固相萃取-高效液相色谱法测定泻痢固肠片中芍药苷、甘草苷、橙皮苷的含量

Determination of paeoniflorin, liquiritin and hesperidin in Xieli Guchang tablets by SPE-HPLC

目的建立固相萃取-高效液相色谱同时测定泻痢固肠片中芍药苷、甘草苷、橙皮苷含量的方法。方法采用固相萃取对泻痢固肠片中的有效成分进行净化、富集,用高效液相色谱法测定含量。色谱柱为Kromasil C_(18)柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%磷酸溶液(24∶76),检测波长230、284 nm,柱温25℃,进样量20μL,流速1 mL·min^(-1)。结果芍药苷、甘草苷、橙皮苷分别在3.998~199.9μg·mL^(-1)(r=1.000)、0.6356~31.78μg·mL^(-1)(r=0.9999)、0.4940~24.70μg·mL^(-1)(r=0.9998)线性关系良好,平均回收率(n=6)分别为98.6%、97.0%、98.0%,RSD分别为0.34%、0.63%、0.62%。结论该方法操作简单,结果准确,可用于泻痢固肠片中芍药苷、甘草苷、橙皮苷有效成分的含量测定。

Objective To establish a solid-phase extraction with high-performance liquid chromatography（SPEHPLC） method for the determination of paeoniflorin, liquiritin and hesperidin in Xieli Guchang tablet. Methods Using solid-phase extraction to purified and enriched the active ingredients of Xieli Guchang tablet. The contents was analyzed by HPLC method with Kromasil C_（18） column（4.6 mm×250 mm, 5 μm）. The mobile phase composed of acetonitrile and 0.1% phosphoric acid（24∶76）. Detection wavelength were set at 230 nm and 284 nm. The column temperature was maintained at 25 ℃, and injection volume was 20 μL. The flow rate was 1.0 mL· min^（-1）. Results The calibration curves of paeoniflorin, liquiritin and hesperidin respectively showed good linearity within 3.998- 199.9 μg·mL（-1）（r = 1.000）, 0.6356- 31.78 μg·mL（-1）（r = 0.9999）, 0.4940-24.70 μg· mL（-1）（r = 0.9998）. The average recoveries of these were 98.6%, 97.0%, 98.0%, respectively. RSDs were 0.34%, 0.63%, 0.62%, respectively. Conclusion The method is simple, accurate, which can be used for the quality control of paeoniflorin, liquiritin and hesperidin in Xieli Guchang tablet.