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高效液相色谱法对生物流体中甲氟喹的立体特异性测定

Stereospecific determination of mefloquine in biological fluids by high-performance liquid chromatography.

作者信息

Souri E, Farsam H, Jamali F

机构信息

Department of Medicinal Chemistry, Faculty of Pharmacy, University of Medical Sciences, Tehran, Iran.

出版信息

J Chromatogr B Biomed Sci Appl. 1997 Oct 24;700(1-2):215-22. doi: 10.1016/s0378-4347(97)00322-8.

Abstract

A sensitive stereoselective HPLC method was developed for determination of mefloquine (MFQ) enantiomers in plasma, urine and whole blood. The assay involved liquid-liquid extraction of MFQ from biological fluids with a mixture of hexane and isopropanol in the presence of sodium hydroxide and derivatization of the residue by (+)-(S)-naphthylethylisocyanate (NEIC) as chiral derivatizing reagent. Separation of the resulting diastereomers was performed on a silica normal-phase column using chloroform-hexane-methanol (25:74:1) as the mobile phase with a flow-rate of 1 ml/min. Using 200 microl of plasma or whole blood, the limit of determination was 0.2 microg/ml with UV detection for both enantiomers. The limit of determination in 500 microl of urine was 0.08 microg/ml with UV detection.

摘要

建立了一种灵敏的立体选择性高效液相色谱法,用于测定血浆、尿液和全血中的甲氟喹(MFQ)对映体。该测定方法包括在氢氧化钠存在下,用己烷和异丙醇的混合物从生物流体中液-液萃取MFQ,并用(+)-(S)-萘基异氰酸酯(NEIC)作为手性衍生试剂对残留物进行衍生化。所得非对映异构体在硅胶正相柱上进行分离,以氯仿-己烷-甲醇(25:74:1)为流动相,流速为1 ml/min。使用200微升血浆或全血,两种对映体的紫外检测测定限均为0.2微克/毫升。500微升尿液中的紫外检测测定限为0.08微克/毫升。

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