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Discrimination between closely related synthetic cannabinoids by GC–Cold–EI–MS

Published: Aug 23, 2017

Author(s): Evgeny Smolianitski‐Fabian, Etia Cohen, Marina Dronova, Anna Voloshenko‐Rossin, Ovadia Lev

Journal: Drug Testing and Analysis

Gas chromatography thermal‐electron ionization mass spectrometry (GC–EI–MS) is an established method for the identification of mind‐altering substances and is routinely used by forensic laboratories. However, some commonly analyzed drugs of abuse, relating to the synthetic cannabinoids receptor agonist group (SCs), pose a challenge for this conventional technique. As the molecular cation radicals of many excited SCs...

Read More thumbnail image: Discrimination between closely related synthetic cannabinoids by GCColdEIMS

Determination of testosterone esters in the hair of male greyhound dogs using liquid chromatography–high resolution mass spectrometry

Published: Aug 23, 2017

Author(s): Jayasree Leela Devi, Paul Zahra, John H. Vine, Ted Whittem

Journal: Drug Testing and Analysis

The doping of greyhound dogs with testosterone is done in an attempt to improve their athletic performance, but such doping cannot easily be confirmed, especially in male dogs owing to the natural presence of endogenous testosterone. As testosterone is usually administered as its esters, their direct detection in hair would provide confirmatory evidence of the administration of a pharmaceutical product. This article demonstrates that the...

Read More thumbnail image: Determination of testosterone esters in the hair of male greyhound dogs using liquid chromatographyhigh resolution mass spectrometry

Calculation of topological indices from molecular structures and applications

Published: Aug 23, 2017

Author(s): Qingyou Zhang, Kaixia Xiao, Mengyao Chen, Lu Xu

Journal: Journal of Chemometrics

Abstract This mini review presents a brief description of the research efforts for new topological indices of organic molecular structures undertaken in the authors' laboratory at Changchun Institute of Applied Chemistry, Chinese Academy of Sciences. They were used for the processing of chemical information, as highly selective topological indices for uniqueness determination, as highly selective atomic chiral indices for chiral...

Read More thumbnail image: Calculation of topological indices from molecular structures and applications

Sampling error profile analysis (SEPA) for model optimization and model evaluation in multivariate calibration

Published: Aug 23, 2017

Author(s): Wanchao Chen, Yiping Du, Feiyu Zhang, Ruoqiu Zhang, Boyang Ding, Zengkai Chen, Qin Xiong

Journal: Journal of Chemometrics

A novel method called sampling error profile analysis (SEPA) based on Monte Carlo sampling and error profile analysis is proposed for outlier detection, cross validation, pretreatment method and wavelength selection, and model evaluation in multivariate calibration. With the Monte Carlo sampling in SEPA, a number of submodels are prepared and the subsequent error profile analysis yields a median and a standard deviation of the...

Read More thumbnail image: Sampling error profile analysis SEPA for model optimization and model evaluation in multivariate calibration

Determination of effective atomic numbers and mass attenuation coefficients of samples using in‐situ energy‐dispersive X‐ray fluorescence analysis

Published: Aug 23, 2017

Author(s): Qingxian Zhang, Yinglei Guo, Haitao Bai, Yi Gu, Yang Xu, Jiankun Zhao, Liangquan Ge, Yi Peng, Jun Liu

Journal: X-Ray Spectrometry

The matrix effect has a major impact on energy‐dispersive X‐ray fluorescence analysis (EDXRFA) and is difficult to be evaluated due to that the contents of some low‐atomic‐number elements cannot be identified by in‐situ EDXRFA. Up to today, the fundamental parameter algorithm proposed by Rousseau has been widely applied to correct the matrix effect. Accordingly, determining the matrix and mass attenuation coefficient (μ/ρ) of sample is a...

Read More thumbnail image: Determination of effective atomic numbers and mass attenuation coefficients of samples using insitu energydispersive Xray fluorescence analysis

The preparation of microfluidic architecture with monolithic materials using a dual porous silica structure

Published: Aug 23, 2017

Author(s): Christopher Birch, Mohammad Mehdi Nasr Esfahani, Kirsty J Shaw, Cordula Kemp, Stephen James Haswell, Charlotte Dyer

Journal: ELECTROPHORESIS

A microfluidic device (MD) has been developed which features a porous silica (PS) monolithic disk synthesized from tetramethyl orthosilicate, incorporated into the device post‐fabrication and sealed in place with a second PS monolithic layer, synthesized from potassium silicate. This dual porous silica (DPS) structure provides a pathway for sample introduction to the MD and offers an ideal platform for solid phase extraction (SPE)...

Read More thumbnail image: The preparation of microfluidic architecture with monolithic materials using a dual porous silica structure

Determination of tigecycline in human plasma by LC–MS/MS and its application to population pharmacokinetics study in Chinese patients with hospital‐acquired pneumonia

Published: Aug 21, 2017

Author(s): Rong Shao, Xingang Li, Yangmin Hu, Jinliang Chen, Honggang Lou, Haibin Dai

Journal: Biomedical Chromatography

Abstract A selective, sensitive and rapid liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated for the determination of tigecycline (TGC) in human plasma, using tigecycline‐d9 as an internal standard (IS). Analytical samples were prepared using a protein precipitation method coupled with a concentration process. The analyte and IS were separated on a reversed‐phase Waters Acquity UPLC® BEH‐C18 column...

Read More thumbnail image: Determination of tigecycline in human plasma by LCMSMS and its application to population pharmacokinetics study in Chinese patients with hospitalacquired pneumonia

High‐performance liquid chromatography–tandem mass spectrometry for simultaneous determination of raltegravir, dolutegravir and elvitegravir concentrations in human plasma and cerebrospinal fluid samples

Published: Aug 21, 2017

Author(s): Kiyoto Tsuchiya, Mayu Ohuchi, Naoe Yamane, Hiroaki Aikawa, Hiroyuki Gatanaga, Shinichi Oka, Akinobu Hamada

Journal: Biomedical Chromatography

Abstract A simple sample treatment procedure and sensitive liquid chromatography–tandem mass spectrometry method were developed for the simultaneous quantification of the concentrations of human immunodeficiency virus‐1 integrase strand transfer inhibitors – raltegravir, dolutegravir and elvitegravir – in human plasma and cerebrospinal fluid (CSF). Plasma and CSF samples (20 μL each) were deproteinized with acetonitrile....

Read More thumbnail image: Highperformance liquid chromatographytandem mass spectrometry for simultaneous determination of raltegravir dolutegravir and elvitegravir concentrations in human plasma and cerebrospinal fluid samples

HPLC fingerprinting approach for raw material assessment and unit operation tracking for IVIG production from Cohn I+II+III fraction

Published: Aug 21, 2017

Author(s): Sebastijan Peljhan, Tina Jakop, Dunja Šček, Vid Skvarča, Blaž Goričar, Romina Žabar, Nina Mencin

Journal: ELECTROPHORESIS

The plasma‐derived IgG used either for diagnostic purpose or intravenous application (in form of IVIG) in various medical therapies is certainly gaining more and more attention on annual basis. Different manufacturing processes are used to isolate immunoglobulins from human plasma. However, a quest for alternative paths in IgG isolation not only requires development of the most efficient isolation process, but also a rapid and reliable...

Read More thumbnail image: HPLC fingerprinting approach for raw material assessment and unit operation tracking for IVIG production from Cohn IIIIII fraction

Production of β‐Lactoglobulin hydrolysates by monolith based immobilized trypsin reactors

Published: Aug 21, 2017

Author(s): Yuhong Mao, Urh Černigoj, Viktor Zalokar, Aleš Štrancar, Ulrich Kulozik

Journal: ELECTROPHORESIS

Tryptic hydrolysis of β‐Lactoglobulin (β‐Lg) is attracting more and more attention due to the reduced allergenicity and the functionality of resulting hydrolysates. To produce hydrolysates in an economically viable way, immobilized trypsin reactors (IMTRs), based on polymethacrylate monolith with pore size 2.1 μm (N1) and 6 μm (N2), were developed and used in a flow‐through system. IMTRs were characterized in terms of...

Read More thumbnail image: Production of Lactoglobulin hydrolysates by monolith based immobilized trypsin reactors

Tilted pillar array fabrication by the combination of proton beam writing and soft lithography for microfluidic cell capture Part 2: Image sequence analysis based evaluation and biological application

Published: Aug 21, 2017

Author(s): Gábor Járvás, Tamás Varga, Márton Szigeti, László Hajba, Péter Fürjes, István Rajta, András Guttman

Journal: ELECTROPHORESIS

Abstract As a continuation of our previously published work, this paper presents a detailed evaluation of a microfabricated cell capture device utilizing a doubly tilted micropillar array. The device was fabricated using a novel hybrid technology based on the combination of proton beam writing and conventional lithography techniques. Tilted pillars offer unique flow characteristics and support enhanced fluidic interaction for...

Read More thumbnail image: Tilted pillar array fabrication by the combination of proton beam writing and soft lithography for microfluidic cell capture Part 2 Image sequence analysis based evaluation and biological application

PDMS/glass hybrid device with a reusable carbon electrode for on‐line monitoring of catecholamines using microdialysis sampling coupled to microchip electrophoresis with electrochemical detection

Published: Aug 21, 2017

Author(s): Rachel A. Saylor, Susan M. Lunte

Journal: ELECTROPHORESIS

On‐line separations‐based sensors employing microdialysis (MD) coupled to microchip electrophoresis (ME) enable the continuous monitoring of multiple analytes simultaneously. Electrochemical detection (EC) is especially amenable to on‐animal systems employing MD‐ME due to its ease of miniaturization. However, one of the difficulties in fabricating MD‐ME‐EC systems is incorporating carbon working electrodes into the device. In this paper,...

Read More thumbnail image: PDMSglass hybrid device with a reusable carbon electrode for online monitoring of catecholamines using microdialysis sampling coupled to microchip electrophoresis with electrochemical detection

Discrimination of Polygoni Multiflori radix and Cynanchi Auriculati radix using ultra‐high performance liquid chromatography fingerprints and chemical pattern recognition

Published: Aug 18, 2017

Author(s): Lili Sun, Meng Wang, Yali Liu, Huijie Zhang, Yanan Liu, Xiaoliang Ren, Yanru Deng

Journal: Biomedical Chromatography

Abstract In this work, a strategy was proposed to discriminate Polygoni Multiflori Radix (PMR) and its adulterant (Cynanchi Auriculati Radix, CAR). Ultra‐high performance liquid chromatography (UHPLC) fingerprints were established to analyze samples containing PMR, CAR and mixtures simultaneously. Multivariate classification methods were applied to analyze the obtained UHPLC fingerprints, including principal component analysis...

Read More thumbnail image: Discrimination of Polygoni Multiflori radix and Cynanchi Auriculati radix using ultrahigh performance liquid chromatography fingerprints and chemical pattern recognition

Screening and identification of metabolites of two kinds of main active ingredients and hepatotoxic pyrrolizidine alkaloids in rat after lavage Farfarae Flos extract by UHPLC‐Q‐TOF‐MS mass spectrometry

Published: Aug 18, 2017

Author(s): Xiaoye Cheng, Man Liao, Xinpeng Diao, Yupeng Sun, Lantong Zhang

Journal: Biomedical Chromatography

Abstract Farfarae Flos, the dried flower buds of Tussilago farfara L., is usually used to treat coughs, bronchitic and asthmatic conditions as an important traditional Chinese medicine. Tussilagone and methl butyric acid tussilagin ester are seen as representatives of two kinds of active substances. In addition, the pyrrolizidine alkaloids, mainly senkirkine and senecionine, present in the herb can be hepatoxic. In this study, a rapid and...

Read More thumbnail image: Screening and identification of metabolites of two kinds of main active ingredients and hepatotoxic pyrrolizidine alkaloids in rat after lavage Farfarae Flos extract by UHPLCQTOFMS mass spectrometry

Simultaneous determination and method validation of difenoconazole, propiconazole and pyraclostrobin in pepper and soil by LC–MS/MS in field trial samples from three provinces, China

Published: Aug 17, 2017

Author(s): Sizhuo Wu, Haizhen Zhang, Kunming Zheng, Banghua Meng, Fei Wang, Ying Cui, Song Zeng, Kankan Zhang, Deyu Hu

Journal: Biomedical Chromatography

Abstract A liquid chromatography–electrospray ionization tandem mass spectrometry method was developed for simple and accurate detection of the fungicides difenoconazole, propiconazole and pyraclostrobin in peppers and soil. Three fungicides residues were extracted from samples by acetonitrile and cleaned up by dispersive solid‐phase extraction before instrumental analysis. The accuracy and precision of the method were evaluated by...

Read More thumbnail image: Simultaneous determination and method validation of difenoconazole propiconazole and pyraclostrobin in pepper and soil by LCMSMS in field trial samples from three provinces China

Optimization of recombinant β‐glucuronidase hydrolysis and quantification of eight urinary cannabinoids and metabolites by liquid chromatography tandem mass spectrometry

Published: Aug 16, 2017

Author(s): Cristina Sempio, Karl B. Scheidweiler, Allan J. Barnes, Marilyn A. Huestis

Journal: Drug Testing and Analysis

Prolonged urinary cannabinoid excretion in chronic frequent cannabis users confounds identification of recent cannabis intake that may be important in treatment, workplace, clinical, and forensic testing programs. In addition, differentiation of synthetic Δ9‐tetrahydrocannabinol (THC) intake from cannabis plant products might be an important interpretive issue. THC, 11‐hydroxy‐THC (11‐OH‐THC) and 11‐nor‐9‐carboxy‐THC (THCCOOH) urine...

Read More thumbnail image: Optimization of recombinant glucuronidase hydrolysis and quantification of eight urinary cannabinoids and metabolites by liquid chromatography tandem mass spectrometry

Investigation of drug products received for analysis in the Swedish STRIDA project on new psychoactive substances

Published: Aug 16, 2017

Author(s): Matilda Bäckberg, Karl‐Henrik Jönsson, Olof Beck, Anders Helander

Journal: Drug Testing and Analysis

The web‐based open sale of unregulated new psychoactive substances (NPS) has shown a steady increase in recent years. Analysis of drug products sold as NPS is useful to confirm the true chemical contents, for comparison with the substances detected in corresponding body fluids, but also to study drug trends. This work describes the examination of 251 drug products that were randomly submitted for analysis in 173 cases of suspected...

Read More thumbnail image: Investigation of drug products received for analysis in the Swedish STRIDA project on new psychoactive substances

Development and validation of a high‐performance liquid chromatography method for the quantification of talazoparib in rat plasma: Application to plasma protein binding studies

Published: Aug 15, 2017

Author(s): Mahendra Kumar Hidau, Srikanth Kolluru, Srinath Palakurthi

Journal: Biomedical Chromatography

Abstract A sensitive and selective RP‐HPLC method has been developed and validated for the quantification of a highly potent poly ADP ribose polymerase inhibitor talazoparib (TZP) in rat plasma. Chromatographic separation was performed with isocratic elution method. Absorbance for TZP was measured with a UV detector (SPD‐20A UV–vis) at a λmax of 227 nm. Protein precipitation was used to extract the drug from plasma samples using methanol–acetonitrile...

Read More thumbnail image: Development and validation of a highperformance liquid chromatography method for the quantification of talazoparib in rat plasma Application to plasma protein binding studies

Application of headspace solid‐phase microextraction followed by gas chromatography coupled with mass spectrometry to determine esters of carboxylic acids and other volatile compounds in Dermestes maculatus and Dermestes ater lipids

Published: Aug 15, 2017

Author(s): Magdalena Cerkowniak, Mieczysława I. Boguś, Emilia Włóka, Piotr Stepnowski, Marek Gołębiowski

Journal: Biomedical Chromatography

Abstract A constant problem in veterinary medicine, human healthcare, agriculture, forestry and horticulture is the large number of pests, and the lack of effective methods to combat them which cause no harm to the rest of the environment. It is recommended and desired to reduce the use of chemicals and increase the use of agents based on knowledge acquired in the fields of biology, chemistry and agrochemicals. To learn the defense...

Read More thumbnail image: Application of headspace solidphase microextraction followed by gas chromatography coupled with mass spectrometry to determine esters of carboxylic acids and other volatile compounds in Dermestes maculatus and Dermestes ater lipids

Chromatographic HPV‐16 E6/E7 plasmid vaccine purification employing L‐histidine and 1‐benzyl‐L‐histidine affinity ligands

Published: Aug 14, 2017

Author(s): Lúcia F. A. Amorim, Rita Gaspar, Patrícia Pereira, Urh Černigoj, Fani Sousa, João António Queiroz, Ângela Sousa

Journal: ELECTROPHORESIS

Affinity chromatography based on amino acids as interacting ligands was already indicated as an alternative compared to ion exchange or hydrophobic interaction for plasmid DNA purification. Understanding the recognition mechanisms occurring between histidine‐based ligands and nucleic acids enables more efficient purification of a DNA vaccine, as the binding and elution conditions can be adjusted in order to enhance the purification...

Read More thumbnail image: Chromatographic HPV16 E6E7 plasmid vaccine purification employing Lhistidine and 1benzylLhistidine affinity ligands
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