论文部分内容阅读
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 a method for the quantitative determination of amlodipine in human plasma by HPLC-MS / MS. METHODS: Clindamycin was used as internal standard and Shim-pack VP-ODS column (150 × 2.0 mm ID, 5 μm, Shimadzu Technologies Inc., Japan) was used as stationary phase. Acetonitrile-10 mmol / L ammonium acetate solution : 10, v / v) as the mobile phase at a flow rate of 0.4 mL / min. The electrospray ionization source (ESI) was used for the detection of positive ion multi-reaction monitoring. The ion pairs used for the detection of amlodipine and the internal standard were m / z 409.3 m / z 238.2 and m / z 425.2 m / z 126.3, respectively. RESULTS: Amlodipine showed a good linearity (r = 0.9968) over the range of 0.10-20.00 ng / mL with a lower limit of quantification of 0.10 ng / mL. The RSDs of intra-day and inter-day precision were all less than 7%. The average recovery Greater than 86%. Conclusion: The proposed method has high accuracy, good sensitivity, specificity and simple operation, and is suitable for the determination of amlodipine and clinical pharmacokinetics.