高效液相色谱法测定血浆中米非司酮  

Determination of Mifepristone in Human Plasma by High Performance Liquid Chromatography

作　　者：郭智勇[1] 魏丹毅[1] 储成顶[2] 尹耕心 贺明莉[3] 吴建力 傅克勤 

机构地区：[1]宁波大学材料科学与化学工程学院宁波市新型功能材料及其制备科学实验室-省部共建国家重点实验室培育基地,宁波315211 [2]安徽医科大学公共卫生学院,合肥230032 [3]安徽省计划生育研究所,合肥230031

出　　处：《理化检验（化学分册）》2007年第1期15-17,20,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省科技厅科技攻关项目(2006C33065);安徽省人口和计划生育委员会专项基金;安徽省教育厅自然科学基金(2005KJ251)资助

摘　　要：建立了测定血浆中米非司酮浓度的高效液相色谱分析方法。血浆样品以乙醚提取,常温下负压挥发至干,所得残渣用甲醇浸溶后进行测定。Spherisorb C18（250 mm×4.6 mmi.d.,5μm）为色谱柱,流动相为甲醇-乙腈-水（50＋25＋25）溶液,检测波长为302 nm,用外标法定量。结果表明,在0.05~10.00 mg.L^-1范围内呈线性,检出限为0.01 mg.L^-1;平均回收率为98.2%,日内、日间平均精密度分别为7.0%,8.3%。米非司酮血浆样品的萃后残渣于-20℃可保存至少7d。An method for the determination of mifepristone in human plasma by high performance liquid chromatography was developed and validated. The plasma sample was extracted with ether which was removed by evaporation at room temperature under reduced pressure. The residue was taken up with methanol and the solution obtained was submitted to analysis by RP-HPLC. The chromatographic column of spherisorb C18 （250 mm × 4.6 mm,i d. 5 μm） was used in the analysis, and a solution containing methanol, aeetonitrile and water mixed in the proportion of 50 to 25 to 25 was used as the mobile phase, passing through the column. Volume of the volumetric loop used was 20 μL. Ultra violet speetrophotometrie detection was made at the wavelength of 302 nm with determination by the external standard method. Mifepristone was well separated in the HPLC, thus leading to high selectivity of determination. Linear relationship between the absorbanee and concentration of mifepristone was obtained in the range of 0. 05 to 10. 00 mg · L^-1 with a detection limit of 0. 01 mg· L^-1. Value of average recovery obtained by the recovery test was 98. 2%. Precision test was made at 3 different concentration levels, average values of RSD＇s （n=5） of within day test and between-day test obtained were 7. 0% and 8. 3% respectively. Residue of the sample obtained after extraction with ether and removal of ether by evaporation was proved to be stable for at least 7 days when preserved at -20 ℃ in the dry state.

关 键 词：高效液相色谱法 米非司酮 人血浆 血药浓度 

分 类 号：O657.7[理学—分析化学]