HPLC梯度洗脱法测定利胆排石片中3组分的含量

目的：建立利胆排石片中黄芩苷、大黄素及大黄酚的含量测定方法。方法：采用HPLC梯度洗脱法，色谱柱：KromasilC18（250mm×4．6mm，5μm）；流动相以乙腈-磷酸盐缓冲液（磷酸0．24％，磷酸氢二钾6．30mmol·L^-1）梯度洗脱；检测波长256nm；流速：1．0ml·min^-1；柱温：35℃。结果：黄芩苷线性浓度范围为O．20-10．0lμg·ml^-1，r=0．9992，平均回收率为99．Ol％，RSD为0．67％（n=6），大黄素线性浓度范围为0．37-18．41μg·ml^-1，r=0．9991，平均回收率为99．37％，RSD为0．50％（n=6），大黄酚线性浓度范围在0．33-16．32μg·ml～，r=0．9994，平均回收率为99．13％，RSD为0．61％（n=6）。结论：方法简便可靠，重复性好，为控制利胆排石片的质量提供了科学依据。

Determination of Three Constituents in Lidan Paishi Tablets by HPLC with Gradient Elution

To establish a method for the determination of baicalin, emodin and chrysophanol in Lidan Paishi tablets by HPLC with gradient elution. Method： The column was Kromasil Cls （250 mm-4.6 mm, 5μm）. The mobile phase was acetonitrilephosphate buffer （ including 0. 24% H3 PO4 and 6. 30 mmol· L^-1K2 HPO4 ） with gradient elution. The detection wavelength was 256 nm and the flow rate was 1.0 ml.min^ -l. The temperature of the column was 35℃. Result： The linear range of baicalin was 0. 20-10. 01 I~g＂ ml ^- l （ r = 0. 999 2 ）, and the average recovery was 99.01% with RSD of 0.67% （ n = 6 ）. The linear range of emodin was 0. 37- 18. 41μg·ml^-l（ r = 0. 999 1 ）, and the average recovery was 99. 37% with RSD of 0. 50% （n = 6）. The linear range of chrysophanol was 0. 33-16. 32μg·m1^-1 （ r = 0. 999 4）, and the average recovery was 99. 13% with RSD of 0. 61% （ n = 6） o Conclusion： The method is simple, accurate, reliable, and can be applied in the quality control of Lidan Paishi tablets.