高效液相色谱法测定人血浆中磷酸哌喹  

HPLC determination of piperaquine phosphate in human plasma

作　　者：刘昌辉[1] 黄天来[1] 洪馨[1] 宓穗卿[1] 王宁生[1] 

机构地区：[1]广州中医药大学临床药理研究所,广州510405

出　　处：《药物分析杂志》2007年第1期63-65,共3页Chinese Journal of Pharmaceutical Analysis

基　　金：世界卫生组织资助项目(ICP/MVP/022 AC:01.01.rg.08);广东省自然基金项目(04010030)

摘　　要：目的:建立人血浆中磷酸哌喹的高效液相色谱紫外检测法。方法:以1 mol·L^(-1)氢氧化钠溶液碱化血浆样品,乙醚萃取,吸取有机相,N_2气流吹干后,流动相复溶;采用 Alltima C_(18)柱(4.6 mm×150 mm,5μm),流动相为乙腈-0.1%(w/v)三氯乙酸-磷酸(25∶75∶0.035,v/v/v),流速0.4 mL·min^(-1),柱温为室温,检测波长345 nm,以磷酸氯喹为内标,进样分析。结果:磷酸哌喹、内标和内源性杂质分离良好,线性范围0.02～1.0μg·mL^(-1)(r=0.9993),定量下限为0.01μg·mL^(-1),日内、日间RSD 小于12%,提取回收率为69.3%～76.3%,方法回收率为93.4%～106.5%。结论:该法准确、稳定,灵敏度高,适用于磷酸哌喹药物动力学及生物利用度的研究。Objective：To establish a sensitive assay method for determination of piperaquine phosphate in human plasma. Method：Chloroquine phosphate as the internal standard, the plasma was alkalized by 1 mol · L-1 sodium hydroxide and extracted with ether, then the organic phase was evaporated to dry thoroughly with soft stream of N2 at 35 ℃, and the residues were reconstituted with 20 μL mobile phase. The reconstitution was chromatographed on the AUtima C18 column （4. 6 mm × 150 mm ,5μm）at ambient temperature with mobile phase acetonitrile -0. 1% （w/v） trichloroacetic acid solution -phosphoric acid（25： 75： 0. 035 ,v/v/v） ,the flow rate was 0. 4 mL · min^-1 and detected at 345 nm. Results： Piperaquine phosphate was well detected in plasma apart from endogenous. The linear range of piperaquine phosphate plasma concentration was 0. 02 - 1.0 μg · mL^-1 （r = 0. 9993 ）, and the lowest limit of detection was 0. 01 μg · mL^-1. The method recovery of piperaquine phosphate was 93.4% - 106. 5% and the extraction recovery was 69. 3% -76. 3% ,the RSDs of intra - day and inter - day were less than 12% for assay respectively. Conclusion：The method has good specificity, reproducibility and high sensitivity and it can be applied to determine the piperaquine phosphate plasma concentrations accurately.

关 键 词：磷酸哌喹 血药浓度 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]