Pawula M, Watson D, Teramura T, Watanabe T, Higuchi S, Cheng K N
Huntingdon Life Sciences Ltd., Cambridgeshire, UK.
J Chromatogr B Biomed Sci Appl. 1998 Nov 20;719(1-2):113-23. doi: 10.1016/s0378-4347(98)00413-7.
A sensitive and specific LC-MS-MS assay has been developed and validated for barnidipine (1-benzyl-3-pyrrolidinyl)methyl-2,6-dimethyl-4(m-nitrophenyl)-1,4-dihydr opyridine-3,5-dicarboxylate). The assay involves a simple and rapid solid-phase extraction procedure. Sample analysis was on a Spherisorb S3ODS2 100 mmX2 mm I.D. column, with a Finnigan TSQ 7000 mass spectrometer, using an electrospray interface and selective reaction monitoring (SRM). The intra- and inter-day precision and accuracy, determined as the coefficient of variation and relative error, respectively, were 11.8% or less. The limit of quantitation was 0.03 ng/ml, and the calibration was linear between 0.03 and 3.0 ng/ml. The method has been used successfully for the measurement of over two thousand human plasma samples from pharmacokinetic clinical trials.
已开发并验证了一种灵敏且特异的液相色谱-串联质谱(LC-MS-MS)测定法,用于测定巴尼地平(1-苄基-3-吡咯烷基)甲基-2,6-二甲基-4-(间硝基苯基)-1,4-二氢吡啶-3,5-二羧酸酯)。该测定法涉及一种简单快速的固相萃取程序。样品分析在一根Spherisorb S3ODS2 100 mm×2 mm内径的色谱柱上进行,使用Finnigan TSQ 7000质谱仪,采用电喷雾接口和选择性反应监测(SRM)。日内和日间精密度及准确度,分别以变异系数和相对误差表示,均在11.8%或更低。定量限为0.03 ng/ml,校准在0.03至3.0 ng/ml之间呈线性。该方法已成功用于药代动力学临床试验中两千多份人体血浆样品的测定。