EarlyView Articles
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LC‐MS/MS method for the determination of pitolisant: application to rat pharmacokinetic and brain penetration studies
Published: Jun 13, 2013
Author(s): Ramakrishna Nirogi, Devender Reddy Ajjala, Vishwottam Kandikere, Hanumanth Rao Pantangi, Mahesh Reddy Jonnala, Gopinadh Bhyrapuneni, Nageswar Rao Muddana, Himabindu Vurimindi
Journal: Biomedical Chromatography
ABSTRACT A simple and sensitive LC‐MS/MS method was developed and validated for the quantitation of pitolisant, an H3 receptor antagonist/inverse agonist. Acetonitrile protein precipitation technique was used to prepare rat blood and brain tissue homogenate samples by using aripiprazole as internal standard (IS). Chromatographic separation was performed by using Xbridge column (2.1 × 50 mm, 3.5 µm) with a gradient elution program. The mobile...
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Comparative study on the excretion of vitexin‐4′′‐ O ‐glucoside in mice after oral and intravenous administration by using HPLC
Published: Jun 13, 2013
Author(s): Shuang Cai, Yinghui Chen, Wenjie Zhang, Xixiang Ying
Journal: Biomedical Chromatography
ABSTRACT The aim of the present study was to characterize the excretion of pure vitexin‐4”‐O‐glucoside (VOG) in mice following oral and intravenous administration at a dose of 30 mg/kg. A sensitive and specific HPLC method with hespridin as internal standard, a Diamonsil C18 column protected with a KR C18 guard column and a mixture consisting of methanol–acetonitrile–tetrahydrofuran–0.1% glacial acetic acid (6:2:18:74, v/v/v/v) as mobile phase...
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Fabrication of electroactive composite nanofibers of functionalized polymer and CNT capable of specifically binding with the IgE (Immunoglobulin E) antibody
Published: Jun 11, 2013
Author(s): Omotunde Olubi, Deepti Gadi, Biswajit Sannigrahi, Michael Williams, Barbara Baird, Ishrat Khan
Journal: Surface and Interface Analysis
Electroactive nanofibers decorated with α,ω‐bi‐(dinitrophenylcaproic acid), abbreviated as DNP, have been prepared by electrospinning a solution of α,ω‐bi[2,4‐dinitrophenylcaproic][poly(ethyleneoxide)‐b‐poly(2‐methoxystyrene)‐b‐poly(ethylene oxide)], polystyrene and single‐walled carbon nanotubes (SWCNTs). The α,ω‐bi[2,4‐dinitrophenylcaproic][poly(ethyleneoxide)‐b‐poly(2‐methoxystyrene)‐b‐poly(ethyleneoxide)] polymers were synthesized by...
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Bacteriocin activity against various pathogens produced by Pediococcus pentosaceus VJ13 isolated from Idly batter
Published: Jun 11, 2013
Author(s): Venkatasubramanian Vidhyasagar, Kadirvelu Jeevaratnam
Journal: Biomedical Chromatography
ABSTRACT Bacteriocins, an antimicrobial peptide, is known to have wide spectrum antimicrobial activity against various pathogens. Because they are easily digested in the intestine, they are considered as safe and are widely used as food preservatives. Hence their purification and characterization have attracted considerable attraction, especially for those having activity against human pathogens. In this study, the bacteriocin...
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Validated LC‐MS method for simultaneous quantitation of catalpol and harpagide in rat plasma: application to a comparative pharmacokinetic study in normal and diabetic rats after oral administration of Zeng‐Ye‐Decoction
Published: Jun 11, 2013
Author(s): Yukun Feng, Zhenzhen Liu, Ying Peng, Lunhui Zhang, Ping Ju, Kaishun Bi, Xiaohui Chen
Journal: Biomedical Chromatography
ABSTRACT A simple and efficient liquid chromatography‐mass spectrometry (LC‐MS) method was developed and validated for simultaneous quantitation of catalpol and harpagide in normal and diabetic rat plasma. Protein precipitation extraction with acetonitrile was carried out using salidroside as the internal standard (IS). The LC separation was performed on an Elite C18 column (150 × 4.6 mm, 5 µm) with the mobile phase consisting of acetonitrile...
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Multimodal, label‐free nonlinear optical imaging for applications in biology and biomedical science
Published: Jun 11, 2013
Author(s): R. Mouras, P. Bagnaninchi, A. Downes, A. Elfick
Journal: Journal of Raman Spectroscopy
We have developed a multimodal optical platform for label‐free imaging on the basis of nonlinear optical microscopy (NLO) for applications in biology and biomedical science. Three application areas have been chosen as examples: regenerative medicine, drug delivery monitoring and cancer diagnosis. Obtained data showed the potential of NLO microscopy for the following: (1) investigating the stem cell differentiation states prior their use...
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Quantification of aconitine in post‐mortem specimens by validated liquid chromatography‐tandem mass spectrometry method: Three case reports on fatal ´monkshood´ poisoning
Published: Jun 10, 2013
Author(s): Wolfgang Bicker, Fabio Monticelli, Andreas Bauer, Gabriele Roider, Thomas Keller
Journal: Drug Testing and Analysis
The diester‐diterpene alkaloid aconitine was quantified by liquid chromatography‐tandem mass spectrometry in post‐mortem specimens of three cases where suicidal ingestion of Aconitum napellus L. (´monkshood´) was supposed. In an attempt at rationalization, sample preparation and chromatographic conditions of plasma/serum drug analysis routine were utilized. Linearity was established from 0.5 to 20 µg L‐1 using newborn calf serum (NCS) as a surrogate...
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Electrochemical in situ surface enhanced Raman spectroscopic characterization of a trinuclear ruthenium complex, Ru‐red
Published: Jun 10, 2013
Author(s): Khurram Saleem Joya, Huub J. M. Groot
Journal: Journal of Raman Spectroscopy
To study the fate of a molecular di‐μ‐oxo‐bridged trinuclear ruthenium complex, [(NH3)5Ru–O–Ru(NH3)4–O–Ru(NH3)5]6+, also known as Ru‐red, during the electro‐driven water oxidation reaction, electrochemical in situ surface enhanced Raman spectroscopy (SERS) investigations have been conducted on an electrochemically roughened gold surface in acidic condition. It was previously described that on a basal plane pyrolitic graphite electrode in 0.1 M H2SO4 aqueous...
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Multivariate curve resolution for understanding complex reactions
Published: Jun 9, 2013
Author(s): Randy J. Pell, Xiaoyun Chen
Journal: Journal of Chemometrics
Chemometrics is applied to in situ infrared spectra collected from a complex reacting mixture to elucidate the reaction mechanism. A series of models beginning with simple peak area progressing to classical least squares then to multivariate curve resolution with nonnegative spectral and concentration profile constraints and finally to multivariate curve resolution with nonnegative constraints and spectral and concentration profile...
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Detection of myo ‐inositol tris pyrophosphate (ITPP) in equine following an administration of ITPP
Published: Jun 4, 2013
Author(s): Geoffrey Lam, Sarah Zhao, Jasmeet Sandhu, Rong Yi, Devan Loganathan, Barbara Morrissey
Journal: Drug Testing and Analysis
Myo‐Inositol tris pyrophosphate (ITPP) is a powerful allosteric modulator of haemoglobin that increases oxygen‐releasing capacity of red blood cells. It is capable of crossing the red blood cell membrane unlike its open polyphosphate analog myo‐inositol hexakisphosphate (IHP). Systemic administration of ITPP enhanced the exercise capacity in mice. There have been rumours of its abuse in the horse racing industry to enhance the performance of racing...
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Pharmacokinetics of GHB and detection window in serum and urine after single uptake of a low dose of GBL – an experiment with two volunteers
Published: Jun 4, 2013
Author(s): Alexandra Schröck, Yvonne Hari, Stefan König, Volker Auwärter, Stefan Schürch, Wolfgang Weinmann
Journal: Drug Testing and Analysis
During the last few years γ‐hydroxybutyric acid (GHB) and γ‐butyrolactone (GBL) have attracted much interest as recreational drugs and knock‐out drops in drug‐facilitated sexual assaults. This experiment aims at getting an insight into the pharmacokinetics of GHB after intake of GBL. Therefore Two volunteers took a single dose of 1.5 ml GBL, which had been spiked to a soft drink. Assuming that GBL was completely metabolized to GHB, the...
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Characterizing the interaction between enantiomers of eight psychoactive drugs and highly sulfated‐ β ‐cyclodextrin by counter‐current capillary electrophoresis
Published: Jun 4, 2013
Author(s): Lucía Asensi‐Bernardi, Laura Escuder‐Gilabert, Yolanda Martín‐Biosca, Salvador Sagrado, María José Medina‐Hernández
Journal: Biomedical Chromatography
ABSTRACT The estimation of apparent binding constants and limit mobilities of the complexes of the enantiomers that characterize the interaction of enantiomers with chiral selectors, in this case highly sulfated β‐cyclodextrin, was approached using a simple and economic electrophoretic modality, the complete filling technique (CFT) in counter‐current mode. The enantiomers of eight psychoactive drugs, four antihistamines (dimethindene,...
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A sensitive LC‐MS/MS method for the quantification of febuxostat in human plasma and its pharmacokinetic application
Published: Jun 4, 2013
Author(s): Venkata Rami Reddy Vaka, Jaswanth Kumar Inamadugu, Nageswara Rao Pilli, Mullangi Ramesh, Hussain Reddy Katreddi
Journal: Biomedical Chromatography
ABSTRACT An improved, simple and highly sensitive LC‐MS/MS method has been developed and validated for quantification of febuxostat with 100 μL human plasma using febuxostat‐d7 as an internal standard (IS) according to regulatory guidelines. The analyte and IS were extracted from human plasma via liquid–liquid extraction using diethyl ether. The chromatographic separation was achieved on a Zorbax C18 column using a mixture of acetonitrile and...
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The effect of the pH on the interaction of L‐arginine with colloidal silver nanoparticles. A Raman and SERS study
Published: Jun 4, 2013
Author(s): C. Garrido, T. Aguayo, E. Clavijo, J. S. Gómez‐Jeria, M. M. Campos‐Vallette
Journal: Journal of Raman Spectroscopy
Raman and surface enhanced Raman scattering (SERS) spectroscopies were used to study the pH effect (7 to 9) on the interaction of arginine (Arg) with colloidal Ag nanoparticles (AgNps). A new methodology was implemented in order to obtain reproducible SERS spectra in solution. The dependence of the Arg concentration on the stability of the AgNps is discussed. A pH increasing of the colloidal solution to the limits of the Arg pKa2 value...
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Quantification of human high‐energy phosphate metabolite concentrations at 3 T with partial volume and sensitivity corrections
Published: Jun 3, 2013
Author(s): AbdEl‐Monem M. El‐Sharkawy, Refaat E. Gabr, Michael Schär, Robert G. Weiss, Paul A. Bottomley
Journal: NMR in Biomedicine
Practical noninvasive methods for the measurement of absolute metabolite concentrations are key to the assessment of the depletion of myocardial metabolite pools which occurs with several cardiac diseases, including infarction and heart failure. Localized MRS offers unique noninvasive access to many metabolites, but is often confounded by nonuniform sensitivity and partial volume effects in the large, poorly defined voxels commonly used...
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Studies on paint cross sections of a glass painting by using FT‐IR and Raman microspectroscopy supported by univariate and hierarchical cluster analyses
Published: Jun 3, 2013
Author(s): Emilia Staniszewska, Kamilla Malek, Zofia Kaszowska
Journal: Journal of Raman Spectroscopy
Fourier transform infrared (FT‐IR) and Raman spectroscopy is used for the non‐destructive analysis of painting materials and ageing compounds in micrometric cross sections of a glass painting. The combination of both techniques in conjunction with imaging/mapping function provides the spatial distribution of chemical components identified in vibrational spectra. The aim of our work is to show the applicability of the FT‐Raman mapping...
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Top‐down HPLC – ESI ‐ MS characterization of rat gliadoralin A , a new member of the family of rat submandibular gland glutamine‐rich proteins and potential substrate of transglutaminase
Published: May 30, 2013
Author(s): Tiziana Cabras, Federica Iavarone, Davide Pirolli, Maria Cristina De Rosa, Alberto Vitali, Gavino Faa, Massimo Cordaro, Irene Messana, Jörgen Ekström, Massimo Castagnola
Journal: Journal of Separation Science
During HPLC–ESI‐MS/MS analysis of rat submandibular saliva secreted under isoprenaline stimulation, a protein with an experimental [M+H]1+ = 10 544.24 m/z was detected (17.5 ± 0.7 min). The MS/MS fragmentation pattern, manually investigated, allowed establishing an internal sequence in agreement with a DNA‐derived sequence of an unknown rat protein coded D3Z9M3 (Swiss‐Prot). To match the experimental MS/MS fragmentation pattern and...
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Analysis of mural paintings using in situ non‐invasive XRF, FTIR spectroscopy and optical microscopy
Published: May 30, 2013
Author(s): Nicoleta Vornicu, Cristina Bibire, Elena Murariu, Daniela Ivanov
Journal: X-Ray Spectrometry
An analytical protocol consisting of X‐ray fluorescence spectroscopy, optical microscopy and Fourier transform infrared spectroscopy was used to study the origin and the nature of the materials (pigments, binders and coating preparation) of the Fundenii Doamnei church mural paint from Bucharest. The main interest of the present study consisted in the original votive paint from narthex, painted in 1757 in a secco technique. ...
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Identification and quantification of synthetic cannabinoids in ‘spice‐like’ herbal mixtures: A snapshot of the German situation in the autumn of 2012
Published: May 30, 2013
Author(s): Nico Langer, Rainer Lindigkeit, Hans‐Martin Schiebel, Ludger Ernst, Till Beuerle
Journal: Drug Testing and Analysis
Synthetic compounds mimicking cannabis‐like effects are a recent trend. Currently, these so‐called synthetic cannabinoids are the largest and fastest growing class of newly appearing designer drugs. Many national authorities are continuously adapting their regulations to keep pace with the permanently changing variety of compounds. We have analyzed eight herbal smoking blends containing synthetic cannabinoids. Altogether, nine compounds...
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Simultaneous determination of morniflumate and its major active metabolite, niflumic acid, in human plasma by high‐performance liquid chromatography in stability and pharmacokinetic studies
Published: May 30, 2013
Author(s): Hea‐Young Cho, Geun‐Kyeong Park, Yong‐Bok Lee
Journal: Biomedical Chromatography
ABSTRACT A rapid, sensitive and stable high‐performance liquid chromatography (HPLC) method was developed and validated for the simultaneous determination of morniflumate and its major active metabolite, niflumic acid, in human plasma. HPLC analysis was carried out using a 5 µm particle size, C18‐bonded silica column with a mixture of acetonitrile and 0.005 m potassium phosphate monobasic in water (60:40, v/v) as the mobile phase and UV...
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