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      • Record: found
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      Application of LC–MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

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          Abstract

          Liquid chromatography tandem mass chromatography (LC–MS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC–MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisition modes (SIM, MRM) for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using LC–MS/MS and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis.

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          Identification of a cannabimimetic indole as a designer drug in a herbal product

          Nahoko Uchiyama, Ruri Kikura-Hanajiri, Nobuo Kawahara … (2009)
          Article 0 comments Cited 45 times – based on 0 reviews     Review now
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            A sensitive voltammetric sensor for determination of synthetic corticosteroid triamcinolone, abused for doping.

            Rajendra N Goyal, Vinod Gupta, Sanghamitra Chatterjee (2009)
            Edge plane pyrolytic graphite electrode (EPPGE) modified with single-wall carbon nanotubes (SWNTs) has been used as a sensor to determine triamcinolone, abused by athletes for doping. A comparison of the voltammetric behavior between SWNTs modified EPPGE and fullerene - C(60)-modified EPPGE indicated that SWNTs modified EPPGE is more sensitive. The electrode exhibited an effective catalytic response with good reproducibility and stability. The effect of several parameters such as pH, square wave frequency and steroid concentration were studied. The square wave voltammetric response of the electrode to triamcinolone is linear in the range 0.1-25 nM with a detection limit and sensitivity of 8.9 x 10(-10)M and 2.06 microA nM(-1), respectively. The method was applied for the determination of triamcinolone in several commercially available pharmaceuticals and real urine samples obtained from patients undergoing pharmacological treatment with triamcinolone. A comparison of the observed results with HPLC analysis indicated a good agreement. The product obtained after reduction of triamcinolone was also characterized using (1)H NMR and GC-MS and the site of reduction is found to be carbonyl group at position 20. The method described is rapid, simple and accurate and can be easily applied for detecting cases of doping.
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              Fullerene-C60-modified edge plane pyrolytic graphite electrode for the determination of dexamethasone in pharmaceutical formulations and human biological fluids.

              Sanghamitra Chatterjee, Rajendra N Goyal, Vinod Gupta (2009)
              Electrochemical behaviour of dexamethasone at the fullerene-C(60)-modified pyrolytic graphite electrode (PGE) has been investigated using Osteryoung square wave voltammetry (SWV). Compared to a bare PGE and fullerene-C(60)-modified glassy carbon electrode (GCE), the fullerene-C(60)-modified edge plane PGE exhibited an apparent shift of the peak potential to less negative potentials with a marked enhancement in the current response of dexamethasone. The peak potential was linearly dependent on pH with dE(p)/dpH as 59 mV/pH. Calibration plot having good linearity with a correlation coefficient 0.9983 is obtained in the concentration range of 0.05-100 microM and the sensitivity of the method has been found to be 0.685 microA microM(-1). The detection limit is estimated to be 5.5 x 10(-8)M. The electrode showed good sensitivity, stability and reproducibility. The practical analytical utility of the method is illustrated by quantitative determination of dexamethasone in several commercially available pharmaceutical formulations and human blood plasma of patients being treated with dexamethasone. HPLC method was used to compare the results obtained for the quantitative estimation of dexamethasone in biological fluids.
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                Author and article information

                Contributors
                Mohd Rashid
                Journal
                Journal ID (nlm-ta): J Pharm Anal
                Journal ID (iso-abbrev): J Pharm Anal
                Title: Journal of Pharmaceutical Analysis
                Publisher: Xi'an Jiaotong University
                ISSN (Print): 2095-1779
                ISSN (Electronic): 2214-0883
                Publication date PMC-release: 02 April 2013
                Publication date (Print): October 2013
                Publication date (Electronic): 02 April 2013
                Volume: 3
                Issue: 5
                Pages: 341-348
                Affiliations
                [a ]Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Jamia Hamdard (Hamdard University), Hamdard Nagar, New Delhi 110062, India
                [b ]Department of Chemistry, Indian Institute of Technology (IIT), Haridwar, Roorkee 247667, Uttarakhand, India
                [c ]Research Institute of Natural Sciences, Department of Chemistry, Changwon National University, Changwon 641773, Republic of Korea
                Author notes
                [* ]Corresponding author. Tel.: +91 11 26059681, +91 11 26059688x5647, mobile: +91 9911609781; fax: +91 11 16988874. rashidpharm2008@ 123456gmail.com rashidchem2012@ 123456gmail.com
                Article
                Publisher ID: S2095-1779(13)00032-4
                DOI: 10.1016/j.jpha.2013.03.005
                PMC ID: 5760999
                SO-VID: f3bea666-b26b-4fc7-b266-a1ba5677fe9b
                Copyright © © 2013 Xi’an Jiaotong University. Production and hosting by Elsevier B.V.
                License:

                This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

                History
                Date received : 13 June 2012
                Date accepted : 23 March 2013
                Categories
                Subject: Review Paper

                Keywords: lc–ms/ms,ionization techniques,glucocorticoids,stimulants,hyphenated techniques,biological fluid
                Data availability:
                Keywords: lc–ms/ms, ionization techniques, glucocorticoids, stimulants, hyphenated techniques, biological fluid

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