Bergqvist Y, Eckerbom S
J Chromatogr. 1981 Nov 13;226(1):91-7. doi: 10.1016/s0378-4347(00)84209-7.
A gas chromatographic method for the simultaneous determination of chloroquine and its metabolite desethylchloroquine in plasma described. Chloroquine, desethylchloroquine and internal standard are extracted as bases with n-hexane-pentanol (90:10) and then back-extracted to an acid aqueous phase. The aqueous phase is made alkaline and after re-extraction into chloroform and evaporation of the chloroform, acylation with trifluoroacetic anhydride is performed. Separation is achieved on an OV-17 column at 250 degrees C. Chloroquine and desethylchloroquine can be determined down to 0.1-0.2 mumol/l (30-60 ng/ml), with a coefficient of variation of 12%, using a nitrogen detector. The method shows good correlation (r = 0.98) with a recently developed liquid chromatographic method.
本文描述了一种气相色谱法,用于同时测定血浆中的氯喹及其代谢产物去乙基氯喹。氯喹、去乙基氯喹和内标物用正己烷 - 戊醇(90:10)作为碱进行萃取,然后反萃取到酸性水相中。将水相调至碱性,再萃取到氯仿中,氯仿蒸发后,用三氟乙酸酐进行酰化反应。在250℃的OV - 17柱上实现分离。使用氮检测器时,氯喹和去乙基氯喹的测定下限可达0.1 - 0.2μmol/l(30 - 60 ng/ml),变异系数为12%。该方法与最近开发的液相色谱法显示出良好的相关性(r = 0.98)。