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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...

Read More thumbnail image: Automated transfer and injection of hyperpolarized molecules with polarization measurement prior to in vivo NMR

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 thumbnail image: Reliable chemical exchange saturation transfer imaging of human lumbar intervertebral discs using reducedfieldofview turbo spin echo at 3_0T

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 thumbnail image: Validation of isotope dilution surfaceenhanced Raman scattering IDSERS as a higher order reference method for clinical measurands employing international comparison schemes

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 thumbnail image: Pharmacokinetic and tissue distribution of paclitaxel in rabbits assayed by LCUV after intravenous administration of its novel liposomal formulation

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 thumbnail image: Highperformance liquid chromatography tandem mass spectrometry method for the determination of 2CCNBOMe and 25INBOMe in human serum

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 thumbnail image: In vivo threedimensional molecular imaging with Biosensor Imaging of Redundant Deviation in Shifts BIRDS at high spatiotemporal resolution

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 thumbnail image: Evaluation of the oligosaccharide composition of commercial follicle stimulating hormone preparations

Challenging the limits of detection of sialylated T homsen– F riedenreich antigens by in‐gel deglycosylation and nano‐ LCMALDITOFMS

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 thumbnail image: Challenging the limits of detection of sialylated T homsen F riedenreich antigens by ingel deglycosylation and nano LC  MALDI  TOF  MS

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 thumbnail image: LCMS 3 quantification of O glycopeptides in human serum

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 thumbnail image: Imaging mass spectrometry for assessing temporal proteomics Analysis of calprotectin in Acinetobacter baumannii pulmonary infection

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 thumbnail image: Experimental study of the efficiency of a SDD Xray detector by means of PIXE spectra

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 thumbnail image: A platform for fast screening potential antibreast cancer compounds in traditional Chinese medicines

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 thumbnail image: Enantiomeric separation of meptazinol and its three intermediate enantiomers by capillary electrophoresis quantitative analysis of meptazinol in pharmaceutical formulations

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 thumbnail image: Development and validation of a highly sensitive LCMSMS method for quantitation of bivalirudin in human plasma application to a human pharmacokinetic study

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 thumbnail image: Development and validation of a UPLCMSMS method for the determination of 7hydroxymitragynine a  opioid agonist in rat plasma and its application to a pharmacokinetic study

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 thumbnail image: Preparation and characterization of a novel dualretention mechanism mixedmode stationary phase with PEG 400 and succinic anhydride as ligand for protein separation in WCX and HIC modes

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 thumbnail image: Legal controls on cannabimimetics An international dilemma

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 thumbnail image: Drug concentrations in postmortem femoral blood compared with therapeutic concentrations in plasma

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 thumbnail image: LCMSMS analysis of the endogenous dimethyltryptamine hallucinogens their precursors and major metabolites in rat pineal gland microdialysate

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 thumbnail image: A validated HPLCPDA method for identification and quantification of two bioactive alkaloids ephedrine and cryptolepine in different Sida species
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