补中益气丸的毛细管电泳指纹图谱研究

Capillary electrophoresis fingerprint of Buzhong Yiqi Wan

目的建立补中益气丸(Buzhong Yiqi Wan,BZYQW)毛细管区带电泳指纹图谱,并采用内标法测定甘草次酸含量。方法以50mmol.L-1硼砂-150mmol.L-1磷酸二氢钠-50mmol.L-1磷酸氢二钠(体积比为1∶1∶1)为背景电解质(BGE)溶液,采用未涂层石英毛细管(75cm×75μm,有效长度63cm),以色谱指纹图谱指数F为目标函数优化试验条件,优化出运行电压为11kV,紫外检测波长265nm,重力进样20s(高度10cm)。以10批BZYQW为基础,以甘草次酸峰为参照物峰,确定15个共有指纹峰,建立了BZYQW-CEFP。结果10批BZYQW质量由极好到劣依次可分为1、2、3、4、5、6、7、8级,采用系统指纹定量法评价出S4、S9和S10质量极好(1级),S5质量很好(2级),S3、S6、S7和S8质量好(3级),S1质量中(5级),S2质量次(7级)。选用萘普生作内标,测定甘草次酸在10～100μg.mL-1时线性关系良好,相关系数r=0.999 6,平均回收率为98.2%(n=6)。结论基于整体化学指纹综合定量分析与指标成分定量分析相结合能便捷有效地评价中药质量。

Objective To establish the HPCE fingerprints of Buzhong Yiqi Wan （BZYQW） by capillary zone electrophoresis （CZE） and determine the content of hydroxyglycyrrhetic acid in BZYQW by internal standard method. Methods The electrophoretic separation was performed on a 75 crux 75 μm （with effective length of 63 cm） uncoating fused silica capillary with 50 mmol .L -1 sodium borate-150 mmol.L-1 NaH2PO4-50 mmol . L-1 Na2HPO4 （1 ： 1 ： 1, v/v） as the background electrolyte. Index of the chromatographic fingerprints （F） was applied to optimize the CEFP conditions. The running voltage was 11 kV, and the detection wavelength was 265 nm injecting for 20 s （10 cm） . Based on 10 batches of BZYQW, 15 co-possessing peaks were selected by choosing hydroxyglycyrrhetie acid peak as the referential peak and BZYQW-CEFP was produced. Results The quality of BZYQW was divided into 8 grades from the excellent to the inferior. The quality of S4, S9 and $10 was grade 1; that of S5 was grade 2; of S3, S6, S7 and S8 was grade 3; of S1 was grade 5; and of S2 was grade 7. With naproxen as the internal standard, the standard curve was linear at 10-100 μg . mL-1 with a correlation coefficient 0. 999 6. The average recovery was 98.2%（n=6）. Conclusion The combination of quantitative analysis of the overall chemical fingerprint and determination of special components is convenient and effective to evaluate the quality of traditional Chinese medicine.