新复方珍珠膏的质量控制研究

Quality control study in xinfufangzhenzhugao

目的:研究新复方珍珠膏的质量控制方法。方法:新复方珍珠膏中猪胆粉的薄层色谱(TLC)以胆酸、猪去氧胆酸和鹅去氧胆酸为对照品,异辛烷-乙醚-冰醋酸-正丁醇-水(10∶5∶5∶3∶1)的上层溶液为展开剂进行鉴别。新复方珍珠膏中猪胆粉的牛磺猪去氧胆酸含量以高效液相色谱法(HPLC)进行测定:采用LC-20AT岛津高效液相色谱仪,SPD-20A检测器;色谱柱为Agilent ZORBAX SB-C_(18)(5μm×4.6 mm×250 mm);流动相为乙腈-0.03 mol·L^(-1)磷酸二氢钠(磷酸调pH=4.4),梯度洗脱,检测波长200 nm,体积流量1.0 m L·min^(-1),进样量10μL,柱温25℃。结果:薄层色谱中猪去氧胆酸、鹅去氧胆酸、胆酸分离良好。牛磺猪去氧胆酸在0.095 2~1.904 0μg范围内线性关系良好(r=0.999 9),方法回收率为99.45%,RSD=2.41%(n=6)。结论:对新复方珍珠膏中猪胆粉的鉴别及含量测定方法简便合理,可用于新复方珍珠膏的质量控制。

Objective： To establish a quality control method for xinufangzhenzhugao plaster. Methods： TLC：the upper solution of new prepared isooctane-ether-acetic acid-butanol-water（10∶5∶5∶3∶1） as developer for TLC. HPLC：an Agilent ZORBAX SB-C（18） column（5 μm×4.6 mm×250 mm）was employed, the mobile phase of acetonitrile-0.03mol·L^（-1） sodium dihydrogen phosphate was used at the flow rate 1.0 mL·min^（-1） and the signal was detected at 200 nm and the column temperature was 25℃ for HPLC. Results： The components were well separated on silica gel G plate. Taurohyodeoxycholic acid had good linear relationships in the ranges of 0.095 2-1.904 0 μg（r=0.999 9）, The average recovery were 99.45%. The RSD was 2.41%（n=6）. Conclusion： This method is simple and reliable,which is suitable for the quality control of xinfufangzhenzhugao.