EarlyView Articles
The very latest articles from the scientific literature
on Wiley Online Library...
You can keep up-to date on these EarlyView articles, which focus on spectroscopy
and separation science:
Please check back soon.
Earlyview RSS Feed
rssFilter by Journal
Automated transfer and injection of hyperpolarized molecules with polarization measurement prior to in vivo NMR
Published: Jul 25, 2013
Author(s): Tian Cheng, Mor Mishkovsky, Jessica A. M. Bastiaansen, Olivier Ouari, Patrick Hautle, Paul Tordo, Ben Brandt, Arnaud Comment
Journal: NMR in Biomedicine
Hyperpolarized magnetic resonance via dissolution dynamic nuclear polarization necessitates the transfer of the hyperpolarized molecules from the polarizer to the imager prior to in vivo measurements. This process leads to unavoidable losses in nuclear polarization, which are difficult to evaluate once the solution has been injected into an animal. We propose a method to measure the polarization of the hyperpolarized molecules inside the...
Read More
Reliable chemical exchange saturation transfer imaging of human lumbar intervertebral discs using reduced‐field‐of‐view turbo spin echo at 3.0 T
Published: Jul 25, 2013
Author(s): Qi Liu, Ning Jin, Zhaoyang Fan, Yutaka Natsuaki, Wafa Tawackoli, Gadi Pelled, Hyun Bae, Dan Gazit, Debiao Li
Journal: NMR in Biomedicine
The reduced field‐of‐view (rFOV) turbo‐spin‐echo (TSE) technique, which effectively suppresses bowel movement artifacts, is developed for the purpose of chemical exchange saturation transfer (CEST) imaging of the intervertebral disc (IVD) in vivo. Attempts to quantify IVD CEST signals in a clinical setting require high reliability and accuracy, which is often compromised in the conventionally used technique. The proposed rFOV TSE CEST method...
Read More
Validation of isotope dilution surface‐enhanced Raman scattering (IDSERS) as a higher order reference method for clinical measurands employing international comparison schemes
Published: Jul 25, 2013
Author(s): Sabine Zakel, Stefan Wundrack, Gavin O'Connor, Bernd Güttler, Rainer Stosch
Journal: Journal of Raman Spectroscopy
Isotope dilution surface‐enhanced Raman scattering (IDSERS) was established as a higher order reference measurement method for clinical measurands in international comparison schemes and in direct comparison with established mass spectrometric methods. IDSERS represents the most accurate and precise quantitative Raman technique and is capable of providing SI‐traceable amount‐of‐substance measurements. IDSERS has now been validated by...
Read More
Pharmacokinetic and tissue distribution of paclitaxel in rabbits assayed by LC‐UV after intravenous administration of its novel liposomal formulation
Published: Jul 25, 2013
Author(s): Yumeng Wei, Zhengkai Xue, Yun Ye, Peng Wang, Yu Huang, Ling Zhao
Journal: Biomedical Chromatography
ABSTRACT A simple, rapid and sensitive LC‐UV method was developed and validated for the determination of paclitaxel (PTX) in rabbit plasma and tissues. A 2 mL aliquot of acetonitrile and 10 μL ammonium acetate (pH 5.0, 6 m) as extraction agents were used to markedly increase the extraction recoveries and greatly reduce the endogenous substances. The separation was achieved on a C18 column at 30 °C using an acetonitrile–ammonium acetate buffer...
Read More
High‐performance liquid chromatography tandem mass spectrometry method for the determination of 2CC‐NBOMe and 25I‐NBOMe in human serum
Published: Jul 25, 2013
Author(s): Justin L. Poklis, Jezelle Charles, Carl E. Wolf, Alphonse Poklis
Journal: Biomedical Chromatography
ABSTRACT 2CC‐NBOMe {4‐chloro‐2,5‐dimethoxyphenethyl‐N‐[(2‐methoxyphenyl) methyl] ethanamine} and 25I‐NBOMe {2‐(4‐iodo‐2,5‐dimethoxyphenyl)‐N‐[(2‐methoxyphenyl) methyl] ethanamine} are of a class of N‐benzyl phenethylamine derivatives whose synthesis was first reported in the scientific literature in 2011. Recent reports from ‘personal drug experience websites’ and in the popular press indicate these drugs are the latest in a series of designer ...
Read More
In vivo three‐dimensional molecular imaging with Biosensor Imaging of Redundant Deviation in Shifts (BIRDS) at high spatiotemporal resolution
Published: Jul 24, 2013
Author(s): Daniel Coman, Robin A. Graaf, Douglas L. Rothman, Fahmeed Hyder
Journal: NMR in Biomedicine
Spectroscopic signals which emanate from complexes between paramagnetic lanthanide (III) ions (e.g. Tm3+) and macrocyclic chelates (e.g. 1,4,7,10‐tetramethyl‐1,4,7,10‐tetraazacyclododecane‐1,4,7,10‐tetraacetate, or DOTMA4–) are sensitive to physiology (e.g. temperature). Because nonexchanging protons from these lanthanide‐based macrocyclic agents have relaxation times on the order of a few milliseconds, rapid data acquisition is possible with chemical shift...
Read More
Evaluation of the oligosaccharide composition of commercial follicle stimulating hormone preparations
Published: Jul 24, 2013
Author(s): Angela Lombardi, Concetta Andreozzi, Vincenzo Pavone, Valeria Triglione, Luca Angiolini, Paolo Caccia
Journal: ELECTROPHORESIS
Glycosylation is an important PTM in proteins, and it is of paramount importance for the manufacture and efficacy of therapeutic glycoproteins. The elucidation of the glycosylation patterns is greatly hampered by the structural heterogeneity, which involves the oligosaccharide moieties, and sometimes also the protein chain. Several strategies are used to map the glycosylation state of glycoproteins: they generally involve analysis of the...
Read More
Challenging the limits of detection of sialylated T homsen– F riedenreich antigens by in‐gel deglycosylation and nano‐ LC ‐ MALDI ‐ TOF ‐ MS
Published: Jul 24, 2013
Author(s): Andreia Almeida, José A. Ferreira, Filipe Teixeira, Catarina Gomes, M. Natália D. S. Cordeiro, Hugo Osório, Lúcio Lara Santos, Celso A. Reis, Rui Vitorino, Francisco Amado
Journal: ELECTROPHORESIS
The identification of sialylated Thomsen–Friedenreich antigens in proteins poses much interest in the context of cancer research. MALDI‐TOF‐MS is a powerful technique for this purpose; still it shows considerable low sensitivity for sialylated molecules due to in‐source and metastable decomposition. Herein, we report a target‐driven strategy to identify these antigens in minute amounts of glycoproteins isolated in polyacrylamide gels. The...
Read More
LC‐MS 3 quantification of O ‐glycopeptides in human serum
Published: Jul 24, 2013
Author(s): Miloslav Sanda, Petr Pompach, Julius Benicky, Radoslav Goldman
Journal: ELECTROPHORESIS
Quantitative analysis of site‐specific glycosylation of proteins is a challenging part of glycoproteomic research. Multiple enrichment steps are typically required in the analytical workflows to achieve adequate characterization of the site‐specific glycoforms. In spite of recent advances, quantitative workflows need further development. Here, we report a selective and sensitive MS2 followed by further fragmentation in the linear IT‐MS...
Read More
Imaging mass spectrometry for assessing temporal proteomics: Analysis of calprotectin in Acinetobacter baumannii pulmonary infection
Published: Jul 24, 2013
Author(s): Jessica L. Moore, Kyle W. Becker, Joshua J. Nicklay, Kelli L. Boyd, Eric P. Skaar, Richard M. Caprioli
Journal: PROTEOMICS
Imaging MS is routinely used to show spatial localization of proteins within a tissue sample and can also be employed to study temporal protein dynamics. The antimicrobial S100 protein calprotectin, a heterodimer of subunits S100A8 and S100A9, is an abundant cytosolic component of neutrophils. Using imaging MS, calprotectin can be detected as a marker of the inflammatory response to bacterial challenge. In a murine model of Acinetobacter...
Read More
Experimental study of the efficiency of a SDD X‐ray detector by means of PIXE spectra
Published: Jul 24, 2013
Author(s): S. Limandri, G. Bernardi, S. Suárez
Journal: X-Ray Spectrometry
The efficiency of a silicon drift detector with ultrathin window was studied for energies between 0.27 and 25 keV. Experimental values of the X‐ray yields from samples of known stoichiometry were obtained by impact of 2 MeV protons. By using theoretical calculations of these yields the relative efficiency of the detector was evaluated. The results are compared with efficiency values obtained from the window transmission and the detector...
Read More
A platform for fast screening potential anti‐breast cancer compounds in traditional Chinese medicines
Published: Jul 24, 2013
Author(s): Zhang‐xiao Peng, Yan Wang, Xue Gu, Yuan‐yuan Wen, Chao Yan
Journal: Biomedical Chromatography
ABSTRACT Several Chinese herbs, namely, Pu‐Gong‐Ying, Gan‐Cao, Chai‐Hu, Mu‐Xiang, Gua‐Lou and Huang‐Yao‐Zi, are frequently used in complex traditional Chinese medicing formulas for breast hyperplasia and breast tumor therapy. The pharmacological effects of these Chinese herbs are all described as ‘clearing heat‐toxin and resolving masses’ in traditional use. However, the chemical profiles of anti‐breast cancer constituents in these...
Read More
Enantiomeric separation of meptazinol and its three intermediate enantiomers by capillary electrophoresis: quantitative analysis of meptazinol in pharmaceutical formulations
Published: Jul 24, 2013
Author(s): Jia Yu, Zhen Jiang, Tiemin Sun, Fenfen Ji, Shuying Xu, Lan Wei, Xingjie Guo
Journal: Biomedical Chromatography
ABSTRACT A new capillary electrophoresis (CE) method using carboxymethyl‐β‐cyclodextrin (CM‐β‐CD) as chiral selector has been developed for the enantiomeric separation of meptazinol and its three intermediate enantiomers (intermediates II–IV), and validated for the application of quantitative determination of meptazinol in tablets. The primary factors affecting the separation efficiency, which include the chiral selector and its concentration,...
Read More
Development and validation of a highly sensitive LC‐MS/MS method for quantitation of bivalirudin in human plasma: application to a human pharmacokinetic study
Published: Jul 24, 2013
Author(s): Dong Chai, Rui Wang, Nan Bai, Yun Cai, Beibei Liang
Journal: Biomedical Chromatography
ABSTRACT A sensitive, specific and simple LC‐MS/MS method was developed for the identification and quantification of bivalirudin in human plasma using diazepam as an internal standard (IS). The API‐4000 LC‐MS/MS was operated under multiple‐reaction monitoring mode using electrospray ionization. The sample preparation consisted of an easy protein precipitation sample pretreatment with methanol. Chromatographic separation was achieved...
Read More
Development and validation of a UPLC‐MS/MS method for the determination of 7‐hydroxymitragynine, a μ ‐opioid agonist, in rat plasma and its application to a pharmacokinetic study
Published: Jul 24, 2013
Author(s): Pradeep K. Vuppala, Seshulatha Jamalapuram, Edward B. Furr, Christopher R. McCurdy, Bonnie A. Avery
Journal: Biomedical Chromatography
ABSTRACT A simple, sensitive and specific ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS) method was developed and validated to determine the concentrations of 7‐hydroxymitragynine in rat plasma. Following a single‐step liquid–liquid extraction of plasma samples using chloroform, 7‐hydroxymitragynine and the internal standard (tryptoline) were separated on an Acquity UPLCTM BEH C18 (1.7 µm, 2.1 × 50 mm)...
Read More
Preparation and characterization of a novel dual‐retention mechanism mixed‐mode stationary phase with PEG 400 and succinic anhydride as ligand for protein separation in WCX and HIC modes
Published: Jul 24, 2013
Author(s): Chao Song, Jianshan Wang, Kailou Zhao, Quan Bai
Journal: Biomedical Chromatography
ABSTRACT A novel dual‐retention mechanism mixed‐mode stationary phase based on silica gel functionalized with PEG 400 and succinic anhydride as the ligand was prepared and characterized by infrared spectra and elemental analysis. Because of the ligand containing PEG 400 and carboxyl function groups, it displayed hydrophobic interaction chromatography (HIC) characteristic in a high‐salt‐concentration mobile phase, and weak cation...
Read More
Legal controls on cannabimimetics: An international dilemma?
Published: Jul 23, 2013
Author(s): L. A. King
Journal: Drug Testing and Analysis
Since early 2009, over 80 illicitly produced synthetic cannabinoid receptor agonists have been notified to the European Monitoring Centre for Drugs and Drug Addiction (EMCDDA). Yet more have been reported in other countries or offered for sale on websites. These cannabinoids typically act as agonists at CB1 receptors, and mimic the effects of Δ9‐tetrahydrocannabinol (THC), the principal psychoactive constituent of Cannabis L. As with other ‘new...
Read More
Drug concentrations in post‐mortem femoral blood compared with therapeutic concentrations in plasma
Published: Jul 23, 2013
Author(s): Terhi Launiainen, Ilkka Ojanperä
Journal: Drug Testing and Analysis
Therapeutic drug concentrations measured in plasma are of limited value as reference intervals for interpretation in post‐mortem (PM) toxicology. In this study, drug concentration distributions were studied in PM femoral venous blood from 57 903 Finnish autopsy cases representing all causes of death during an 11‐year period. Cause‐of‐death information was obtained from death certificates issued by forensic pathologists. Median, mean, and...
Read More
LC/MS/MS analysis of the endogenous dimethyltryptamine hallucinogens, their precursors, and major metabolites in rat pineal gland microdialysate
Published: Jul 23, 2013
Author(s): Steven A. Barker, Jimo Borjigin, Izabela Lomnicka, Rick Strassman
Journal: Biomedical Chromatography
ABSTRACT We report a qualitative liquid chromatography–tandem mass spectrometry (LC/MS/MS) method for the simultaneous analysis of the three known N,N‐dimethyltryptamine endogenous hallucinogens, their precursors and metabolites, as well as melatonin and its metabolic precursors. The method was characterized using artificial cerebrospinal fluid (aCSF) as the matrix and was subsequently applied to the analysis of rat brain pineal...
Read More
A validated HPLC‐PDA method for identification and quantification of two bioactive alkaloids, ephedrine and cryptolepine, in different Sida species
Published: Jul 23, 2013
Author(s): Arnab Chatterjee, Satyanshu Kumar, Sunil K. Chattopadhyay
Journal: Biomedical Chromatography
ABSTRACT A simple, rapid, accurate and reproducible reverse‐phase HPLC method has been developed for the identification and quantification of two alkaloids ephedrine and cryptolepine in different extracts of Sida species using photodiode array detection. Baseline separation of the two alkaloids was achieved on a Waters RP‐18 X‐terra column (250 × 4.6 mm, 5 µm) using a solvent system consisting of a mixture of water containing 0.1%...
Read More
