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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。
Objective: To establish a method for the determination of baicalin, emodin and chrysophanol in Lixia Pai tablet. METHODS: The mobile phase was eluted with acetonitrile-phosphate buffer (0.24% phosphoric acid, 6.30 mmol·L ~ (-) phosphate) 1)) gradient; detection wavelength of 256nm; flow rate: 1.0ml · min -1; column temperature: 35 ℃. Results: The linear range of baicalin was 0.20-10.01μg · ml -1, r = 0.999 2, the average recovery was 99.01%, RSD was 0.67% (n = 6), the linear range of emodin was 0.37 ~ The average recovery was 99.37%, the RSD was 0.50% (n = 6), the linear range of chrysophanol was 0.33 ~ 16.32μg · ml ~ (-1), r = 0.9994 with an average recovery of 99.13% and a RSD of 0.61% (n = 6). Conclusion: The method is simple and reliable with good repeatability and provides a scientific basis for the quality control of gallbladder.