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Bhatt M.,P.A. College | Bhatt M.,Synchron Research Services Private Ltd | Shah S.,P.A. College | Shivprakash,Synchron Research Services Private Ltd
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2010

A simple, rapid, sensitive and specific ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the quantification of ethosuximide in human plasma is described. Analyte was chromatographed on a Hypersil Gold C18 column (100 mm × 2.1 mm, i.d., 1.9 μm) with isocratic elution at a flow rate of 0.250 mL/min and pravastatin was used as the internal standard. The assay involves a simple solid-phase extraction procedure of 0.25 mL human plasma and the analysis was performed on a triple-quadrupole tandem mass spectrometer by MRM mode via electrospray ionization (ESI). The method was linear in the concentration range of 0.25-60.0 μg/mL. The lower limit of quantification (LLOQ) was 0.25 μg/mL. The within- and between-day precision and accuracy of the quality control samples were within 10.0%. The recovery was 95.1% and 94.4% for ethosuximide and pravastatin, respectively. The analysis time for each sample was 1.8 min. The method was highly reproducible and gave peaks with excellent chromatography properties. © 2010 Elsevier B.V. All rights reserved.


Bhatt M.,P.A. College | Bhatt M.,Synchron Research Services Private Ltd | Shah S.,P.A. College | Shivprakash,Synchron Research Services Private Ltd
Biomedical Chromatography | Year: 2010

A rapid, sensitive and rugged solid-phase extraction ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for determination of paroxetine in human plasma. The procedure for sample preparation includes simple SPE extraction procedure coupled with Hypersil Gold C18 column (100 mm x 2.1 mm, i.d., 1.9 μm) with isocratic elution at a fl ow-rate of 0.350 mL/min and fl uoxetine was used as the internal standard. The analysis was performed on a triple-quadrupole tandem mass spectrometer by multiple reactions monitoring mode via electrospray ionization. Using 500 μL plasma, the methods were validated over the concentration range 0.050-16.710 ng/mL for paroxetine, with a lower limit of quantifi cation of 0.050 ng/mL. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recovery was 69.2 and 74.4% for paroxetine and fl uoxetine respectively. Total run time was only 1.9 min. The method was highly reproducible and gave peaks with excellent chromatography properties. Copyright © 2009 John Wiley & Sons, Ltd.


Bhatt M.,P.A. College | Bhatt M.,Synchron Research Services Private Ltd | Shah S.,P.A. College | Shivprakash,Synchron Research Services Private Ltd
Biomedical Chromatography | Year: 2011

A rapid and sensitive ultraperformance liquid chromatography tandem mass spectrometry assay was developed for the simultaneous analysis of oxcarbazepine and its main metabolite in human plasma. The assay involves a simple solid-phase extraction procedure of 0.3mL of human plasma and analysis was performed on a triple-quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionization. Separation was achieved on an Acquity UPLC™ BEH C18 column (50×2.1mm, i.d., 1.7μm) with isocratic elution at a flow-rate of 0.25mL/min and imipramine was used as the internal standard. The standard calibration curve was linear over the range 9.580-5070.205ng/mL for oxcarbazepine (OXC) and 19.444-10290.800ng/mL for 10,11-dihydro-10-hydroxycarbamazepine (MHD), expressed by the linear correlation coefficient r2, which was better than 0.995 for OXC and MHD. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recoveries were 81.0, 89.6 and 66.6% for OXC, MHD and imipramine, respectively. The total run time was 1.5min only for each sample, which makes it possible to analyze more than 350 samples per day. © 2010 John Wiley & Sons, Ltd.


Bhatt M.,P.A. College | Bhatt M.,Synchron Research Services Private Ltd | Bhatt M.,Synchron Research Services Private Ltd | Shah S.,P.A. College | Shivprakash,Synchron Research Services Private Ltd
Biomedical Chromatography | Year: 2010

A method based on ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) in combination with solid-phase extraction for sample pretreatment has been developed for the simultaneous analysis of amitriptyline and its main metabolite in human plasma. The extraction of the analytes from plasma samples was carried out by means of a selective SPE procedure using hydrophilic-lipophilic balance cartridges. The assay involves a simple solid-phase extraction (SPE) procedure of 0.2 mL of human plasma and analysis was performed on a triple-quadrupole tandem mass spectrometer by multiple reactions monitoring (MRM) mode via electrospray ionization (ESI). The standard calibration curve was linear over the ranges 0.370-95.539 ng/mL for amitriptyline and 0.365-94.374 ng/mL for nortriptyline, expressed by the linear correlation coefficient r 2, which was better than 0.995 for both. The intra- and inter-day precision and accuracy of the quality control samples were within 10.0%. The recovery was 85.3, 88.4 and 80.7% for amitriptyline, nortriptyline and doxepin respectively. Total run time was 1.2 min only for each sample, which makes it possible to analyze more than 400 samples per day. The method was highly reproducible and gave peaks with excellent chromatography properties. Copyright © 2010 John Wiley & Sons, Ltd.

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