Just Published: Journal of Pharmaceutical and Biomedical Analysis

A new issue of this journal has just been published. To see abstracts of the papers it contains (with links through to the full papers) click here:

Journal of Pharmaceutical and Biomedical Analysis
http://rss.sciencedirect.com/publication/science/5266

Selected papers from the latest issue:

1.

Exploring better column selectivity choices in Ultra-High Performance Liquid Chromatography using Quality by Design principles   Original Research Article Available online 28 February 2013 Róbert Kormány, Imre Molnár, Hans-Jürgen Rieger Graphical abstract Highlights ► We developed UHPLC methods by DryLab software on 9 different type stationary phases. ► The predicted retention times were in good agreement with the experimental ones. ► The type of stationary phase not influences the effectiveness of computer simulation.

2.

Analysis of the microcrystalline inclusion compounds of triclosan with β-cyclodextrin and its tris-O-methylated derivative   Original Research Article Available online 28 February 2013 Ana I. Ramos, Teresa M. Braga, José A. Fernandes, Patrícia Silva, Paulo J. Ribeiro-Claro, Filipe A. Almeida Paz, Maria de Fátima Silva Lopes, Susana S. Braga Graphical abstract We isolated solid 1:1 inclusion compounds of triclosan with the hosts (-CD and TRIMEB and identified by single-crystal diffraction a new phase for (-CD·triclosan. The TRIMEB adduct was amorphous and displayed promising antimicrobial action, being more active than triclosan against ATCC 7644 strain of Listeria monocytogenes and the V583, ATCC 29212 and DSM 20478 strains of Enterococcus faecalis and less toxic against environmental strains from sweet water. Highlights ► Triclosan forms 1:1 solids with β-CD and TRIMEB, the latter being amorphous. ► β-CD·Triclosan is microcrystalline and contains at least two different phases. ► Single-crystal diffraction on one of these showed host-guest dimers (2:2) with channel packing. ► Ab initio studies helped estimate the position of disordered triclosan inside the β-CD dimers. ► The inclusion of triclosan into TRIMEB is beneficial for antimicrobial action.

3.

Rapid screening and structural elucidation of a novel sibutramine analogue in a weight loss supplement: 11-desisobutyl-11-benzylsibutramine    Available online 28 February 2013 Daniel J. Mans, Ashley C. Gucinski, Jamie D. Dunn, Connie M. Gryniewicz-Ruzicka, Laura C. Mecker-Pogue, Jeff L.-F. Kao, Xia Ge Graphical abstract . Highlights ► A novel analogue of sibutramine was detected in weight loss supplements. ► Nuclear magnetic resonance and tandem mass spectrometry led to ID. ► Ion mobility spectrometry served as a rapid screening method for detection.

4.

Development of a HPLC-UV method for thE quantitative determination of four Short-Chain fatty acids and lactic acid produced by intestinal bacteria during in-vitro fermentation   Original Research Article Available online 28 February 2013 S. De Baere, V. Eeckhaut, M. Steppe, C. De Maesschalk, P. De Backer, F. Van Immerseel, S. Croubels Graphical abstract Highlights ► Determination of four short-chain fatty acids (SCFAs) and lactic acid in supernatants of faecal bacterial culture samples. ► Rapid HPLC-UV analysis (run-time: 15min). ► straightforward sample preparation procedure (liquid-liquid extraction). ► In-house method validation. ► Application of the method in the field ofin-vitrotesting of bacterial SCFA fermentation.

5.

Rapid classification of pharmaceutical ingredients with Raman spectroscopy using compressive detection strategy with PLS-DA multivariate filters   Original Research Article Available online 28 February 2013 Derya Cebeci Maltaş, Kaho Kwok, Ping Wang, Lynne S. Taylor, Dor Ben-Amotz Graphical abstract Highlights ► A new Raman PAT sensor with hardware based compressive detection system is proposed. ► Compressive detection filters are generated with PLS-DA algorithm. ► A hybrid supervised/unsupervised strategy is employed for rapid classification.

6.

Stir bar sorptive extraction with EG-Silicone coating for bisphenols determination in personal care products by GC-MS   Original Research Article Available online 27 February 2013 Juan Ignacio Cacho, Natalia Campillo, Pilar Viñas, Manuel Hernández-Córdoba Graphical abstract Highlights ► Ethylene glycol-silicone coated stir bars are used for the preconcentration of bisphenols. ► No derivatization is required for the TD-GC-MS procedure. ► Sensitivity is not as high as could be expected but time and reagents are saved.

7.

Metabolic fate of combretastatin A-1: LC-DAD-MS/MS investigation and biological evaluation of its reactive metabolites   Original Research Article Available online 27 February 2013 Silvio Aprile, Roberta Zaninetti, Erika Del Grosso, Armando A. Genazzani, Giorgio Grosa Graphical abstract Highlights ►In vitro/in vivometabolism investigation of combretastatin A-1. ► LC-UV and LC-MS experiments. ► Synthesis and spectroscopic characterization of the quinone metabolite Q1. ► Cytotoxicity and antitubulinic activities of combretastatins quinone metabolites. ► Chemical reactivity toward tubulin (Ellman's assay).

8.

Qualitative and quantitative analysis of the major constituents in Chinese medicinal preparation Dan-Lou Tablet by ultra high performance liquid chromatography/ diode-array detector/quadrupole time-of-flight tandem mass spectrometry   Original Research Article Available online 27 February 2013 Juan Dong, Yan Zhu, Xiumei Gao, Yanxu Chang, Meng Wang, Peng Zhang Graphical abstract Highlights ► The qualitative analysis of Dan-Lou tablet was reported for the first time. ► The quantitative analysis of Dan-Lou tablet was reported for the first time. ► Sixty-eight compounds were identified in 40min by using UPLC-DAD-QTOF method. ► Nineteen compounds were quantified in 30min by using UPLC-DAD method. ► The characteristic behaviors of six kinds of compounds were summarized.

9.

A UPLC-MS/MS method for the simultaneous plasma quantification of all isomeric forms of the new anti-HCV protease inhibitors Boceprevir and Telaprevir   Original Research Article Available online 27 February 2013 Antonio D’Avolio, Amedeo De Nicolò, Danilo Agnesod, Marco Simiele, Adnan Mohamed Abdi, Sujan Dilly Penchala, Lucio Boglione, Giuseppe Cariti, Giovanni Di Perri Graphical abstract Highlights ► First method to simultaneously quantify Telaprevir and Boceprevir isomers ► We use human acidified plasma, avoiding the transition from one isomer to another ► The first time use of UPLC-MS/MS, allowing a short and high selective run ► We use a easy to buy and cheap IS (quinoxaline) ► The extraction procedure is very fast and cheap (No SPE cartridges).

10.

Immobilised magnetic beads based multi-target affinity selection coupled with high performance liquid chromatography-mass spectrometry for screening anti-diabetic compounds from a Chinese medicine “Tang-Zhi-Qing”   Original Research Article Available online 27 February 2013 Yi Tao, Zhui Chen, Yufeng Zhang, Yi Wang, Yiyu Cheng Graphical abstract Schematic diagram of the magnetic beads based multi-target affinity selection-mass spectrometry approach. Highlights ► A multi-target affinity selection-mass spectrometry approach was established. ► Screen anti-diabetic compounds from formula Tang-Zhi-Qing using the approach. ► Screening parameters were optimized using three model inhibitors. ► Five anti-diabetic compounds were identified. ► Three of them were identified for the first time.

11.

UPLC-Q-TOF-MS/MS fingerprinting of Traditional Chinese Formula SiJunZiTang   Original Research Article Available online 27 February 2013 Yanyan Wang, Shan He, Xiaochen Cheng, Yuxin Lu, Yunpeng Zou, Qinglin Zhang Graphical abstract UPLC-Q-TOF-MS/MS chromatographic fingerprinting of Traditional Chinese Formula SiJunZi Tang. Highlights ► UPLC/MS fingerprinting of SiJunZi Tang, a classic Traditional Chinese Formula, was developed. ► 66 compounds were detected and originality was confirmed. ► 58 compounds were identified by comparing the accurate mass and fragment information. ► The major constituents in SJZT extract came from Radix Ginseng and Glycyrrhiza uralensis.

12.

Monitoring Blend Potency in a Tablet Press Feed Frame Using Near Infrared Spectroscopy   Original Research Article Available online 27 February 2013 Howard W. Ward, Daniel O. Blackwood, Mark Polizzi, Hugh Clarke Graphical abstract . Schematic representation of the NIR probe in relationship to key elements of the Kilian T-100 tablet press feed frame. Highlights ► NIR probe installed into the feed frame of a rotary tablet press to monitor API concentration. ► Excellent correlations shown between the NIR signal and tablet potency from stratified tablets. ► This PAT application may be used to better understand powder mixing dynamics in a tablet press. ► Integration with the tablet press control system may enable Real-Time-Release testing.

13.

Analysis of impurities in vertilmicin sulfate by liquid chromatography ion-trap mass spectrometry    Available online 27 February 2013 Yao-zuo Yuan, Mei Zhang, Xia-Lei Fan, Chang-qin Hu, Shao-hong Jin, Ann Van Schepdael, Jos Hoogmartens, Erwin Adams Graphical abstract Main ion trap mass fragmentation pathways of vertilmicin. Highlights ► An LC/MS method for characterization of impurities in vertilmicin was developed. ► The impurity profile of vertilmicin sulfate was reported for the first time. ► 18 impurities, of which 11 new ones, were detected and identified in a bulk sample. ► Alkaline mobile phase reduces ion suppression and improves MS sensitivity.

14.

Simultaneous analysis of codeine and its active metabolites in human plasma using liquid chromatography-tandem mass spectrometry: Application to a pharmacokinetic study after oral administration of codeine   Original Research Article Available online 27 February 2013 Xiujun Wu, Weiping Zhang, Yin Bai, Tao Guo, Jingkai Gu Graphical abstract A rapid sensitive bioassay based on LC MS/MS has been developed and validated for the simultaneous determination of codeine and its active metabolities, including morphine, morphine3β-glucoronide (M3G) and morphine 6β-glucuronide (M)G, in human plasma, The assay achieves a qualitation limit of 0.05ng/ml for all four analytes in a much reduced run time (5min) and has been applied to a pharmacokinetic study of codeine in healthy Mongolian Chinese volunteers after a 30mg oral dose.