Rp－HPLC法测定血清中的抗生育甾体药物利洛司酮  

DETERMINATION OF THE PROGESTERONE ANTAGONlST LILOPRISTONE IN SERUM BY RP-PLC

作　　者：余琛[1] 张慧[1] 洪有采[1] 包淳洋 武镇忆 丁训诚 

机构地区：[1]上海市徐汇区中心医院,上海计划生育科学研究所

出　　处：《药学学报》1995年第6期449-453,共5页Acta Pharmaceutica Sinica

摘　　要：以ＲＵ４８６为内标，建立了血清样品中新型抗孕激素甾体药物利洛司酮（ｌｉｌｏｐｒｉｓｔｏｎｅ）的反相高效液相色谱法。色谱分析条件为μＢｏｎｄａｐａｋＣ１８柱１０μｍ，３００ｍｍ×３．９ｍｍＩＤ；流动相为甲醇－二氯甲烷－１０ｍｍｏｌ·Ｌ－１磷酸盐缓冲液（ｐＨ４．０）（６７：５：２８ｖ／ｖ）；紫外检测波长为３０２ｎｍ。利洛司酮的检测限为１ｎｇ（Ｓ／Ｎ≥４：１）。血清样品经二次液一液超声振荡萃取后，得到了较好的净化。血清样品中利洛司酮的方法回收率为１０３．３％，日内精密度及日间精密度平均ＲＳＤ为３．５１％及２．９２％。在浓度为１０～１０００ｎｇ·ｍｌ－１血清范围内呈线性关系。To 1.0 ml of serum containing lilopristone were added RU486 solution(internal standard, IS)and 1 ml of 1.0mol·L-1 NaOH. The mixture was extracted with diethyl ether for 2 times.After extraction ,the combined organic phase was evaporated to dryness and the residue was dissolved in the mobile phase and washed with petroleum ether.After centrifugation,20 μl of the lower layer was subjected to HPLC,A μBondapak-C18(10μm)column(30 cm × 3. 9 mm) was used and the column temperature was kept at 50℃, The flow rate of mobile phase(methanol- dichloromethane-0.01mol·L-1 phosphate buffer,pH 4.0,67:5:28v/v)was 1.1 ml· min-1 and UV detection was performed at 302 nm. The retention times of lilopristone and IS were 6.85 and 9. 07 min respectively and the detection limit was 10 ng·ml-1(S/N≥4 )serum. The extraction recoveries of lilopristone and IS were over 85%. The relative standard deviations were2.21 to 4.23%, This method has been applied to study the pharmacokinetic of lilopristone in rats.

关 键 词：高效液相色谱 利洛司酮 血药浓度 避孕药 

分 类 号：R969.1[医药卫生—药理学] R979.21[医药卫生—药学]