Rp-HPLC法测定血清中的抗生育甾体药物利洛司酮

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。

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

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.