dos Santos Magalhães Igor Rafael, Sueli Bonato Pierina
Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, São Paulo, Brazil.
J Sep Sci. 2008 Sep;31(16-17):3106-16. doi: 10.1002/jssc.200800320.
A selective method using three-phase liquid-phase microextraction (LPME) in conjunction with LC-MS-MS was devised for the enantioselective determination of chloroquine and its n-dealkylated metabolites in plasma samples. After alkalinization of the samples, the analytes were extracted into n-octanol immobilized in the pores of a polypropylene hollow fiber membrane and back extracted into the acidic acceptor phase (0.1 M TFA) filled into the lumen of the hollow fiber. Following LPME, the analytes were resolved on a Chirobiotic V column using methanol/ACN/glacial acetic acid/diethylamine (90:10:0.5:0.5 by volume) as the mobile phase. The MS detection was carried out using multiple reaction monitoring with ESI in the positive ion mode. The optimized LPME method yielded extraction recoveries ranging from 28 to 66%. The method was linear over 5-500 ng/mL and precision (RSD) and accuracy (relative error) values were below 15% for all analytes. The developed method was applied to the determination of the analytes in rat plasma samples after oral administration of the racemic drug.
设计了一种使用三相液相微萃取（LPME）结合液相色谱-串联质谱（LC-MS-MS）的选择性方法，用于对血浆样品中氯喹及其正烷基代谢物进行对映体选择性测定。样品碱化后，分析物被萃取到固定在聚丙烯中空纤维膜孔中的正辛醇中，然后反萃取到填充在中空纤维内腔的酸性接受相（0.1 M 三氟乙酸）中。液相微萃取后，使用甲醇/乙腈/冰醋酸/二乙胺（体积比为90:10:0.5:0.5）作为流动相，在Chirobiotic V柱上分离分析物。质谱检测采用电喷雾电离正离子模式下的多反应监测。优化后的液相微萃取方法的萃取回收率在28%至66%之间。该方法在5 - 500 ng/mL范围内呈线性，所有分析物的精密度（相对标准偏差）和准确度（相对误差）值均低于15%。所建立的方法应用于对消旋药物口服给药后大鼠血浆样品中分析物的测定。
