Yasuda T, Tanaka M, Iba K
Research Center, Sumitomo Pharmaceuticals Co. Ltd., Osaka, Japan.
J Mass Spectrom. 1996 Aug;31(8):879-84. doi: 10.1002/(SICI)1096-9888(199608)31:8<879::AID-JMS373>3.0.CO;2-F.
A sensitive and specific liquid chromatographic method coupled with tandem mass spectrometry was developed for the quantification of amlodipine in human and rat serum, which is a dihydropyridine derivative with calcium antagonist activity. An atmospheric pressure chemical ionization interface was used as the ion source and the analysis was performed in the selected reactive monitoring (SRM) mode. Deuterated amlodipine was used as the internal standard, and serum samples were treated with diethyl ether extraction prior to analysis. Serum levels in the range 0.014-7.2 ng ml-1 were measured accurately by this method, and the lower limit of quantitation (LOQ) was 0.014 ng ml-1 using 1 ml of human serum. The accuracy was within 7% of the expected values. The intra-assay precision was less than 3% and the inter-assay precision was less than 6%. The method was applied to a pharmacokinetic study of amlodipine in rats, in which the measurable range was 0.14-72 ng ml-1 using 0.1 ml of serum because of a limitation on the sample volume.
建立了一种灵敏且特异的液相色谱-串联质谱法，用于定量测定人血清和大鼠血清中的氨氯地平，氨氯地平是一种具有钙拮抗剂活性的二氢吡啶衍生物。采用大气压化学电离接口作为离子源，分析在选择反应监测（SRM）模式下进行。氘代氨氯地平用作内标，血清样品在分析前用乙醚萃取处理。该方法可准确测定0.014 - 7.2 ng/ml范围内的血清水平，使用1 ml人血清时定量下限（LOQ）为0.014 ng/ml。准确度在预期值的7%以内。批内精密度小于3%，批间精密度小于6%。该方法应用于氨氯地平在大鼠体内的药代动力学研究，由于样品体积限制，使用0.1 ml血清时可测量范围为0.14 - 72 ng/ml。
