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目的:建立用液相色谱-串联质谱法测定人血浆中吡格列酮(PIO)及其活性代谢物酮基吡格列酮(M-Ⅲ)、羟基吡格列酮(M-Ⅳ)的方法。方法:血浆样品的处理采用乙腈沉淀法,定量方法采用内标法,内标为卡马西平。结果:吡格列酮、酮基吡格列酮、羟基吡格列酮定量下限分别为10.22,3.24,4.61ng.mL-1,线性范围分别为10.22～1 704.00,3.24～540.00,4.61～768.00ng.mL-1。各待测物批内和批间精密度RSD在1.89%～7.92%,准确度在92.09%～97.12%,提取回收率在71.63%～96.82%,内标的提取回收率为96.61%,无基质效应干扰,稳定性试验表明在试验条件下各待测物均保持稳定,符合生物样品分析要求。结论:本试验建立的方法可简单、快速、准确地测定人血浆中吡格列酮及其活性代谢物酮基吡格列酮、羟基吡格列酮,并已成功地用于吡格列酮在人体中的药动学研究。
Objective: To establish a method for the determination of pioglitazone (PIO) and its active metabolites ketopaglitazone (M-Ⅲ) and hydroxy pioglitazone (M-Ⅳ) in human plasma by liquid chromatography-tandem mass spectrometry. Methods: Plasma samples were treated with acetonitrile precipitation method, quantitative method using internal standard method, the internal standard of carbamazepine. Results: The lower limit of quantification of pioglitazone, ketopiglitazone and hydroxy pioglitazone was 10.22,3.24,4.61ng.mL-1, respectively. The linear range was 10.22-1 704.00,3.24-540.00,4.61-768.00ng.mL-1. The intra-assay and inter-assay RSDs ranged from 1.89% to 7.92% with accuracy of 92.09% -97.12%, extraction recoveries ranged from 71.63% to 96.82%, internal standard recoveries of 96.61% and no matrix effects Interference, stability tests showed that under the conditions of the test substances were stable, in line with biological sample analysis requirements. Conclusion: The method established in this study can be used to determine pioglitazone and its active metabolites pioglitazone and hydroxy pioglitazone in human plasma easily, rapidly and accurately, and has been successfully used in the study of pharmacokinetics of pioglitazone in human.