Simultaneous analysis of allopurinol and oxypurinol using a validated liquid chromatography-tandem mass spectrometry method in human plasma

详细信息    查看全文

• 作者：Dhiraj M. Rathod^a ; ^b ; Keyur R. Patel^b ; Hiren N. Mistri^b ; Arvind G. Jangid^b ; Pranav S. Shrivastav^c ; ^{pranav_shrivastav@yahoo.com} ; Mallika Sanyal^d
• 关键词：Allopurinol ; Oxypurinol ; Liquid chromatography&ndash ; tandem mass spectrometry ; Bioequivalence study
• 刊名：Journal of Pharmaceutical Analysis
• 出版年：2017
• 出版时间：February 2017
• 年：2017
• 卷：7
• 期：1
• 页码：56-62
• 全文大小：632 K
• 卷排序：7

文摘

The present study describes a simple, reliable and reproducible liquid chromatography–tandem mass spectrometry method (LC–MS/MS) for the simultaneous determination of allopurinol and its active metabolite, oxypurinol in human plasma for a pharmacokinetic/bioequivalence study. After protein precipitation (PPT) of 100 µL plasma sample with 1.0% formic acid in acetonitrile, the recovery of the analytes and allopurinol-d2 as an internal standard ranged from 85.36% to 91.20%. The analytes were separated on Hypersil Gold (150 mm×4.6 mm, 5 µm) column using 0.1% formic acid-acetonitrile (98:2, v/v) as the mobile phase. Quantification was done using electrospray ionization in the positive mode. The calibration concentration range was established from 60.0 to 6000 ng/mL for allopurinol and 80.0–8000 ng/mL for oxypurinol. Matrix effect in human plasma, expressed as IS-normalized matrix factors ranged from 1.003 to 1.030 for both the analytes. The developed method was found suitable for a clinical study with 300 mg allopurinol tablet formulation in healthy subjects.