Stereoselective determination of hydroxychloroquine and its metabolites in human urine by liquid-phase microextraction and CE

✍ Scribed by Anderson Rodrigo Moraes de Oliveira; Carmen Dickow Cardoso; Pierina Sueli Bonato

• Publisher: John Wiley and Sons
• Year: 2007
• Tongue: English
• Weight: 473 KB
• Volume: 28
• Category: Article
• ISSN: 0173-0835
• DOI: 10.1002/elps.200600420

✦ Synopsis

Abstract

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 μL 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‐β‐CD and 30 mg/mL HP‐β‐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.