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目的:建立一种简便、灵敏的测定人血浆中米格列奈钙浓度的高效液相色谱-串联质谱(HPLC-MS/MS)方法。方法:以瑞格列奈为内标,样品处理采用乙腈直接沉淀的方法,用Agilent-C_(18)反相色谱柱(2.1 mm×150 mm,3.5μm)进行分离,以乙腈-甲醇-水(70:20:10)为流动相,柱温20℃,流速0.2 mL·min~(-1)。采用电喷雾负离子化,多反应监测(MRM)进行定量分析。结果:米格列奈钙在10～4000 ng·mL~(-1)浓度范围线性关系良好,相关系数为0.9994;最低检测浓度为2 ng·mL~(-1)(S/N≥3)。日内与日间RSD均小于10%(n=6),方法回收率在97.8%～104.9%之间。结论:本方法简便快速、灵敏准确,适用于米格列奈钙在人体内的药代动力学研究。
Objective: To establish a simple and sensitive method for the determination of mitochondrial calcium in human plasma by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS). METHODS: Repaglinide was used as an internal standard. The samples were separated by direct acetonitrile precipitation on an Agilent-C 18 reversed-phase column (2.1 mm × 150 mm, 3.5 μm) using acetonitrile-methanol-water (70:20:10) as the mobile phase at a flow rate of 0.2 mL · min ~ (-1) at a column temperature of 20 ℃. Electrospray ionization and multiple reaction monitoring (MRM) were used for quantitative analysis. RESULTS: Mitiglinide showed a good linearity in the concentration range of 10-4000 ng · mL -1 with a correlation coefficient of 0.9994. The lowest concentration of 2 ng · mL -1 (S / N ≥ 3) . The daily and intraday RSD were less than 10% (n = 6), the recovery rate was between 97.8% and 104.9%. Conclusion: The method is rapid, sensitive and accurate and suitable for the study of the pharmacokinetics of mitiglinide in human.