de Oliveira Anderson Rodrigo Moraes, Cardoso Carmen Dickow, Bonato Pierina Sueli
Faculdade de Ciências Farmacêuticas de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto, São Paulo, Brazil.
Electrophoresis. 2007 Apr;28(7):1081-91. doi: 10.1002/elps.200600420.
Liquid-phase microextraction based on polypropylene hollow fibers and CE were applied for the chiral determination of hydroxychloroquine (HCQ) and its metabolites (desethylchloroquine, DCQ; desethylhydroxychloroquine, DHCQ; bisdesethylchloroquine, BDCQ) in human urine. The analytes were extracted from 3 mL of urine spiked with the internal standard (metoprolol) and alkalinized with 250 muL of 2 M NaOH. The analytes were extracted into 1-octanol impregnated in the pores of the hollow fiber, and into an acid acceptor solution inside the hollow fiber. The electrophoretic separations were carried out in 100 mmol/L Tris buffer (pH adjusted to 9.0 with phosphoric acid) containing 1% w/v S-beta-CD and 30 mg/mL HP-beta-CD with a constant voltage of +18 kV. The method was linear over the concentration range of 10-1000 ng/mL for each HCQ stereoisomer and 21-333 ng/mL for each metabolite stereoisomer. Within-day and between-day assay precision and accuracy for the analytes were studied at three concentration levels for each stereoisomer and were lower than 15%. The developed method was applied for the determination of the cumulative urinary excretion of HCQ, DCQ, and DHCQ after oral administration of rac-HCQ to a health volunteer. The results obtained are in agreement with previous literature data.
基于聚丙烯中空纤维的液相微萃取和毛细管电泳被应用于人体尿液中羟氯喹（HCQ）及其代谢物（去乙基氯喹，DCQ；去乙基羟氯喹，DHCQ；双去乙基氯喹，BDCQ）的手性测定。将分析物从3 mL加有内标（美托洛尔）并用250 μL 2 M氢氧化钠碱化的尿液中萃取出来。分析物被萃取到中空纤维孔中浸渍的1-辛醇中，并进入中空纤维内部的酸接受溶液中。电泳分离在含有1% w/v S-β-环糊精和30 mg/mL HP-β-环糊精的100 mmol/L Tris缓冲液（用磷酸将pH调节至9.0）中进行，恒定电压为+18 kV。该方法对于每种HCQ立体异构体在10 - 1000 ng/mL的浓度范围内呈线性，对于每种代谢物立体异构体在21 - 333 ng/mL的浓度范围内呈线性。对每种立体异构体在三个浓度水平上研究了分析物的日内和日间测定精密度和准确度，均低于15%。所建立的方法被应用于对一名健康志愿者口服消旋HCQ后HCQ、DCQ和DHCQ的累积尿排泄量的测定。获得的结果与先前的文献数据一致。
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