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Effects of elevated levels of lead in ceramics on provenancing studies using non‐destructive PXRF: a case study in Byzantine Cypriot glazed ceramics
Published: Jul 29, 2013
Author(s): Nicola Forster, Peter Grave
Journal: X-Ray Spectrometry
Glazed ceramics are ubiquitous in the medieval archaeological record in the Mediterranean. The effects of lead volatilisation during firing of glazed ceramics on non‐destructive PXRF (portable X‐ray fluorescence) are evaluated using 25 Byzantine Cypriot glazed ceramics. Significant spectral interferences reduce the number of discriminating elements for multivariate statistical analysis, limiting the capacity of non‐destructive PXRF to...
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High‐performance liquid chromatographic enantioseparation of naphthol‐substituted tetrahydroisoquinolines on polysaccharide‐based chiral stationary phases
Published: Jul 29, 2013
Author(s): István Ilisz, Zsanett Gecse, István Szatmári, Ferenc Fülöp, Antal Péter
Journal: Biomedical Chromatography
ABSTRACT The stereoisomers of 15 naphthol‐substituted tetrahydroisoquinoline analogs were separated on chiral stationary phases containing the chiral selectors cellulose tris‐(3,5‐dimethylphenyl carbamate) (Cellulose 1), cellulose tris‐(3‐chloro‐4‐methylphenyl carbamate) (Cellulose 2), cellulose tris‐(4‐methylbenzoate) (Cellulose 3) and cellulose tris‐(4‐chloro‐3‐methylphenyl carbamate) (Cellulose 4). Experiments were performed in normal‐phase mode with...
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Liquid chromatography–tandem mass spectrometry of porphyrins and porphyrinogens in biological materials: separation and identification of interfering poly(ethylene) glycol by travelling wave ion mobility spectrometry/tandem mass spectrometry
Published: Jul 29, 2013
Author(s): Christopher M. Benton, Chang Kee Lim, Caje Moniz, Donald J. L. Jones
Journal: Biomedical Chromatography
ABSTRACT Biological and clinical samples for porphyrin and porphyrinogen analyses by liquid chromatography–tandem mass spectrometry (LC‐MS/MS) are often contaminated with poly(ethylene)glycol (PEG), which complicates the interpretation of mass spectra and characterisation of new porphyrin metabolites. Two contaminating PEG molecules (m/z 833 and m/z 835) were completely separated from uroporphyrin I (m/z 831) by travelling wave ion mobility...
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In vivo GABA T 2 determination with J ‐refocused echo time extension at 7 T
Published: Jul 26, 2013
Author(s): A. Andreychenko, D. W. J. Klomp, R. A. Graaf, P. R. Luijten, V. O. Boer
Journal: NMR in Biomedicine
A method to measure the T2 relaxation time of GABA with spectral editing techniques is proposed. Spectral editing techniques can be used to unambiguously extract signals of low concentration J‐coupled spins such as γ‐aminobutyric acid (GABA) from overlapping resonances such as creatine and macromolecules. These sequences, however, generally have fixed and relatively long echo times. Therefore, for the absolute quantification of the edited spectrum, ...
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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...
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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...
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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...
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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 ...
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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...
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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...
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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...
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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...
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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,...
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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...
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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)...
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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...
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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...
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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...
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Chemical effects of high‐resolution Yb Lγ 4 emission spectra: a possible probe for chemical analysis
Published: Jul 23, 2013
Author(s): Hisashi Hayashi, Noriko Kanai, Naomi Kawamura, Yasuhiro H. Matsuda, Kentaro Kuga, Satoru Nakatsuji, Tetsuro Yamashita, Shigeo Ohara
Journal: X-Ray Spectrometry
An ‘eccentric’ X‐ray emission, YbLγ4, was measured for Yb metal, Yb2O3, YbF3, β‐YbAlB4, YbNi3Al9, and YbNi3Ga9 with a resolution of ~0.9 eV. Peak splitting of the YbLγ4 line was observed in all the recorded spectra and was attributed to the two components originating from the LS coupling of the Yb5p hole, the Yb5p1/2 (LIOII: Lγ4′) and Yb5p3/2 components (LIOIII: Lγ4). The spectra were substantially different depending on the chemical environment of Yb. The position of the...
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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...
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