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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

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        Analysis of undeclared synthetic phosphodiesterase-5 inhibitors in dietary supplements and herbal matrices by LC-ESI-MS and LC-UV.

        A liquid chromatography-electrospray ionisation-mass spectrometry (LC-ESI-MS) method was developed to screen for the presence of synthetic phosphodiesterase type 5 (PDE-5) inhibitors including sildenafil, tadalafil and vardenafil. The method was applied to the analysis of dietary supplements and bulk herbal materials. Bulk powders or composites of tablets, capsules or liquids were prepared and an extraction of PDE-5 inhibitors was performed using a mixture of acetonitrile and water with sonication. Identification of sildenafil, vardenafil or tadalafil was accomplished using a single quadrupole mass spectrometer coupled to a liquid chromatograph with an electrospray interface. Positive ion detection in the full scan mode was used while in-source collision induced dissociation (CID) provided several structurally significant fragment ions to aid in the mass spectral identification. Approximately half of the 40 botanical products analyzed were found to contain undeclared synthetic PDE-5 inhibitors. For products found to contain one of these three compounds by LC-MS, HPLC with UV detection was used for quantitation.
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          Liquid chromatography coupled with time-of-flight and ion trap mass spectrometry for qualitative analysis of herbal medicines

          With the expansion of herbal medicine (HM) market, the issue on how to apply up-to-date analytical tools on qualitative analysis of HMs to assure their quality, safety and efficacy has been arousing great attention. Due to its inherent characteristics of accurate mass measurements and multiple stages analysis, the integrated strategy of liquid chromatography (LC) coupled with time-of-flight mass spectrometry (TOF-MS) and ion trap mass spectrometry (IT-MS) is well-suited to be performed as qualitative analysis tool in this field. The purpose of this review is to provide an overview on the potential of this integrated strategy, including the review of general features of LC-IT-MS and LC-TOF-MS, the advantages of their combination, the common procedures for structure elucidation, the potential of LC-hybrid-IT-TOF/MS and also the summary and discussion of the applications of the integrated strategy for HM qualitative analysis (2006–2011). The advantages and future developments of LC coupled with IT and TOF-MS are highlighted.
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            Author and article information

            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
            Contributors
            Journal
            J Pharm Anal
            J Pharm Anal
            Journal of Pharmaceutical Analysis
            Xi'an Jiaotong University
            2095-1779
            2214-0883
            02 April 2013
            October 2013
            02 April 2013
            : 3
            : 5
            : 341-348
            5760999 S2095-1779(13)00032-4 10.1016/j.jpha.2013.03.005
            © 2013 Xi’an Jiaotong University. Production and hosting by Elsevier B.V.

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

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