HPLC梯度洗脱法测定利胆排石片中3组分的含量

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

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:KromasilC_(18)(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0.20～10.01μg·ml^(-1),r=0.999 2,平均回收率为99.01%,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^(-1),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。

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.