EarlyView Articles

Ultraperformance convergence chromatography‐high resolution tandem mass spectrometry for lipid biomarker profiling and identification

Published: Sep 29, 2016

Author(s): Jace W. Jones, Claire L. Carter, Fei Li, Jianshi Yu, Keely Pierzchalski, Isabel L. Jackson, Zeljko Vujaskovic, Maureen A. Kane

Journal: Biomedical Chromatography

Abstract Lipids represent biologically ubiquitous and highly dynamic molecules in terms of abundance and structural diversity. Whereas the potential for lipids to inform on disease/injury is promising, their unique characteristics make detection and identification of lipids from biological samples analytically demanding. We report the use of ultraperformance convergence chromatography (UPC2), a variant of supercritical fluid...

Simultaneous determination of pyrroquinazoline alkaloids and flavonoids in Adhatoda beddomei and Adhatoda vasica and their marketed herbal formulations using ultra‐high‐performance liquid chromatography coupled with triple quadrupole linear ion trap mass spectrometry

Published: Sep 29, 2016

Author(s): Awantika Singh, Sunil Kumar, Vikas Bajpai, Brijesh Kumar

Journal: Biomedical Chromatography

Abstract Adhatoda beddomei and Adhatoda vasica leaf, known as ‘Vasaka’ and/or ‘Vasa’ in Ayurveda and ‘Malabar nut’ in English, is an official drug in the Indian Pharmacopoeia. The medicinal properties of these plants are due to the presence of pyrroquinazoline alkaloids. An UHPLC–ESI/MS/MS method in both positive and negative electrospray ionization in multiple‐reaction‐monitoring mode was developed and validated for the estimation of alkaloids...

Selective detection of chloramphenicol in milk based on a molecularly imprinted polymer–surface‐enhanced Raman spectroscopic nanosensor

Published: Sep 29, 2016

Author(s): Yunfei Xie, Mengyao Zhao, Qi Hu, Yuliang Cheng, Yahui Guo, He Qian, Weirong Yao

Journal: Journal of Raman Spectroscopy

In this study, a novel hybrid molecularly imprinted polymer (MIP) with a surface‐enhanced Raman spectroscopy (SERS) sensor was proposed for the detection of chloramphenicol in milk. The MIP was prepared by precipitation polymerization, and the template molecule was extracted by ultrasonic wave. The polymer was placed in a sodium citrate reduction reaction to prepare the chloramphenicol–MIP–Au substrate. The optimal detection conditions...

Aging behavior of dielectric barrier discharge‐modified Twaron fibers in different storage environments

Published: Sep 29, 2016

Author(s): Caixia Jia, Qian Wang, Ping Chen, Qi Yu, Dapeng Li

Journal: Surface and Interface Analysis

The aging behavior of air dielectric barrier discharge plasma treatment was investigated by storing the treated fibers respectively in air and in the oxidizing environment. Based on several testing methods, this study led us to the conclusion that the aging effects in the oxidizing environment were less obvious than that in air. X‐ray photoelectron spectroscopy and Fourier transform infrared spectroscopy indicated that the decay of fiber...

The dispersion of graphene in conductive epoxy composites investigated by Raman spectroscopy

Published: Sep 29, 2016

Author(s): Fanyu Zhao, Liangzhong Ling, Liyan Liu, Amina Zafar, Zhenhua Ni

Journal: Journal of Raman Spectroscopy

The two‐dimensional structure and unique properties make graphene an efficient candidate to strengthen the electrical and mechanical characteristics of polymer composites. The effectiveness for improving the electrical property of composites strongly depends on the size, electrical conductivity and dispersion of graphene fillers in polymer matrix. Here, we demonstrate that Raman spectroscopy can be used to study the dispersion of...

Determination of cannabinoids in hemp nut products in Taiwan by HPLC‐MS/MS coupled with chemometric analysis: quality evaluation and a pilot human study

Published: Sep 29, 2016

Author(s): Chih‐Wei Chang, Chun‐Wei Tung, Chin‐Chuan Tsai, Yu‐Tse Wu, Mei‐Chich Hsu

Journal: Drug Testing and Analysis

Hemp nuts are mature cannabis seeds obtained after shelling and that are commonly used in traditional Chinese medicine for treating functional constipation. In this work, we screened hemp nut products, classified them, and verified the legality of consuming them. A total of 18 products were purchased from Taiwan, China, and Canada. Validated high‐performance liquid chromatography with tandem mass spectrometry methods were developed for...

Adsorption and decomposition of HMX and CL‐20 on Al(111) surface by DFT investigation

Published: Sep 29, 2016

Author(s): Cai‐Chao Ye, Qi An, Si‐Yu Xu, Xue‐Hai Ju

Journal: Surface and Interface Analysis

The adsorption and decomposition of HMX and CL‐20 molecules on the Al(111) surface were investigated by the generalized gradient approximation of density functional theory. The calculations employed a supercell (6 × 6 × 3) slab model and three‐dimensional periodic boundary conditions. The strong attractive forces between HMX (or CL‐20) molecule and Al atoms induce the breaking of N‐O and N‐N bonds in nitro group. Subsequently, the...

Urinary excretion study following consumption of various poppy seed products and investigation of the new potential street heroin marker ATM4G

Published: Sep 29, 2016

Author(s): Alexandra Maas, Michael Krämer, Konrad Sydow, Pai‐Shan Chen, Torsten Dame, Frank Musshoff, Bernd W.K. Diehl, Burkhard Madea, Cornelius Hess

Journal: Drug Testing and Analysis

Discrimination between street heroin consumption and poppy seed ingestion represents a major toxicological challenge in daily routine work. Several difficulties associated with conventional street heroin markers originate from their versatile occurrence in various poppy seed products and medications, respectively, as well as to small windows of detection. A novel opportunity to overcome these hindrances is represented by the new potential...

Urinary human chorionic gonadotropin isoform concentrations in doping control samples

Published: Sep 29, 2016

Author(s): Anthony W. Butch, Getachew A. Woldemariam

Journal: Drug Testing and Analysis

Anti‐doping laboratories routinely use immunoassays to measure urinary concentrations of human chorionic gonadotropin (hCG). To minimize immunoassay differences and false positive screen results from inactive isoforms (free β‐subunit (hCGβ), β‐subunit core fragment (hCGβcf)) laboratories now use intact hCG instead of total hCG immunoassays to measure hCG. To determine the distribution of hCG isoforms in urine, we determined the...

Identification and characterization of N‐tert ‐butoxycarbonyl‐MDMA: a new MDMA precursor

Published: Sep 29, 2016

Author(s): Michael Collins, Christopher Donnelly, Shane Cameron, Mark Tahtouh, Helen Salouros

Journal: Drug Testing and Analysis

In September 2015, 80 litres of a viscous, light‐red liquid, described as hair product, was seized by the Australian Border Force (ABF). Initial testing by ABF indicated that the liquid was the 3,4‐methylenedioxymethamphetamine (MDMA) precursor chemical safrole and custody of the material was transferred to the Australian Federal Police (AFP) who coordinated all subsequent investigations. Initial gas chromatography–mass spectrometry...

Identification of secondary salts and their sources in deteriorated stone monuments using micro‐Raman spectroscopy, SEM‐EDS and XRD

Published: Sep 29, 2016

Author(s): Mariola Marszałek

Journal: Journal of Raman Spectroscopy

Salts crystallisation is a cause of deterioration of stone monuments. Very small sizes of salt crystals, often a multiphase composition and usually low concentrations hamper their identification. Therefore, micro‐Raman spectroscopy, scanning electron microscopy and, in some cases, X‐ray diffraction have been used to identify the salts that crystallised within and on the weathered limestone and sandstone architectonic details of the...

Quantitative analysis of total hydrocarbons and water in oil‐contaminated soils with attenuated total reflection infrared spectroscopy

Published: Sep 29, 2016

Author(s): Alena Guryanova, Vasiliy Ermakov, Vladislav Galyanin, Viacheslav Artyushenko, Tatiana Sakharova, Iskander Usenov, Dmitriy Bykov, Andrey Bogomolov

Journal: Journal of Chemometrics

The feasibility of direct (ie, without sample preparation) quantitative analysis of total hydrocarbons and water in oil‐contaminated soils using mid‐infrared spectroscopy and an attenuated total reflection (ATR) probe has been investigated. Spectral characteristics of unpolluted and oil‐contaminated soils composed of sand, clay, dolomite, and humus have been studied over the full mid‐infrared range (4000‐400 cm−1). Spectra of 25...

Proceedings SaskVal 2015

Published: Sep 29, 2016

Author(s):

Journal: Drug Testing and Analysis

Determination of antibacterial agent tilmicosin in pig plasma by LC/MS/MS and its application to pharmacokinetics

Published: Sep 28, 2016

Author(s): Bing Li, Shi‐Yue Gong, Xu‐Zheng Zhou, Ya‐Jun Yang, Jian‐Yong Li, Xiao‐Juan Wei, Fu‐Sheng Cheng, Jian‐Rong Niu, Xi‐Wang Liu, Ji‐Yu Zhang

Journal: Biomedical Chromatography

Abstract A rapid and sensitive high‐performance liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed and validated to quantify tilmicosin in pig plasma. Plasma samples were prepared by liquid–liquid extraction. Chromatographic separation was achieved on a C18 column (2.1 × 30 mm, 3.5 μm) using acetonitrile–water (90:10, v/v; water included 0.1% formic acid) as the mobile phase. Mass detection was carried out using...

Simultaneous determination of ginsenosides and bufadienolides in rat plasma after the oral administration of Shexiang Baoxin Pill for pharmacokinetic study by liquid chromatography tandem mass spectrometry following solid‐phase extraction

Published: Sep 28, 2016

Author(s): Jianfei Tao, Ling Mao, Bailun Zhou, Qun Liu, Aigang Yang, Guobing Wei, Runhui Liu, Wei‐dong Zhang, Wen Xu, Ji Ye

Journal: Biomedical Chromatography

Abstract A sensitive and reliable bioanalytical method was established for quantitati\ve and pharmacokinetic investigation of nine ginsenosides and seven bufadienolides in rat plasma after the oral administration of Shexiang Baoxin Pill by liquid chromatography–electrospray ionization tandem mass spectrometry, using tinidazole and digoxin as internal standards (ISTDs). All of the analytes and ISTDs obtained satisfactory recoveries...

Determination of MLN0128, an investigational antineoplastic agent, in human plasma by LC–MS/MS

Published: Sep 28, 2016

Author(s): Sandeep R. Kunati, Yan Xu

Journal: Biomedical Chromatography

Abstract MLN0128, an mTOR kinase inhibitor, is currently undergoing clinical investigation for treatment of a variety of cancers. To support this work, an LC–MS/MS method has been developed for the determination of MLN0128 in human plasma. A structural analog STK040263 was used as the internal standard. Both MLN0128 and the IS were first extracted from plasma using methyl tert‐butyl ether; then separated on a Waters XTerra® MS C18 column using...

A UPLC–MS/MS approach for simultaneous determination of eight flavonoids in rat plasma, and its application to pharmacokinetic studies of Fu‐Zhu‐Jiang‐Tang tablet in rats

Published: Sep 28, 2016

Author(s): Yi Tao, Xi Chen, Yanhui Jiang, Baochang Cai

Journal: Biomedical Chromatography

Abstract The purpose of this study is to establish and validate a UPLC–MS/MS approach to determine eight flavonoids in biological samples and apply the method to pharmacokinetic study of Fu‐Zhu‐Jiang‐Tang tablet. A Waters BEH C18 UPLC column was employed with methanol/0.1% formic acid–water as mobile phases. The mass analysis was carried out in a triple quadrupole mass spectrometer using multiple reaction monitoring with negative scan mode. A...

DNA fragment separations by on‐line combination of capillary isotachophoresis–capillary zone electrophoresis with UV detection

Published: Sep 28, 2016

Author(s): Milan Fraňo, Katarína Džuganová, Pavol Koiš, Marián Masár

Journal: ELECTROPHORESIS

A high‐speed DNA fragment separation system based on an on‐line combination of capillary ITP with CZE (CITP‐CZE) and using UV detection at 260 nm was developed. A novel CITP‐CZE buffer system of pH 6.1 was designed for the separation of ten DNA fragments with sizes ranging from 100 to 1000 bp. An effect of underivatized α‐, β‐ and γ‐cyclodextrins on the resolution of DNA fragments in the CZE step of the CITP‐CZE combination was...

Chromatography column comparison and rapid pretreatment for the simultaneous analysis of amantadine, rimantadine, acyclovir, ribavirin, and moroxydine in chicken muscle by ultra high performance liquid chromatography and tandem mass spectrometry

Published: Sep 28, 2016

Author(s): Qiaoyan Zhang, Chaogeng Xiao, Wei Wang, Mingrong Qian, Jie Xu, Hua Yang

Journal: Journal of Separation Science

In this work, a chromatography column comparison and rapid pretreatment development were carried out. A multi‐class method was built based on the quick, easy, cheap, effective, rugged, and safe pretreatment method with hydrophilic interaction ultra high performance liquid chromatography and tandem mass spectrometry for the high‐throughput analysis of five antivirals in chicken muscle. The HSS T3 column, BEH HILIC column and BEH Amide...

Thickness determination of gold layer on pre‐Columbian objects and a gilding frame, combining pXRF and PLS regression

Published: Sep 27, 2016

Author(s): Fabio Lopes, Fabio Luiz Melquiades, Carlos Roberto Appoloni, Roberto Cesareo, Marcia Rizzutto, Tiago F. Silva

Journal: X-Ray Spectrometry

In conservation, restoration and characterization studies of art and archaeological objects, the improvement of analytical techniques is a tendency. X‐ray fluorescence (XRF) is a versatile technique, and it has been widely used in the last decades for characterization of a great variety of materials (metals, glass, paints, inks, ceramics, etc.) applied to cultural heritage studies. Besides the chemical composition, it is possible to infer...