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目的建立液质联用色谱法(LC-MS-MS)测定人血浆中米格列奈(mitiglinide)浓度。方法空白血浆加米格列奈,用乙腈做为沉淀剂,取上清液用于LC-MS-MS分析。分析柱为日本资生堂CAPCELL PAK C18 MG5,μm150 mm×2.0 mm(ID)柱,流动相为乙腈-10 mmol/L乙酸铵(0.1%氨水)分段洗脱(0～2 min 10∶90,2.1～8 min 90∶10,8.1～10 min 10∶90),流速为0.3 ml/min;质谱条件:电喷雾离子化电离源ESI负离子检测,喷雾电压(SP)4000 kV,鞘气(SGP)流速30 Arb,辅助气(AGP)流速0 Arb,毛细管温度(TEM)314℃;米格列奈和内标瑞格列奈的碰撞能量均分别为21 EV、23 EV;选择反应监测(SRM)分别测定米格列奈和内标瑞格列奈负离子m/z 314→189和m/z451→379.2。结果米格列奈在2.5～2000μg/L检测浓度范围内呈良好线性关系(R>0.99),最低定量限(LLOQ)为2.5μg/L,绝对回收率在70%以上,高中低3种浓度的日内和日间RSD≤15%。结论该方法操作简便、灵敏、准确,适用于临床米格列奈的血药浓度监测及其药动学研究。
Objective To establish a method for the determination of mitiglinide in human plasma by liquid chromatography-mass spectrometry (LC-MS-MS). Methods Blank plasma gaglinide, with acetonitrile as precipitant, the supernatant was used for LC-MS-MS analysis. The analytical column was a CAPCELL PAK C18 MG5, μm 150 mm × 2.0 mm column with a mobile phase of acetonitrile-10 mmol / L ammonium acetate (0.1% ammonia) ~ 8 min 90:10, 8.1-10 min 10:90) at a flow rate of 0.3 ml / min. Mass spectrometry conditions: Electrospray ionization Ionization ESI negative ion detection, Spray voltage (SP) 4000 kV, Sheath gas 30 Arb, AGP flow rate 0 Arb and capillary temperature (TEM) 314 ℃ respectively. The collisional energies of mitiglinide and repaglinide were 21 EV and 23 EV, respectively. The selective reaction monitoring (SRM) Mitiglinide and the internal standard repaglinide anions were determined for m / z 314 → 189 and m / z 451 → 379.2. Results Mitiglinid showed a good linearity (R> 0.99) in the concentration range of 2.5-2000μg / L, the lowest limit of quantitation (LLOQ) was 2.5μg / L, the absolute recovery was above 70% The days and days RSD ≤ 15%. Conclusion The method is simple, sensitive and accurate and is suitable for the clinical monitoring and pharmacokinetic study of mitiglinide.