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目的建立LC-MS/MS法测定小鼠组织中马尼地平的浓度。方法组织样品用甲基叔丁基醚提取,Agilient-TC-C18柱分离;流动相为甲醇-乙腈-1mmol·L-1醋酸铵(含体积分数为0.05%的甲酸溶液)(体积比为70∶15∶15),流速为0.5mL·min-1;质谱:采用多反应检测模式,正离子方式检测。结果马尼地平的质量分数在1.0×10-8~1.0×10-6内线性关系良好;定量下限为1.0×10-8;日间日内精密度(relative standard deviation,RSD)均不大于12.2%,准确度(relative error,RE)为0.48%~3.36%。马尼地平在小鼠组织内分布迅速、广泛。结论该法适合于小鼠组织中马尼地平的含量测定,并为马尼地平的进一步临床研究奠定基础。
Objective To establish a method for the determination of manidipine in mouse tissues by LC-MS / MS. Methods Tissue samples were extracted with methyl tert-butyl ether and separated on a Agilient-TC-C18 column. The mobile phase consisted of methanol-acetonitrile-1mmol·L-1 ammonium acetate (containing formic acid solution with a volume fraction of 0.05% : 15:15), the flow rate of 0.5mL · min-1; mass spectrometry: multi-reaction detection mode, positive ion detection. Results Manidipine showed a good linearity within 1.0 × 10-8 ~ 1.0 × 10-6 with a lower limit of quantitation of 1.0 × 10-8. The relative standard deviations (RSDs) were not more than 12.2% , The relative error (RE) was 0.48% ~ 3.36%. Manidipine is rapidly and widely distributed in mouse tissues. Conclusion This method is suitable for the determination of the content of manidipine in mouse tissues and lay the foundation for the further clinical study of manidipine.