HPLC-MS/MS_测定人血浆中米格列奈钙的浓度___

 

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-C₁₈反相色谱柱 (2.1 mm×150 mm，3.5 μm) 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,sensitive method of high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) for determination of mitiglinide calcium in human plasma.Method:The internal standard is repaglinide,the plasma samples were deposited by acetonitrile directly,then the analytes were separated by using Agilent-C₁₈ (2.1 mm×150 mm,3.5 μm) column,the mobile phase consisted of acetonitrile-methanol-water (70∶20∶10),the column temperature was 20 ℃,the flow rate was 0.2 mL·min^-1.Mitiglinide calcium was quantitated by multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI-).Results:The minimal detectable plasma drug concentration was 2 ng·mL^-1 (S/N≥ 3),the calibration curve was linear in the range of 10-4000 ng·mL^-1,with coefficient of determination 0.9994.The average recovery was between 97.8% and 104.9%.Intra-day and inter-day RSDs were less than 10% (n=6).Conclusion:The method is simple,sensitive and accurate.It is suitable for the study of pharmacokinetics of mitiglinide calcium in human plasma.

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