Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS

A simple, rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLCâMS/MS) method has been developed for the simultaneous determination of cilostazol and its pharmacologically active metabolite 3,4-dehydro cilostazol in human plasma using deuterated analogs as intern...

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Main Authors: Nejal M. Bhatt, Vijay D. Chavada, Daxesh P. Patel, Primal Sharma, Mallika Sanyal, Pranav S. Shrivastav
Format: Article
Language:English
Published: Elsevier 2015-02-01
Series:Journal of Pharmaceutical Analysis
Online Access:http://www.sciencedirect.com/science/article/pii/S2095177914000689
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author Nejal M. Bhatt
Vijay D. Chavada
Daxesh P. Patel
Primal Sharma
Mallika Sanyal
Pranav S. Shrivastav
author_facet Nejal M. Bhatt
Vijay D. Chavada
Daxesh P. Patel
Primal Sharma
Mallika Sanyal
Pranav S. Shrivastav
author_sort Nejal M. Bhatt
collection DOAJ
description A simple, rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLCâMS/MS) method has been developed for the simultaneous determination of cilostazol and its pharmacologically active metabolite 3,4-dehydro cilostazol in human plasma using deuterated analogs as internal standards (ISs). Plasma samples were prepared using solid phase extraction and chromatographic separation was performed on UPLC BEH C18 (50 mmÃ2.1 mm, 1.7 µm) column. The method was established over a concentration range of 0.5â1000 ng/mL for cilostazol and 0.5â500 ng/mL for 3,4-dehydro cilostazol. Intra- and inter-batch precision (% CV) and accuracy for the analytes were found within 0.93â1.88 and 98.8â101.7% for cilostazol and 0.91â2.79 and 98.0â102.7% for the metabolite respectively. The assay recovery was within 95â97% for both the analytes and internal standards. The method was successfully applied to support a bioequivalence study of 100 mg cilostazol in 30 healthy subjects. Keywords: Cilostazol, 3,4-dehydro cilostazol, UPLCâMS/MS, Sensitive, High throughput
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spelling doaj.art-a169356b2045486ea5bb6e33917d68fe2022-12-21T22:57:42ZengElsevierJournal of Pharmaceutical Analysis2095-17792015-02-0151111Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MSNejal M. Bhatt0Vijay D. Chavada1Daxesh P. Patel2Primal Sharma3Mallika Sanyal4Pranav S. Shrivastav5Department of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380009, Gujarat, IndiaDepartment of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380009, Gujarat, IndiaDepartment of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380009, Gujarat, IndiaDepartment of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380009, Gujarat, IndiaDepartment of Chemistry, St. Xavier׳s College, Navrangpura, Ahmedabad 380009, Gujarat, IndiaDepartment of Chemistry, School of Sciences, Gujarat University, Navrangpura, Ahmedabad 380009, Gujarat, India; Corresponding author. Tel.: +91 079 26300969; fax: +91 079 26308545.A simple, rapid and sensitive ultra performance liquid chromatography-tandem mass spectrometry (UPLCâMS/MS) method has been developed for the simultaneous determination of cilostazol and its pharmacologically active metabolite 3,4-dehydro cilostazol in human plasma using deuterated analogs as internal standards (ISs). Plasma samples were prepared using solid phase extraction and chromatographic separation was performed on UPLC BEH C18 (50 mmÃ2.1 mm, 1.7 µm) column. The method was established over a concentration range of 0.5â1000 ng/mL for cilostazol and 0.5â500 ng/mL for 3,4-dehydro cilostazol. Intra- and inter-batch precision (% CV) and accuracy for the analytes were found within 0.93â1.88 and 98.8â101.7% for cilostazol and 0.91â2.79 and 98.0â102.7% for the metabolite respectively. The assay recovery was within 95â97% for both the analytes and internal standards. The method was successfully applied to support a bioequivalence study of 100 mg cilostazol in 30 healthy subjects. Keywords: Cilostazol, 3,4-dehydro cilostazol, UPLCâMS/MS, Sensitive, High throughputhttp://www.sciencedirect.com/science/article/pii/S2095177914000689
spellingShingle Nejal M. Bhatt
Vijay D. Chavada
Daxesh P. Patel
Primal Sharma
Mallika Sanyal
Pranav S. Shrivastav
Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
Journal of Pharmaceutical Analysis
title Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
title_full Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
title_fullStr Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
title_full_unstemmed Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
title_short Determination of cilostazol and its active metabolite 3,4-dehydro cilostazol from small plasma volume by UPLCâMS/MS
title_sort determination of cilostazol and its active metabolite 3 4 dehydro cilostazol from small plasma volume by uplcams ms
url http://www.sciencedirect.com/science/article/pii/S2095177914000689
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