioactive constituents in goji berry based on capillary electrophoresis field amplified sample stacking

Speciation analysis of mercury by dispersive solid‐phase extraction coupled with capillary electrophoresis

Published: May 21, 2018

Author(s): Jinhua Li, Junying Liu, Wenhui Lu, Fangfang Gao, Liyan Wang, Jiping Ma, Huitao Liu, Chunyang Liao, Lingxin Chen

Journal: ELECTROPHORESIS

Abstract A pretreatment method of dispersive solid‐phase extraction (DSPE) along with back‐extraction followed by CE‐UV detector was developed for the determination of mercury species in water samples. Sulfhydryl‐functionalized SiO2 microspheres (SiO2−SH) were synthesized and used as DSPE adsorbents for selective extraction and enrichment of three organic mercury species namely ethylmercury (EtHg), methylmercury (MeHg), and phenylmercury...

Read More thumbnail image: Speciation analysis of mercury by dispersive solidphase extraction coupled with capillary electrophoresis

Rapid screening and identification of antioxidants in the leaves of Malus hupehensis using off‐line two‐dimensional HPLC–UV–MS/MS coupled with a 1,1′‐diphenyl‐2‐picrylhydrazyl assay

Published: May 21, 2018

Author(s): Minzhuo Liu, Xueqian Huang, Qi Liu, Miao Chen, Sen Liao, Fawei Zhu, Shuyun Shi, Hua Yang, Xiaoqing Chen

Journal: Journal of Separation Science

Abstract The leaves of Malus hupehensis have a strong antioxidant activity and are commonly consumed as a healthy tea. However, detailed information about its antioxidants is incomplete. Herein, we developed an effective strategy based on combining off‐line two‐dimensional high‐performance liquid chromatography with ultraviolet and tandem mass spectrometry detection with a 1,1′‐diphenyl‐2‐picrylhydrazyl assay to rapidly screen and...

Read More thumbnail image: Rapid screening and identification of antioxidants in the leaves of Malus hupehensis using offline twodimensional HPLCUVMSMS coupled with a 11diphenyl2picrylhydrazyl assay

Simultaneous analysis of multiple urinary biomarkers for the evaluation of oxidative stress by automated online in‐tube solid‐phase microextraction coupled with negative/positive ion‐switching mode liquid chromatography–tandem mass spectrometry

Published: May 21, 2018

Author(s): Akihiro Saito, Mariko Hamano, Hiroyuki Kataoka

Journal: Journal of Separation Science

Abstract This study described an automated online method for the simultaneous determination of 8‐isoprostane, 8‐hydroxy‐2′‐deoxyguanosine, and 3‐nitro‐l‐tyrosine in human urine. The method involves in‐tube solid‐phase microextraction using a Carboxen 1006 PLOT capillary column as an extraction device, followed by liquid chromatography with tandem mass spectrometry using a CX column and detection in the negative/positive switching...

Read More thumbnail image: Simultaneous analysis of multiple urinary biomarkers for the evaluation of oxidative stress by automated online intube solidphase microextraction coupled with negativepositive ionswitching mode liquid chromatographytandem mass spectrometry

Molecular identification of Asian lacquers from different trees using Py‐GC/MS and ToF‐SIMS

Published: May 21, 2018

Author(s): Jihye Lee, Se‐Bi Jung, Tanguy Terlier, Kang‐Bong Lee, Yeonhee Lee

Journal: Surface and Interface Analysis

Traditional Asian lacquers are natural products with highly valued properties, including beauty, gloss, and durability. Pyrolysis‐gas chromatography/mass spectrometry is the technique of choice to study insoluble polymeric lacquer films. In the present study, pyrolysis‐gas chromatography/mass spectrometry results showed that the pyrolysis products of lacquer films were different for all of the studied trees, with urushiol derivatives...

Read More thumbnail image: Molecular identification of Asian lacquers from different trees using PyGCMS and ToFSIMS

Different theoretical approaches at optical characterization of randomly rough silicon surfaces covered with native oxide layers

Published: May 21, 2018

Author(s): Ivan Ohlídal, Jiří Vohánka, Jan Mistrík, Martin Čermák, Daniel Franta

Journal: Surface and Interface Analysis

Results of the optical characterization of randomly rough silicon surfaces covered with native oxide layers based on processing experimental data obtained by ellipsometry and reflectometry are presented. It is shown that the Rayleigh‐Rice theory is suitable theoretical approach for characterizing micro‐rough surfaces in contrast to effective medium approximation. Combination of the Rayleigh‐Rice theory and scalar diffraction theory is...

Read More thumbnail image: Different theoretical approaches at optical characterization of randomly rough silicon surfaces covered with native oxide layers

A growth mechanism for carbon nanotubes using metal oxides as catalysts

Published: May 21, 2018

Author(s): Hassan Wahab, Mohamed M. El Gomati, Steven J. Hinder, John F. Watts

Journal: Surface and Interface Analysis

Metal oxides have only recently begun to be used as catalysts for the growth of carbon nanotubes. Here, we propose a new model for the growth of carbon nanotubes, based on the intra‐granular charge transfer transition and the lattice strain of the catalyst nanoparticles. This is supported by results obtained from the doped metal oxides like samarium doped zinc oxide (SmZnO) and terbium doped zinc oxide (TbZnO). The intragranular charge...

Read More thumbnail image: A growth mechanism for carbon nanotubes using metal oxides as catalysts

Enhancements in full‐field PIXE imaging—Large area elemental mapping with increased lateral resolution devoid of optics artefacts

Published: May 20, 2018

Author(s): Josef Buchriegler, Nico Klingner, Daniel Hanf, Frans Munnik, Stanisław H. Nowak, Oliver Scharf, René Ziegenrücker, Axel D. Renno, Johannes von Borany

Journal: X-Ray Spectrometry

The combination of a pn‐junction charge‐coupled device‐based pixel detector with a poly‐capillary X‐ray optics was installed and examined at the Helmholtz‐Zentrum Dresden‐Rossendorf. The set‐up is intended for particle‐induced X‐ray emission imaging to survey the trace elemental composition of flat/polished geological samples. In the standard configuration, a straight X‐ray optics (20 μm capillary diameter) is used to guide the emitted...

Read More thumbnail image: Enhancements in fullfield PIXE imagingLarge area elemental mapping with increased lateral resolution devoid of optics artefacts

The pharmacokinetics and tissue distribution of curcumin and its metabolites in mice

Published: May 18, 2018

Author(s): Junjun Wang, Xuejin Yu, Ling Zhang, Ling Wang, Zhihong Peng, Yong Chen

Journal: Biomedical Chromatography

Abstract Curcumin (CUR) is the major active component of turmeric and plays an important role in the prevention and treatment of many chronic diseases such as respiratory and neurodegenerative disease. In the present work, a rapid and simple LC–MS/MS method was developed to investigate the pharmacokinetics and tissue distribution of CUR and its metabolites in mice after intravenous administration of CUR (20 mg/kg). The results...

Read More thumbnail image: The pharmacokinetics and tissue distribution of curcumin and its metabolites in mice

Stiffness reconstruction methods for MR elastography

Published: May 18, 2018

Author(s): Daniel Fovargue, David Nordsletten, Ralph Sinkus

Journal: NMR in Biomedicine

Assessment of tissue stiffness is desirable for clinicians and researchers, as it is well established that pathophysiological mechanisms often alter the structural properties of tissue. Magnetic resonance elastography (MRE) provides an avenue for measuring tissue stiffness and has a long history of clinical application, including staging liver fibrosis and stratifying breast cancer malignancy. A vital component of MRE consists of the...

Read More thumbnail image: Stiffness reconstruction methods for MR elastography

Analysis of buried interfaces in multilayer device structures with hard XPS (HAXPES) using a CrKα source

Published: May 18, 2018

Author(s): O. Renault, E. Martinez, C. Zborowski, J. Mann, R. Inoue, J. Newman, K. Watanabe

Journal: Surface and Interface Analysis

Applications of laboratory hard X‐ray photoelectron spectroscopy on buried interfaces in devices are presented. We use a novel spectrometer fitted with a monochromated CrKα source (photon energy: 5414.9 eV) and a high‐voltage analyzer. Elements buried at depths as deep as 25 nm underneath various overlayers such as Al/Ta and Pt/Ti are detected and quantified from survey spectra, with chemical shifts accessible from...

Read More thumbnail image: Analysis of buried interfaces in multilayer device structures with hard XPS HAXPES using a CrK source

Optimized two‐dimensional gel electrophoresis in an alkaline pH range improves the identification of intracellular CFDA‐cisplatin‐protein adducts in ovarian cancer cells

Published: May 17, 2018

Author(s): Sandra Kotz, Maximilian Kullmann, Ganna V. Kalayda, Nadine Dyballa‐Rukes, Ulrich Jaehde, Sabine Metzger

Journal: ELECTROPHORESIS

Abstract Intracellular binding of cisplatin to proteins has been associated with acquired resistance to chemotherapy. In our previous study we established an analytical method for the identification of intracellular cisplatin‐binding proteins. The method used a fluorescent carboxyfluorescein‐diacetate‐labeled cisplatin analogue (CFDA‐cisplatin), two‐dimensional gel electrophoresis (2DE) and mass spectrometry, which allows detecting...

Read More thumbnail image: Optimized twodimensional gel electrophoresis in an alkaline pH range improves the identification of intracellular CFDAcisplatinprotein adducts in ovarian cancer cells

Development of a reversed phase liquid chromatographic method for analysis of pyridoxal‐5′‐phosphate and its impurities

Published: May 17, 2018

Author(s): Marwa Fouad Mansour, Micheal Assefa, Ahmed El‐Khouly, Peixi Zhu, Ann Van Schepdael, Erwin Adams

Journal: ELECTROPHORESIS

Abstract Since no proper method is available in literature for the analysis of pyridoxal‐5′‐phosphate, a reversed phase liquid chromatographic method was developed and validated for specificity, sensitivity, linearity, precision and accuracy. Nine potential related substances and forced degradation products could be successfully separated from the main peak. The separation was achieved on a Polaris C18 column...

Read More thumbnail image: Development of a reversed phase liquid chromatographic method for analysis of pyridoxal5phosphate and its impurities

Sonochemical and mechanical stirring synthesis of liquid metal nanograss structures for low‐cost SERS substrates

Published: May 17, 2018

Author(s): Xiaojun Chen, Qinnan Chen, Dezhi Wu, Yuekun Zheng, Zhou Zhou, Kunpeng Zhang, Wenlong Lv, Yang Zhao, Liwei Lin, Daoheng Sun

Journal: Journal of Raman Spectroscopy

Abstract Micro‐nanofabrication technologies are frequently used to prepare surface‐enhanced Raman scattering (SERS)‐active substrates with specially shaped microstructures, whose characteristics of high sensitivity and good reproducibility are our unswerving pursuit of the goal. However, these techniques suffer from high cost and low throughput, which limits the fabrication of large‐area SERS substrates and restricts their practical...

Read More thumbnail image: Sonochemical and mechanical stirring synthesis of liquid metal nanograss structures for lowcost SERS substrates
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