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Raman scattering and phase transitions in (NH4)3TiF7

Published: Apr 6, 2018

Author(s): Y.V. Gerasimova, A.S. Oreshonkov, N.M. Laptash, A.S. Krylov, A.R. Aliev, E.M. Roginsky

Journal: Journal of Raman Spectroscopy

Abstract Raman spectra of (NH4)3TiF7 within spectral range 10–3,400 cm−1 at temperatures 8–370 K are recorded, which revealed 2 phase transitions at temperatures T1 = 355 K and T2 = 283 K. First principles calculations of lattice dynamics and assignment of the observed lines to specific vibrational types are performed. The first phase transition is classified as an “order–disorder” one. Manifestation of 97 cm−1...

Read More thumbnail image: Raman scattering and phase transitions in NH43TiF7

Full‐field XRF instrument for cultural heritage: Application to the study of a Caillebotte painting

Published: Apr 6, 2018

Author(s): Philippe Walter, Philippe Sarrazin, Marc Gailhanou, Dominique Hérouard, Antoine Verney, David Blake

Journal: X-Ray Spectrometry

A novel full‐field X‐ray fluorescence spectrometer developed for cultural heritage applications is presented. Named “CartiX,” it was designed for routine deployment in the field (museum, archeological site) and uses a concept under development at NASA for planetary exploration. CartiX utilizes 2 miniature X‐ray tubes, a square pore Micro‐channel Plate X‐ray Optic, and a direct‐illumination CCD camera to collect spatially resolved X‐ray...

Read More thumbnail image: Fullfield XRF instrument for cultural heritage Application to the study of a Caillebotte painting

Quantitative determination of meloxicam in dog plasma by high performance liquid chromatography–tandem mass spectrometry and its application in a pharmacokinetic study

Published: Apr 4, 2018

Author(s): Yongzhi Tian, Xiao Wu, Mingjie Zhang, Longshan Zhao, Zhili Xiong, Feng Qin

Journal: Biomedical Chromatography

Abstract A rapid, selective and sensitive high‐performance liquid chromatography–tandem mass spectrometry (HPLC‐MS/MS) method was developed to determine meloxicam in beagle dog plasma. Sample pretreatment involved a one‐step protein precipitation with methanol of 0.1 mL plasma. Analysis was performed on a Venusil ASB‐C18 column with mobile phase consisting of methanol–water (containing 0.1% formic acid) (75:25, v/v). The detection was performed...

Read More thumbnail image: Quantitative determination of meloxicam in dog plasma by high performance liquid chromatographytandem mass spectrometry and its application in a pharmacokinetic study

A validated, sensitive electrophoretic method for the detection of activin receptor type II‐Fc fusion proteins in human blood

Published: Apr 4, 2018

Author(s): L. Martin, N. Zouhiri, M. Audran, A. Marchand

Journal: Drug Testing and Analysis

Abstract New therapeutic proteins that trap circulating members of the transforming growth factor (TGF) beta superfamily (activins and growth differentiation factors) show promising effects on erythropoiesis and muscular growth. They are dimeric recombinant fusion proteins composed of the extracellular domain of a human activin receptor (ActRIIA or IIB) linked to the Fc part of human IgG1. Sotatercept (ActRIIA‐Fc) and Luspatercept...

Read More thumbnail image: A validated sensitive electrophoretic method for the detection of activin receptor type IIFc fusion proteins in human blood

High‐throughput multipesticides residue analysis in earthworms by the improvement of purification method: Development and application of magnetic Fe 3 O 4 ‐SiO 2 nanoparticles based dispersive solid‐phase extraction

Published: Apr 4, 2018

Author(s): Yuhan Sun, Peipei Qi, Tao Cang, Zhiwei Wang, Xiangyun Wang, Xuewei Yang, Lidong Wang, Xiahong Xu, Qiang Wang, Xinquan Wang, Changshan Zhao

Journal: Journal of Separation Science

Abstract As a key representative organism, earthworms can directly illustrate the influence of pesticides on environmental organisms in soil ecosystems. The present work aimed to develop a high‐throughput multipesticides residue analytical method for earthworms using solid–liquid extraction with acetonitrile as the solvent and magnetic material‐based dispersive solid‐phase extraction for purification. Magnetic Fe3O4 nanoparticles...

Read More thumbnail image: Highthroughput multipesticides residue analysis in earthworms by the improvement of purification method Development and application of magnetic Fe 3 O 4 SiO 2 nanoparticles based dispersive solidphase extraction

Characterization of imatinib mesylate formulations distributed in South American countries: Determination of genotoxic impurities by UHPLC–MS/MS and dissolution profile

Published: Apr 3, 2018

Author(s): Fernanda Caroline Wolff, Thaís Luise Dillenburg, Marina Venzon Antunes, Rafael Linden, Sandrine Comparsi Wagner, Simone G. Verza

Journal: Biomedical Chromatography

Abstract Imatinib mesylate (IM) is an anti‐neoplasic drug used for the treatment of cancer. Recent new guidelines specify daily doses and concentration limits for genotoxic impurities (GTIs) in pharmaceutical final products. Therefore, in this work an analytical method using UHPLC–MS/MS was developed, validated and applied to characterize IM tablets for two GTIs: N‐(2‐methyl‐5‐aminophenyl)‐4‐(3‐pyridyl)‐2‐pyrimidine amine (Imp. 1), and...

Read More thumbnail image: Characterization of imatinib mesylate formulations distributed in South American countries Determination of genotoxic impurities by UHPLCMSMS and dissolution profile

Detection of trace amounts of citrinin in dried orange peel by using an optimized extraction method coupled with ultra‐performance liquid chromatography–tandem mass spectrometry

Published: Apr 3, 2018

Author(s): Yanqing Liu, Hongwu Wang, Su Yao, Peijie Zhu

Journal: Biomedical Chromatography

Abstract A fast and sensitive method involving ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) was introduced to detect citrinin in dried orange peel. A series of extraction, purification and chromatographic conditions was also systematically examined. With the proposed method, the obtained calibration graph was linear, with an R of 0.9996 within a concentration range of 0.5–10 ng/mL. The estimated limits of...

Read More thumbnail image: Detection of trace amounts of citrinin in dried orange peel by using an optimized extraction method coupled with ultraperformance liquid chromatographytandem mass spectrometry

Automated solid‐phase extraction of phenolic acids using layered double hydroxide–alumina–polymer disks

Published: Apr 3, 2018

Author(s): Milad Ghani, Carlos Palomino Cabello, Mohammad Saraji, Jose Manuel Estela, Víctor Cerdà, Gemma Turnes Palomino, Fernando Maya

Journal: Journal of Separation Science

Abstract The application of layered double hydroxide–Al2O3–polymer mixed‐matrix disks for solid‐phase extraction is reported for the first time. Al2O3 is embedded in a polymer matrix followed by an in situ metal‐exchange process to obtain a layered double hydroxide–Al2O3–polymer mixed‐matrix disk with excellent flow‐through properties. The extraction performance of the prepared disks is evaluated as a proof of concept for the automated extraction using...

Read More thumbnail image: Automated solidphase extraction of phenolic acids using layered double hydroxidealuminapolymer disks

Separation of positional isomers of nine 2‐phenethylamine‐derived designer drugs by liquid chromatography–tandem mass spectrometry

Published: Apr 3, 2018

Author(s): Christina Grumann, Volker Auwärter

Journal: Drug Testing and Analysis

Abstract The synthesis of positional isomers of designer drugs is a common way of bypassing legal restrictions. For forensic case work, and especially for the legal assessment of cases, there is a need for screening methods capable of the unequivocal identification of positional isomers. The presented liquid chromatography–electrospray ionization–tandem mass spectrometry (LC–ESI–MS/MS) method facilitates separation of positional...

Read More thumbnail image: Separation of positional isomers of nine 2phenethylaminederived designer drugs by liquid chromatographytandem mass spectrometry

Validation of a blood marker for plasma volume in endurance athletes during a live‐high train‐low altitude training camp

Published: Apr 3, 2018

Author(s): Louisa M. Lobigs, Laura A. Garvican‐Lewis, Victor L. Vuong, Nicolin Tee, Christopher J. Gore, Peter Peeling, Brian Dawson, Yorck O. Schumacher

Journal: Drug Testing and Analysis

Abstract Altitude is a confounding factor within the Athlete Biological Passport (ABP) due, in part, to the plasma volume (PV) response to hypoxia. Here, a newly developed PV blood test is applied to assess the possible efficacy of reducing the influence of PV on the volumetric ABP markers; haemoglobin concentration ([Hb]) and the OFF‐score. Endurance athletes (n=34) completed a 21‐night simulated live‐high train‐low (LHTL) protocol...

Read More thumbnail image: Validation of a blood marker for plasma volume in endurance athletes during a livehigh trainlow altitude training camp

Temperature‐controlled liquid–liquid microextraction combined with high‐performance liquid chromatography for the simultaneous determination of diazinon and fenitrothion in water and fruit juice samples

Published: Apr 3, 2018

Author(s): Alireza Bazmandegan‐Shamili, Shayessteh Dadfarnia, Ali Mohammad Haji Shabani, Masoud Rohani Moghadam, Mahboubeh Saeidi

Journal: Journal of Separation Science

Abstract A simple, environmentally benign, and rapid method based on temperature‐controlled liquid–liquid microextraction using a deep eutectic solvent was developed for the simultaneous extraction/preconcentration of diazinon and fenitrothion. The method involved the addition of deep eutectic solvent to the aqueous sample followed by heating the mixture in a 75°C water bath until the solvent was completely dissolved in the aqueous...

Read More thumbnail image: Temperaturecontrolled liquidliquid microextraction combined with highperformance liquid chromatography for the simultaneous determination of diazinon and fenitrothion in water and fruit juice samples

Method for the simultaneous determination of monoaromatic and polycyclic aromatic hydrocarbons in industrial effluents using dispersive liquid–liquid microextraction with gas chromatography–mass spectrometry

Published: Apr 3, 2018

Author(s): Patrycja Makoś, André Fernandes, Grzegorz Boczkaj

Journal: Journal of Separation Science

Abstract We present a new method for simultaneous determination of 22 monoaromatic and polycyclic aromatic hydrocarbons in postoxidative effluents from the production of petroleum bitumen using dispersive liquid–liquid microextraction coupled to gas chromatography and mass spectrometry. The eight extraction parameters including the type and volume of extraction and disperser solvent, pH, salting out effect, extraction, and...

Read More thumbnail image: Method for the simultaneous determination of monoaromatic and polycyclic aromatic hydrocarbons in industrial effluents using dispersive liquidliquid microextraction with gas chromatographymass spectrometry

Highly sensitive VOC gas sensor employing deep cooling of SERS film

Published: Apr 3, 2018

Author(s): Myoung‐Kyu Oh, Ranjit De, Sang‐Youp Yim

Journal: Journal of Raman Spectroscopy

Abstract The potential of surface‐enhanced Raman spectroscopy (SERS) as a highly sensitive and selective gas sensor was investigated experimentally. Especially, the relation between the temperature of a SERS film and gas adsorption or signal intensity was observed systemically and quantitatively, from which the enhancement of gas adsorption and signal intensity by up to 40 times was observed with the SERS film temperature of approx....

Read More thumbnail image: Highly sensitive VOC gas sensor employing deep cooling of SERS film

A sensitive LC–MS/MS method for simultaneous determination of cabozantinib and its metabolite cabozantinib N ‐oxide in rat plasma and its application in a pharmacokinetic study

Published: Apr 2, 2018

Author(s): Lian‐jie Ren, Hua‐jing Wu, Li‐han Sun, Xue Xu, Li‐ying Mo, Lei Zhang, Jun‐ying Zhang, Chun‐yong Wu

Journal: Biomedical Chromatography

Abstract Cabozantinib (CBZ) is used for the treatment of progressive, metastatic medullary thyroid cancer. Its major oxidative metabolite is cabozantinib N‐oxide (CBN), which contains a structural alert associated with mutagenicity, yet the pharmacokinetics studies lack the simultaneous investigation of CBN and dose proportionality. In the current study a simple LC–MS/MS method was developed and validated for the simultaneous...

Read More thumbnail image: A sensitive LCMSMS method for simultaneous determination of cabozantinib and its metabolite cabozantinib N oxide in rat plasma and its application in a pharmacokinetic study

Determination of metoserpate, buquinolate, and diclofenac in pork, eggs, and milk using liquid chromatography–tandem mass spectrometry

Published: Apr 2, 2018

Author(s): Jin‐A Park, A. M. Abd El‐Aty, Weijia Zheng, Seong‐Kwan Kim, Jeong‐min Choi, Ahmet Hacımüftüoğlu, Jae‐Han Shim, Ho‐Chul Shin

Journal: Biomedical Chromatography

Abstract In this work, a method was developed for the simultaneous determination of residual metoserpate, buquinolate and diclofenac in pork, milk, and eggs. Samples were extracted with 0.1% formic acid in acetonitrile, defatted with n‐hexane, and filtered prior to analysis using liquid chromatography–tandem mass spectrometry. The analytes were separated on a C18 column using 0.1% acetic acid and methanol as the mobile phase. The matrix‐matched...

Read More thumbnail image: Determination of metoserpate buquinolate and diclofenac in pork eggs and milk using liquid chromatographytandem mass spectrometry

Lipophilicity evaluation of some thiazolyl‐1,3,4‐oxadiazole derivatives with antifungal activity

Published: Apr 2, 2018

Author(s): Cristina Ioana Stoica, Ioana Ionuț, Laurian Vlase, Brîndușa Tiperciuc, Gabriel Marc, Smaranda Oniga, Cătălin Araniciu, Ovidiu Oniga

Journal: Biomedical Chromatography

Abstract The chromatographic behavior of a series of thiazolyl‐1,3,4‐oxadiazoles with antifungal activity was studied by reverse‐phase thin‐layer chromatography (RP‐TLC). The lipophilicity parameters derived from RP‐TLC were correlated with the data derived from liquid‐chromatography mass‐spectrometry. Good linear relationships were observed between the chromatographic lipophilicity parameters and the theoretical lipophilicity...

Read More thumbnail image: Lipophilicity evaluation of some thiazolyl134oxadiazole derivatives with antifungal activity

Simultaneous determination of evodiamine and its four metabolites in rat plasma by LC–MS/MS and its application to a pharmacokinetic study

Published: Apr 2, 2018

Author(s): Cuiyun Wang, Fang Yue, Guangfeng Ai, Jie Yang

Journal: Biomedical Chromatography

Abstract A simple and sensitive liquid chromatography tandem mass spectrometry method was validated for simultaneous quantification of evodiamine and its metabolites 10‐hydroxyevodiamine (M1), 18‐hydroxyevodiamine (M2), 10‐hydroxyevodiamine‐glucuronide (M3) and 18‐hydroxy‐ evodiamine‐glucuronide (M4) in rat plasma for the first time. The analytes were extracted with acetonitrile and separated on a C18 column within 3 min. The...

Read More thumbnail image: Simultaneous determination of evodiamine and its four metabolites in rat plasma by LCMSMS and its application to a pharmacokinetic study

Enantioseparation and determination of dufulin enantiomers in cucumber and soil by chiral liquid chromatography–tandem mass spectrometry

Published: Apr 2, 2018

Author(s): Haizhen Zhang, Min Huang, Weiwei Yu, A'wei Zhang, Kankan Zhang, Deyu Hu

Journal: Biomedical Chromatography

Abstract A simple and rapid method for enantioselective determination of dufulin in cucumber and soil was developed by liquid chromatography with tandem mass spectrometry. The enantiomers were separated on a Superchiral S‐OD chiral cellulose tris(3,5‐dimethylphenylcarbamate) column at 20°C, with a mixture of acetonitrile and water (0.1% formic acid; 52:48, v/v) as mobile phase at a flow rate of 0.65 mL/min. The pretreatment conditions were...

Read More thumbnail image: Enantioseparation and determination of dufulin enantiomers in cucumber and soil by chiral liquid chromatographytandem mass spectrometry

Quantification of amlodipine and atorvastatin in human plasma by UPLC–MS/MS method and its application to a bioequivalence study

Published: Apr 2, 2018

Author(s): Mamdouh R. Rezk, Kamal A. Badr

Journal: Biomedical Chromatography

Abstract A robust, rapid and sensitive UPLC–MS/MS method has been developed, optimized and validated for the determination of amlodipine (AML) and atorvastatin (ATO) in human plasma using eplerenone as an internal standard (IS). Multiple‐reaction monitoring in positive electrospray ionization mode was utilized in Xevo TQD LC–MS/MS. Double extraction was used in sample preparation using diethyl ether and ethyl acetate. The prepared...

Read More thumbnail image: Quantification of amlodipine and atorvastatin in human plasma by UPLCMSMS method and its application to a bioequivalence study

Oscillating gradient diffusion kurtosis imaging of normal and injured mouse brains

Published: Mar 30, 2018

Author(s): Dan Wu, Qiang Li, Frances J. Northington, Jiangyang Zhang

Journal: NMR in Biomedicine

Recent advances in diffusion MRI employ multiple diffusion encoding schemes with varying diffusion direction, weighting, and diffusion time to investigate specific microstructural properties in biological tissues. In this study, we examined time‐dependent diffusion kurtosis contrast in adult mouse brains and in neonatal mouse brains after hypoxic–ischemic (HI) injury. In vivo diffusion kurtosis maps were acquired with a short diffusion time using an...

Read More thumbnail image: Oscillating gradient diffusion kurtosis imaging of normal and injured mouse brains
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