LC-MS/MS定量测定人体血浆中氨氯地平浓度

Quantitative Determination of the Amlodipine Concentration in Healthy Human Plasma by LC-MS/MS

目的：建立定量测定人体血浆中氨氯地平浓度的HPLC-MS/MS的方法。方法：以克林霉素为内标,采用Shim-pack VP-ODS柱（150×2.0 mm I.D.,5μm,日本Shimadzu Technologies Inc.公司）为固定相;乙腈-10 mmol/L乙酸铵溶液（90：10,v/v）为流动相,流速为0.4 mL/min;通过电喷雾离子源（ESI）,以正离子多反应监测模式进行检测。氨氯地平与内标用于检测的离子对分别为m/z409.3 m/z 238.2和m/z 425.2 m/z 126.3。结果：氨氯地平在0.10~20.00 ng/mL范围内与峰面积比值线性范围良好（r=0.9968）,定量下限为0.10 ng/mL,日内日间精密度的RSD均小于7%,平均回收率大于86%。结论：所建方法准确度较高,灵敏度好,专属性强且操作简便,可适用于氨氯地平的血药浓度测定和临床药代动力学研究。

Objective： To establish the HPLC-MS/MS method to determine the concentration of amlodipine in healthy human plasma.Methods： Clindamycin was used as internal standard,Shim-pack VP-ODS（150×2.0 mm I.D.,5 μm,Shimadzu Technologies Inc.,Japan）was used as immobile phase and Acetonitrile-10 mmol/L ammonium acetate aqueous solution was used as mobile phase,the flow rate was 0.3 mL/min;Electrospray ionization（ESI） source was applied,and multiple reaction monitoring（MRM） mode was operated in the positive mode with the monitor ions at m/z 409.3 m/z 238.2 for amlodipine and m/z 425.2 m/z 126.3 for clindamycin.Results： The calibration curve for plasma atorvastatin was linear in the range of 0.10~20.00 ng/mL（r=0.9968）,the lower limitation of quantization was 0.10 ng/mL,the inter-and intra-day precision（RSD） were both less than 7%.The average recovery rate was above 86 %.Conclusions： The HPLC-MS/MS method is accurate,sensitive,specific and convenient,and could be used in the determination of plasma amlodipine concentration and the clinical study of its pharmacokinetics.