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Annual banned‐substance review: Analytical approaches in human sports drug testing

Published: Jan 6, 2019

Author(s): Mario Thevis, Tiia Kuuranne, Hans Geyer

Journal: Drug Testing and Analysis

Abstract A number of high profile revelations concerning anti‐doping rule violations over the past 12 months have outlined the importance of tackling prevailing challenges and reducing the limitations of the current anti‐doping system. At this time, the necessity to enhance, expand, and improve analytical test methods in response to the substances outlined in the World Anti‐Doping Agency (WADA) Prohibited List represents an...

Read More thumbnail image: Annual bannedsubstance review Analytical approaches in human sports drug testing

Evaluation of an on‐site test device for the heroin metabolite 6‐acetylmorphine in urine

Published: Jan 6, 2019

Author(s): Fabian Picht, Olof Beck, Michael Böttcher

Journal: Drug Testing and Analysis

Abstract Detection of heroin use is an important task in clinical drug testing and can be best performed by using 6‐acetylmorphine as the target analyte. This study was performed to evaluate an on‐site test for 6‐acetylmorphine screening in urine with an assigned cut‐off limit at 10 ng/mL. The reference method was a forensic accredited liquid chromatography–tandem mass spectrometry method. The study confirmed that negative...

Read More thumbnail image: Evaluation of an onsite test device for the heroin metabolite 6acetylmorphine in urine

The use of hair as a long‐term indicator of low‐dose β 2 agonist treatments in cattle: Implications for growth‐promoting purposes monitoring

Published: Jan 6, 2019

Author(s): Jia Liu, Chaohua Tang, Ruijun Long, Kai Zhang, Yunsheng Han, Qingyu Zhao, Hongliang Wang, Fuzhong Zhao, Qingshi Meng, Junmin Zhang

Journal: Drug Testing and Analysis

Abstract The objective of this study was to assess the feasibility of using hair as a long‐term indicator of cocktail (low‐dose β2 agonists) treatments in cattle. Six male Simmental cattle were treated with a mixture of low‐dose clenbuterol, ractopamine, and salbutamol at dosages of 5.3, 223.3, and 50.0 μg/kg, respectively. The trial lasted for 112 days and included 28 days of treatment and 84 days of withdrawal. Plasma and...

Read More thumbnail image: The use of hair as a longterm indicator of lowdose  2 agonist treatments in cattle Implications for growthpromoting purposes monitoring

Raman analysis of strained graphene grown on dewetted cobalt

Published: Jan 6, 2019

Author(s): Giampiero Amato, Federico Beccaria, Elisabetta Landini, Ettore Vittone

Journal: Journal of Raman Spectroscopy

Abstract Graphene grows onto cobalt by means of diffusion of carbon atoms during the isothermal stage of exposure to hydrocarbon precursor, followed by precipitation during cooling. This method, largely applied with nickel catalyst, is known to produce continuous, but not uniform, layers with the concurrent presence of mono‐ and poly‐graphene areas. With the aid of Raman mapping of graphene still lying onto its catalyst, we are able...

Read More thumbnail image: Raman analysis of strained graphene grown on dewetted cobalt

Chemical study of degradation processes in ancient metallic materials rescued from underwater medium

Published: Jan 6, 2019

Author(s): Estefania Estalayo, Julene Aramendia, José Manuel Matés Luque, Juan Manuel Madariaga

Journal: Journal of Raman Spectroscopy

Abstract Underwater Cultural Heritage understands all traces of human existence having a cultural, historical, or archaeological character, which have been partially or totally underwater, in periodic or continuous forms for at least 100 years, according to UNESCO. This work is focused on two pieces extracted in 1999 from a shipwreck located in Bakio (Basque Country, Northern Spain). The two analyzed pieces were an iron anchor...

Read More thumbnail image: Chemical study of degradation processes in ancient metallic materials rescued from underwater medium

Analysis of platelets in hypertensive and normotensive individuals using Raman and Fourier transform infrared‐attenuated total reflectance spectroscopies

Published: Jan 6, 2019

Author(s): Diana L. García‐Rubio, M. B Mora, Isidro Badillo‐Ramírez, Doris Cerecedo, José M. Saniger, José Luis Benítez‐Benítez, M. Villagrán‐Muniz

Journal: Journal of Raman Spectroscopy

Abstract Platelets of both healthy and hypertensive subjects were analyzed by Raman and Fourier transform infrared by attenuated total reflectance (FTIR‐ATR) spectroscopies. We compared the average relative intensities of the main Raman peaks, the areas of convoluted bands in the amide I region, and the second derivative of the FTIR‐ATR spectra. Key differences were found in the bands reflecting lipid content and protein structure....

Read More thumbnail image: Analysis of platelets in hypertensive and normotensive individuals using Raman and Fourier transform infraredattenuated total reflectance spectroscopies

Dissipation dynamics of intrachain exciton coupled with phonons in MEH‐PPV: Time‐resolved multiplex coherent anti‐Stokes Raman scattering

Published: Jan 6, 2019

Author(s): Jiao Wang, Quan Wang, Wenyan Wang, Lin Wang, Zhihui Kang, Yanqiang Yang, Hanzhuang Zhang, Yinghui Wang

Journal: Journal of Raman Spectroscopy

Abstract Time‐resolved coherent anti‐Stokes Raman spectroscopy can disentangle the exciton energy dissipation (EED) dynamics of the intrachain exciton in conjugated polymers (MEH‐PPV) coupled with several phonon modes and the corresponding phonon relaxation dynamics by adjusting the timing between lasers in the coherent anti‐Stokes Raman spectroscopy system. The intrachain EED process is coupled with phonon modes located at 966;...

Read More thumbnail image: Dissipation dynamics of intrachain exciton coupled with phonons in MEHPPV Timeresolved multiplex coherent antiStokes Raman scattering

Preparation of a monolithic column with a mixed‐mode stationary phase of reversed‐phase/hydrophilic interaction for capillary liquid chromatography

Published: Jan 4, 2019

Author(s): Meng Zhang, Li Gong, Guizhen Liu, Jingwu Kang

Journal: Journal of Separation Science

Abstract A monolithic capillary column with a mixed‐mode stationary phase of reversed‐phase/hydrophilic interaction chromatography was prepared for capillary liquid chromatography. The monolith was created by an in‐situ copolymerization of a homemade monomer N,N‐dimethyl‐N‐acryloxyundecyl‐N‐(3‐sulfopropyl) ammonium betaine and a crosslinker pentaerythritol triacrylate in a binary porogen agent consisting of methanol and isopropanol....

Read More thumbnail image: Preparation of a monolithic column with a mixedmode stationary phase of reversedphasehydrophilic interaction for capillary liquid chromatography

Incorporation of metal‐organic framework amino‐modified MIL‐101 into glycidyl methacrylate monoliths for nano LC separation

Published: Jan 4, 2019

Author(s): Héctor Martínez Pérez‐Cejuela, Enrique Javier Carrasco‐Correa, Ahmed Shahat, Ernesto F. Simó‐Alfonso, José Manuel Herrero‐Martínez

Journal: Journal of Separation Science

Abstract Metal‐organic frameworks consisting of amino‐modified MIL‐101(M: Cr, Al, and Fe) crystals have been synthesized and subsequently incorporated to glycidyl methacrylate monoliths to develop novel stationary phases for nano‐liquid chromatography. Two incorporation approaches of these materials in monoliths were explored. The metal‐organic framework materials were firstly attached to the pore surface through reaction of epoxy...

Read More thumbnail image: Incorporation of metalorganic framework aminomodified MIL101 into glycidyl methacrylate monoliths for nano LC separation

Fabrication of boron‐rich multiple monolithic fibers for the solid‐phase microextraction of carbamate pesticide residues in complex samples

Published: Jan 4, 2019

Author(s): Jiangyi Wu, Meng Mei, Xiaojia Huang

Journal: Journal of Separation Science

Abstract To enrich carbamate pesticides from complex matrices, an adsorbent based on poly (vinylboronic anhydride pyridine complex‐co‐ethylenedimethacrylate) monolith was fabricated and utilized as the extraction phase of multiple monolithic fiber solid‐phase microextraction. Due to the abundant boron atoms in the monolith, the B–N coordination interaction between adsorbent and analytes play a key role in the efficient extraction of analytes....

Read More thumbnail image: Fabrication of boronrich multiple monolithic fibers for the solidphase microextraction of carbamate pesticide residues in complex samples

Preparation of restricted‐access material precolumns by grafting δ‐gluconolactone onto a hybrid silica monolithic column for on‐line solid‐phase extraction of tetracycline residues from milk

Published: Jan 4, 2019

Author(s): Li‐Fei Huang, Bo Jia, Lin Jiang, Wei‐Lun Liu, Li‐Ya Xia, Yun‐Kai Lv

Journal: Journal of Separation Science

Abstract A restricted‐access material–hybrid monolithic column was prepared based on single‐component organosiloxane and dynamic grafting of δ‐gluconolactone for on‐line solid phase extraction of tetracycline antibiotic residues from milk. The hybrid monolithic column was prepared in a stainless‐steel chromatographic column using methyltrimethoxysilane as the single precursor. δ‐Gluconolactone was covalently coupled to aminopropyl...

Read More thumbnail image: Preparation of restrictedaccess material precolumns by grafting gluconolactone onto a hybrid silica monolithic column for online solidphase extraction of tetracycline residues from milk

Highly selective separation and purification of chicoric acid from Echinacea purpurea by quality control methods in macroporous adsorption resin column chromatography

Published: Jan 4, 2019

Author(s): Yidan Bai, Jian Ma, Wanfang Zhu, Lei Wang, Wei Qu, Shengzhi Su, Weiwei Zhai, Feng Feng, Wenyuan Liu, Jie Zhang

Journal: Journal of Separation Science

Abstract Chicoric acid is the main phenolic active ingredient in Echinacea purpurea (Asteraceae), best known for its immune‐enhancing ability, as well as used as a herbal medicine. To achieve further utilization of medicinal ingredients from E. purpurea, an efficient preparative separation of chicoric acid was developed based on macroporous adsorption resin chromatography. The separation characteristics of several different typical macroporous...

Read More thumbnail image: Highly selective separation and purification of chicoric acid from Echinacea purpurea by quality control methods in macroporous adsorption resin column chromatography

Thermoresponsive hydrophobic copolymer grafted on agar microspheres for all‐aqueous bioseparations

Published: Jan 4, 2019

Author(s): Rui Zhang, Yongqin Lv, Tianwei Tan

Journal: Journal of Separation Science

Abstract Agar microspheres were prepared by water–oil emulsification and cross‐linked under alkaline condition. The thermoresponsive hydrophobic copolymer, poly(N‐isopropylacrylamide‐co‐lauryl methacrylate‐co‐acrylamide), was grafted on the agar microspheres via atom transfer radical polymerization. The agar microspheres grafted with copolymers were characterized by light microphotography, elemental analysis, Fourier transform infrared...

Read More thumbnail image: Thermoresponsive hydrophobic copolymer grafted on agar microspheres for allaqueous bioseparations

Controlling selectivity of polymer‐based monolithic stationary phases

Published: Jan 4, 2019

Author(s): Martina Komendová, Luiz Fernando Ribeiro, Jiří Urban

Journal: Journal of Separation Science

Abstract In this work, we aimed to prepare a monolithic capillary column that allowed an isocratic separation of ten dopamine precursors and metabolites in a single run. Segments of five zwitterion sulfobetaine polymer monoliths have been modified by zwitterion phoshorylcholine by using an ultraviolet‐initiated two‐step photografting. Columns with 0, 33, 50, 66, and 100% of modified length were prepared. Effect of length of the...

Read More thumbnail image: Controlling selectivity of polymerbased monolithic stationary phases

Determination of acidic drugs in biological and environmental matrices by membrane‐based dual emulsification liquid‐phase microextraction followed by high‐performance liquid chromatography

Published: Jan 4, 2019

Author(s): Peyman Moradi, Alireza Asghari

Journal: Journal of Separation Science

Abstract A simple method is introduced providing a highly clean microextraction for the determination of some anti‐inflammatory drugs as the model analytes in human urine and environmental matrices. This method is based upon the implementation of two consecutive emulsification liquid‐phase microextractions, which are separated by a syringe filtration step. In this method, the organic extraction solvent (dihexyl ether) is dispersed...

Read More thumbnail image: Determination of acidic drugs in biological and environmental matrices by membranebased dual emulsification liquidphase microextraction followed by highperformance liquid chromatography

Validation of analytical method for furan determination in eight food matrices and its levels in various foods

Published: Jan 4, 2019

Author(s): Soo‐Young Jeong, Hae Won Jang, Trishna Debnath, Kwang‐Geun Lee

Journal: Journal of Separation Science

Abstract In this study, an automated solid‐phase microextraction coupled with gas chromatography and mass spectrometry method was developed and validated for the determination of furan in eight matrices including ham, milk, apple juice, rice porridge, peanut butter, flatfish, tuna (canned) and seaweed. The calibration curves were highly linear (r2 > 0.990) and the limit of detection and limit of quantification ranged from 0.01−0.02...

Read More thumbnail image: Validation of analytical method for furan determination in eight food matrices and its levels in various foods

Rapid method for simultaneous determination of ascorbic acid and zinc in effervescent tablets by capillary zone electrophoresis with contactless conductivity detection

Published: Jan 4, 2019

Author(s): Michelle Miranda A. C. Ribeiro, Aliceana A. Prado, Alex Domingues Batista, Rodrigo Alejandro Abarza Munoz, Eduardo Mathias Richter

Journal: Journal of Separation Science

Abstract Ascorbic acid and zinc are essential nutrients that play important roles in nutrition, immune support, and maintenance of health. For this reason, both compounds are widely used as ingredients in dietary supplements. We report, for the first time, an analytical method for fast simultaneous determination of ascorbic acid and zinc. A single analysis run is possible every 80 s (45 injections/h). The method is based on...

Read More thumbnail image: Rapid method for simultaneous determination of ascorbic acid and zinc in effervescent tablets by capillary zone electrophoresis with contactless conductivity detection

Metabolic profiles and pharmacokinetics of Qingre Xiaoyanning capsule, a traditional Chinese medicine prescription of Sarcandrae Herba, in rats by UHPLC coupled with quadrupole time‐of‐flight tandem mass spectrometry

Published: Jan 4, 2019

Author(s): Pei Lin, Yi Dai, Zhihong Yao, Zifei Qin, Liangliang He, Qiyi Wang, Zhuochun Wei, Yezi Zhang, Xinsheng Yao

Journal: Journal of Separation Science

Abstract Qingre Xiaoyanning capsule is a famous traditional Chinese medicine prescription which consisted of Sarcandrae Herba (also named Caoshanhu in China) water extract for the frequent treatment of inflammation and immunity related diseases. Until now, the in vivo bioactive components of Qingre Xiaoyanning capsule have not yet been fully addressed. In this study, a total of 42 xenobiotics including 20 prototypes and 22...

Read More thumbnail image: Metabolic profiles and pharmacokinetics of Qingre Xiaoyanning capsule a traditional Chinese medicine prescription of Sarcandrae Herba in rats by UHPLC coupled with quadrupole timeofflight tandem mass spectrometry

Preparative separation of the flavonoid fractions from Periploca forrestii Schltr. ethanol extracts using macroporous resin combined with HPLC analysis and evaluation of their biological activities

Published: Jan 4, 2019

Author(s): Huaguo Chen, Qian Liang, Xin Zhou, Xinyue Wang

Journal: Journal of Separation Science

Abstract A preparative separation method using macroporous absorptive resin coupled with high‐performance liquid chromatography was developed for the separation of six fractions of the 80% ethanol extract of Periploca forrestii Schltr. The six ethanol fractions (5–95; A, B, C, D, E, and F) obtained were carefully analyzed to locate the corresponding peaks in the high‐performance liquid chromatography chromatogram of the total extract, which was...

Read More thumbnail image: Preparative separation of the flavonoid fractions from Periploca forrestii Schltr_ ethanol extracts using macroporous resin combined with HPLC analysis and evaluation of their biological activities

Metabolomic prostate cancer fields in HRMAS MRS‐profiled histologically benign tissue vary with cancer status and distance from cancer

Published: Jan 4, 2019

Author(s): Sarah S. Dinges, Lindsey A. Vandergrift, Shulin Wu, Yannick Berker, Piet Habbel, Matthias Taupitz, Chin‐Lee Wu, Leo L. Cheng

Journal: NMR in Biomedicine

In this article, we review the state of the field of high resolution magic angle spinning MRS (HRMAS MRS)‐based cancer metabolomics since its beginning in 2004; discuss the concept of cancer metabolomic fields, where metabolomic profiles measured from histologically benign tissues reflect patient cancer status; and report our HRMAS MRS metabolomic results, which characterize metabolomic fields in prostatectomy‐removed cancerous prostates....

Read More thumbnail image: Metabolomic prostate cancer fields in HRMAS MRSprofiled histologically benign tissue vary with cancer status and distance from cancer
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