Li Jinglai, Zhang Zhenqing, Ruan Jinxiu, Wang Sujun, Liu Keliang
Beijing Institute of Pharmacology and Toxicology, Beijing, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Aug 15;855(2):180-5. doi: 10.1016/j.jchromb.2007.04.046. Epub 2007 May 16.
A sensitive and selective liquid chromatographic-tandem mass spectrometric (LC-MS/MS) method was developed for the determination of serial chiral novel anticholinergic compounds of phencynonate in rat plasma. After a simple protein-precipitation using methanol, the post-treatment samples were separated on a CAPCELL UG120 column with a mobile phase of a mixture of methanol and water (35:65) containing 0.1% formic acid. The serial chiral analytes and internal standard (IS) were all detected by the use of selected reaction monitoring mode (SRM). The method of all serial chiral analytes developed was validated in rat plasma with a daily working range of 0.5-100 ng/ml with correlation coefficient, R(2) > or = 0.99 and a sensitivity of 0.5 ng/ml as lower limit of quantification, respectively. This method was fully validated for the accuracy, precision and stability studies for all serial chiral analytes. The method proved to be accurate and specific, and was applied to the pharmacokinetic study of serial chiral novel anticholinergic compounds of phencynonate in rat plasma.
建立了一种灵敏且选择性高的液相色谱-串联质谱(LC-MS/MS)法,用于测定大鼠血浆中苯环壬酯系列手性新型抗胆碱能化合物。使用甲醇进行简单的蛋白沉淀后,处理后的样品在CAPCELL UG120柱上分离,流动相为含0.1%甲酸的甲醇和水(35:65)混合物。所有系列手性分析物和内标(IS)均采用选择反应监测模式(SRM)进行检测。所建立的所有系列手性分析物的方法在大鼠血浆中进行了验证,每日工作范围为0.5-100 ng/ml,相关系数R(2)≥0.99,定量下限灵敏度为0.5 ng/ml。该方法针对所有系列手性分析物的准确性、精密度和稳定性研究进行了全面验证。该方法被证明准确且特异,并应用于大鼠血浆中苯环壬酯系列手性新型抗胆碱能化合物的药代动力学研究。