Chaulet J F, Grelaud G, Bellemin-Magninot P, Mounier C, Brazier J L
Laboratoire de Biochimie du Professeur Lemontey, Hôpital d'Instruction des Armées Desgenettes, Lyon, France.
J Pharm Biomed Anal. 1994 Jan;12(1):111-7. doi: 10.1016/0731-7085(94)80018-9.
A reversed-phase ion-pair high-performance liquid chromatographic method with ultraviolet detection is described for the simultaneous measurement of chloroquine, proguanil and their major metabolites in human plasma, erythrocytes and urine. After a liquid-solid extraction on a Bond Elut C8 cartridge, the compounds are separated on a C8 Lichrospher 60 RP select B column by isocratic elution; the mobile phase is water-acetonitrile-methanol (78:28:4, v/v/v) with 0.5 M ammonium formate and 0.075 M perchloric acid. The eluent is monitored with an ultraviolet detector at 254 nm. The lower limits of quantification in plasma are near 6.0 ng ml-1 for chloroquine and near 9.0 ng ml-1 for proguanil. No chromatographic interference can be detected from endogenous compounds or from other antimalarial drugs. The method is accurate and precision is good with inter- and intra-assay relative standard deviations lower than 6.8% for plasma samples. N-(2-6 dichlorobenzylidene amino)guanidine is used as an internal standard. The chromatographic procedure takes 35 min and can be used for therapeutic drug monitoring and clinical studies.
本文描述了一种采用紫外检测的反相离子对高效液相色谱法,用于同时测定人血浆、红细胞和尿液中的氯喹、氯胍及其主要代谢产物。在Bond Elut C8柱上进行液固萃取后,化合物在C8 Lichrospher 60 RP select B柱上通过等度洗脱进行分离;流动相为水 - 乙腈 - 甲醇(78:28:4,v/v/v),含有0.5 M甲酸铵和0.075 M高氯酸。用紫外检测器在254 nm处监测洗脱液。血浆中氯喹的定量下限接近6.0 ng/ml,氯胍的定量下限接近9.0 ng/ml。未检测到内源性化合物或其他抗疟药物的色谱干扰。该方法准确,血浆样品的批内和批间相对标准偏差低于6.8%,精密度良好。N -(2 - 6二氯亚苄基氨基)胍用作内标。色谱过程耗时35分钟,可用于治疗药物监测和临床研究。