Online extraction toxicological MS(n) screening system for serum and heparinized plasma and comparison of screening results between plasma and urine in the context of clinical data

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 24 August 2011Daniel M., Mueller , Katharina M., Rentsch Background: The two main matrices for screening are urine or serum and heparinized pl…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 24 August 2011

Daniel M., Mueller , Katharina M., Rentsch

 Background: The two main matrices for screening are urine or serum and heparinized plasma. Whereas urine has the advantage of usually higher concentrations and longer detection windows, serum or heparinized plasma represent the current systemic drug exposure of a patient. Materials and Methods: An online extraction LC-MSn method using a MS2 and MS3 spectral library for the identification of substances has been developed and validated to screen serum and heparinized plasma. Extraction was performed by online turbulent flow chromatography under alkaline conditions. Chromatographic separation was achieved using a phenyl/hexyl column with acidic eluents. For detection, a linear ion trap, equipped with an APCI...

Gas-chromatography-tandem mass spectrometry assay for the quantification of four benzodiazepines and citalopram in eleven postmortem rabbit fluids and tissues, with application to animal and human samples

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 24 August 2011N., Cartiser , F., Bévalot , C., Le Meur , Y., Gaillard , D., Malicier , …Pharmacokinetic studies and postmortem toxicologic…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 24 August 2011

N., Cartiser , F., Bévalot , C., Le Meur , Y., Gaillard , D., Malicier , ...

Pharmacokinetic studies and postmortem toxicological investigations require a validated analytical technique to quantify drugs on a large number of matrices. Three-step liquid/liquid extraction with online derivatization (silylation) ahead of analysis by gas chromatography-tandem mass spectrometry was developed and validated on rabbit specimens in order to quantify citalopram and 4 benzodiazepines (diazepam, nordazepam, oxazepam and temazepam) in 11 biological matrices (blood, urine, bile, vitreous humor, liver, kidney, skeletal muscle, brain, adipose tissue, bone marrow (BM) and lung). Since the 11 biological matrices came from the same animal species, full validation was performed on 1 matrix, bone marrow (considered the most complex),...

Metabolic Profiling of Urine in Young Obese Men using Ultra Performance Liquid Chromatography and Q-TOF Mass Spectrometry (UPLC/Q-TOF MS)

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Cheng, Wang , Rennan, Feng , Dianjun, Sun , Ying, Li , Xinxin, Bi , …Obesity is currently epidemic in many countries worldwid…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Cheng, Wang , Rennan, Feng , Dianjun, Sun , Ying, Li , Xinxin, Bi , ...

Obesity is currently epidemic in many countries worldwide. In the young adult, obesity often accompanies hyperlipemia, which is strongly related to the occurrence and development of obesity-related chronic diseases such as diabetes mellitus, hypertension and cardiovascular disease. This study investigated the differences in metabolomic profiling between obese (with hyperlipemia, n=30) and normal-weight (n=30) young men. Anthropometric parameters and conventional metabolites were measured. There were no significant differences between obese and normal-weight young men in age, height and fasting plasma glucose level. Obese young men showed increased weight, body mass index, fat mass, systolic blood pressure, and triglyeride, total cholesterol and...

Molecularly imprinted microspheres as SPE sorbent for selective extraction of four Sudan dyes in catsup products

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Fengxia, Qiao , Yuru, Geng , Changqing, He , Yupei, Wu , Pengyu, PanA highly selective molecularly imprinted solid-phase extrac…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Fengxia, Qiao , Yuru, Geng , Changqing, He , Yupei, Wu , Pengyu, Pan

A highly selective molecularly imprinted solid-phase extraction (MISPE) coupled with high performance liquid chromatography (HPLC) ultraviolet-visible detection was developed for the simultaneous isolation and determination of four Sudan dyes (I, II, III and IV) in catsup products. The novel molecularly imprinted microspheres (MIM) were synthesized by aqueous suspension polymerization using phenylamine and naphthol as template, which showed high affinity to Sudan dyes in aqueous solution. In order to develop a selective extraction protocol for simultaneous determination the four Sudan dyes from catsup products, the molecular recognition properties of MIM as a SPE sorbent were evaluated. Under the optimized condition, good...

An LC–MS/MS assay to determine plasma pharmacokinetics of cyclic thymic hexapeptide (cTP6) in rhesus monkeys

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Qingfang, Meng , Zhihang, Chen , Jinjing, Che , Yiping, Lu , Huanzhang, Wang , …A robust and simple method for absolute quant…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Qingfang, Meng , Zhihang, Chen , Jinjing, Che , Yiping, Lu , Huanzhang, Wang , ...

A robust and simple method for absolute quantification of a novel bidirectional immunomodulatory drug candidate, cyclic thymic hexapeptide (cTP6), in rhesus monkey plasma was developed and validated by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Plasma proteins were precipitated by adding four volumes of acetonitrile. Peptides in the supernatant were separated by liquid chromatography on an Agilent Zorbax Eclipse Plus-C18 chromatographic column with gradient elution using 0.1% formic acid in water (mobile phase A) and 0.1% formic acid in methanol (mobile phase B) at 0.2mL/min. The analytes were identified by triple quadrupole mass spectrometry in positive ion-mode. The assay...

Preparation and application of a partially degradable gel in mass spectrometry-based proteomic analysis

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Jian, Zhou , Yongbo, Hu , Yong, Lin , Haipeng, Liu , Peng, XieIn-gel digestion is an attractive route in mass spectrometry-base…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Jian, Zhou , Yongbo, Hu , Yong, Lin , Haipeng, Liu , Peng, Xie

In-gel digestion is an attractive route in mass spectrometry-based proteomic analysis, which, however, often suffers from a certain amount of sample loss mainly due to insufficient protein digestion and peptide extraction. To address this, herein we establish a partially degradable gel-assisted protein digestion and peptide recovery method by means of a simple replacement of bis-acrylamide (BA) with bis-acrylylcystamine (BAC). Concretely, the protein sample solubilized using high concentrations of sodium dodecyl sulfate (SDS) and urea were directly entrapped and immobilized into BAC-crosslinked gel by vacuum-dried gel absorption followed by fixation treatment. After removal of SDS and urea by repeated washing, the...

Hb Riesa or ß93 (F9) Cys –> Ser, a New electrophoretically silent Haemoglobin Variant interfering with haemoglobin A1c measurement

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Emmanuel, Bissé , Agnès, Hovasse , Sabine, Preisler-Adams , Thomas, Epting , Oswald, Wagner , …A new ß variant was found i…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Emmanuel, Bissé , Agnès, Hovasse , Sabine, Preisler-Adams , Thomas, Epting , Oswald, Wagner , ...

A new ß variant was found in a German diabetic patient whose blood samples appeared to contain 45% Hb A1c using Bio-Rad Variant V-II A1c-analyzer but 7.6% on boronate affinity chromatography. Structural studies using, HPLC, mass spectrometry, and the genomic DNA analysis revealed a new substitution in which the cysteine residue at position ß93 was replaced by serine. The variant was named Hb Riesa or ß93 (F9) Cys --> Ser and accounted for 54.3% of the total haemoglobin. This suggests that the protein-synthesis processes for the mutant could be slightly more promoted than those of the wild-type. Hb Riesa is...

Analysis of cantharidin in false blister beetles (Coleoptera: Oedemeridae) by headspace solid-phase microextraction and gas chromatography–mass spectrometry

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Ali, Mehdinia , Mina, Asiabi , Ali, Jabbari , S. Mohammad, AbtahiA headspace solid-phase microextraction (HS-SPME) coupled to ga…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Ali, Mehdinia , Mina, Asiabi , Ali, Jabbari , S. Mohammad, Abtahi

A headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) method was developed to determine a type of terpenoid named as cantharidin in the false blister beetles, family Oedemeridae. The experimental parameters for HS-SPME method were optimized. Six commercial fibers for HS-SPME method development were tested and the divinylbenzene/carboxene/polydimethylsiloxane fiber was selected to provide the best detection of analyzed compound. The calibration curve showed linearity in the range of 0.1-50μgmL−1, correlation coefficient (R2=0.992), limit of detection (0.01ngmL−1) and quantitation (0.04ngmL−1) were obtained for the proposed method. The relative standard deviations of intra-day and inter-day assays were 7.8 and 3.4%,...

Detection and Identification of a Serine to Arginine Sequence Variant in a Therapeutic Monoclonal Antibody

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011Diya, Ren , Jian, Zhang , Ross, Pritchett , Hongbin, Liu , Jennifer, Kyauk , …Sequence variants, also known as unintended ami…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 22 August 2011

Diya, Ren , Jian, Zhang , Ross, Pritchett , Hongbin, Liu , Jennifer, Kyauk , ...

Sequence variants, also known as unintended amino acid substitutions in the protein primary structure, are one of the critical quality attributes needed to be monitored during process development of monoclonal antibodies (mAbs). Here we report on analytical methods for detection and identification of a sequence variant in an IgG1 mAb expressed in Chinese hamster ovary (CHO) cells. The presence of the sequence variant was detected by an imaged capillary isoelectric focusing (ICIEF) assay, showing a new basic species in mAb charge variant profile. The new basic variant was fractionated and enriched by ion-exchange chromatography, analyzed by reduced light and heavy...

Comparative studies of HPLC-fluorometry and LC/MS method for the determination of N-acetylneuraminic acid as a marker of deteriorated ophthalmic solutions

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011Kinya, Iwatsuka , Shin-ichi, Yasueda , Eiji, Bando , Hiroyuki, Fujii , Takashi, Terada , …Methods for determining the deterio…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011

Kinya, Iwatsuka , Shin-ichi, Yasueda , Eiji, Bando , Hiroyuki, Fujii , Takashi, Terada , ...

Methods for determining the deterioration of ophthalmic solutions using both high-performance liquid chromatography (HPLC) with fluorescence detection and liquid chromatography coupled with selected ion monitoring mass spectrometry (LC/MS) are described. The methods are based on the determination of N-acetylneuraminic acid (NeuAc) released by the hydrolysis of foreign bodies that contaminate eye drops during use. The released NeuAc was either labeled with 1,2-diamino-4,5-methylenedioxybenzene (DMB) for fluorometric detection or detected without derivatization by mass spectrometry. The calibration curves for NeuAc showed good linearity between 1.2ng/mL and 39ng/mL for fluorometric HPLC and 5.0ng/mL and 100ng/mL for LC/MS, respectively. Detection limits for fluorometric HPLC...

High-throughput comprehensive analysis of D- and L-amino acids using ultra-high performance liquid chromatography with a circular dichroism (CD) detector and its application to food samples

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011Sachise, Eto , Mai, Yamaguchi , Masao, Bounoshita , Toshimi, Mizukoshi , Hiroshi, MiyanoA rapid and comprehensive analytical me…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011

Sachise, Eto , Mai, Yamaguchi , Masao, Bounoshita , Toshimi, Mizukoshi , Hiroshi, Miyano

A rapid and comprehensive analytical method for D- and L-enantiomers of proteinogenic amino acids was developed using ultra-high performance liquid chromatography (UHPLC) equipped with a circular dichroism (CD) detector. Pre-column derivatization reagents were examined for enhanced sensitivity and selectivity for UV and CD detection: 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) was selected. The method, using a CD detector, does not require separation of optical isomers on a column to calculate the enantio ratio (%D) using the g-factor value and produces a simple chromatogram in comparison to other reported methods. Using this advantage, combined with UHPLC technology, analysis time for the derivatized proteinogenic amino acids...

Comparison of molecular dynamics simulation methods for amyloid β1–42 monomers containing d-aspartic acid residues for predicting retention times in chromatography

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011Akifumi, Oda , Kana, Kobayashi , Ohgi, TakahashiMolecular dynamics simulations of amyloid β1–42 containing d-aspartic acid res…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 17 August 2011

Akifumi, Oda , Kana, Kobayashi , Ohgi, Takahashi

Molecular dynamics simulations of amyloid β1–42 containing d-aspartic acid residues were performed using several continuous solvent models to investigate the usefulness of simulation methods for d-amino acid-containing proteins and peptides. Normal molecular dynamics simulations and replica exchange molecular dynamics simulations, which are one of the generalized-ensemble algorithms, were performed. Because the β-structure contents of amyloid β1–42 peptides obtained by replica exchange molecular dynamics simulations with Onufriev-Bashford-Case generalized Born implicit solvent were qualitatively consistent with experimental data, replica exchange molecular dynamics rather than other methods appeared to be more reasonable for calculations of amyloid β1–42 containing d-aspartic acid residues. Computational results...

Quantitative Analysis of PD 332991 in Mouse Plasma Using Automated Micro-Sample Processing and Microbore Liquid Chromatography Coupled with Tandem Mass Spectrometry

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 16 August 2011Danielle, Smith , Max, Tella , Sadayappan V., Rahavendran , Zhongzhou, ShenIn the oncology therapeutic area, the mouse is the pr…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 16 August 2011

Danielle, Smith , Max, Tella , Sadayappan V., Rahavendran , Zhongzhou, Shen

In the oncology therapeutic area, the mouse is the primary animal model used for efficacy studies. Often with mouse pharmacokinetic (PK) and pharmacokinetic/pharmacodynamic (PK/PD) studies, less than 20μL of total plasma sample volume is available for bioanalysis due to the small size of the animal and the need to split samples for other measurements such as biomarker analyses. The need to conduct automated “small volume” sample processing for quantitative bioanalysis has therefore increased. An automated fit for purpose protein precipitation (PPT) method using a Hamilton MicroLab Star (Reno, NV, USA) to support mouse PK and PK/PD studies for an oncology...

Immobilized metal affinity chromatography using open tubular capillary for phosphoprotein analysis: comparison between polymer brush coating and surface functionalization

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 12 August 2011Khadija El, Idrissi , Saïd, Eddarir , Caroline, Tokarski , Christian, RolandoIn the present article, open tubular-IMAC columns,…

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 12 August 2011

Khadija El, Idrissi , Saïd, Eddarir , Caroline, Tokarski , Christian, Rolando

In the present article, open tubular-IMAC columns, functionalized by iminodiacetic acid (IDA) for the immobilization of Fe3+, were prepared by in-situ chemical modification of fused silica capillary using two chemistries, polymer brush coating and surface functionalization. One column was based on a poly-(glycidyl methacrylate) brush (GMA) and the other on 3-glycidoxypropyltrimethoxysilane (GLYMO). Phosphopeptide enrichment on the open tubular columns was evaluated on an αS1, αS2 mixture and β casein peptides. The optimized enrichment protocol includes sample loading in a slightly acidic solution made with pure deionized water, a washing step with 10% acetonitrile, 0.1% formic acid, and an elution step...

DETERMINATION OF TRANEXAMIC ACID CONCENTRATION BY SOLID PHASE MICROEXTRACTION AND LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY. FIRST STEP TO IN VIVO ANALYSIS

Publication year: 2011Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 10 August 2011Barbara, Bojko , Dajana, Vuckovic , Erasmus, Cudjoe , Md Ehsanul, Hoque , Fatemeh, Mirnaghi , …A solid phase microextraction …

Publication year: 2011
Source: Journal of Chromatography B, In Press, Accepted Manuscript, Available online 10 August 2011

Barbara, Bojko , Dajana, Vuckovic , Erasmus, Cudjoe , Md Ehsanul, Hoque , Fatemeh, Mirnaghi , ...

A solid phase microextraction (SPME) method followed by LC-MS/MS analysis was developed to determine the concentration of tranexamic acid (TA) concentration in plasma. The use of a new biocompatible C18 coating allowed the direct extraction from complex biological samples without prior sample preparation; no matrix effect was observed. The results revealed that SPME was suitable for the analysis of polar drugs such as TA; such an application was previously inaccessible because of the limited availability of SPME coatings that can extract polar molecules. The proposed method was validated according to the bioanalytical method validation guidelines. LOD and LLOQ) were 0.5...