高效液相色谱法同时测定黄氏响声丸中5种蒽醌类成分含量

Simultaneous determination of five anthraquinone constituents in Huangshixiangsheng Pills by high performance liquid chromatography

目的:建立黄氏响声丸中5种蒽醌类活性成分的高效液相色谱含量测定方法,有利于制剂的质量控制。方法:采用高效液相色谱法,色谱柱:Shimadzu VP-ODS柱(4.6mm×250mm,5μm),流动相为乙腈-0.1%磷酸梯度洗脱,流速为1.0ml/min,检测波长为254nm,柱温30℃。结果:5种成分为芦荟大黄素0.042～0.840μg(r=0.9996)、大黄酸0.168～3.352μg(r=0.9998)、大黄素0.084～1.680μg(r=0.9997)、大黄酚0.093～1.852μg(r=0.9999)和大黄素甲醚0.174～3.488μg(r=0.9994)内成良好线性关系,平均回收率分别为99.8%(RSD=1.34%,n=5)、99.8%(RSD=1.72%,n=5)、100.0%(RSD=0.89%,n=5)、99.5%(RSD=0.97%,n=5)和100.2%(RSD=1.04%,n=5)。结论:该方法简便、快捷、准确、可靠,重复性好,可用于同时测定黄氏响声丸中5种蒽醌类成分的含量。

Objective：To establish an HPLC method for determining five anthraquinones contents in Huangshixiangsheng Pills,and make it used for the quality control of Huangshixiangsheng Pills.Methods：HPLC was carried out on Shimadzu VP-ODS（4.6mm×250mm,5.0μm） with acetonitrile-0.1% phosphoric acid in gradient elution.The flow rate was 1.0 mL·min-1,the detection wavelength was 254 nm and the column temperature was 30℃.Results：Five anthraquinones had good linear relationship：Aloe-emodin in the range of 0.042～0.840 μg（r=0.9996）,rhein in the range of 0.168～3.352 μg（r=0.9998）,emodin in the range of 0.084～1.680 μg（r=0.9997）,chrysophanol and physcion in the range of 0.093-1.852 μg（r=0.9999） and 0.174～3.488 μg（r=0.9994）.Their average recoveries were 99.8%（RSD=1.34%,n=5）,99.8%（RSD=1.72%,n=5）,100.0%（RSD=0.89%,n=5）,99.5%（RSD=0.97%,n=5）,and 100.2%（RSD=1.04%,n=5）,respectively.Conclusion：This method is rapid,simple and accurate and it can be used for the determination of aloe-emodin,rhein,emodin,chrysophanol and physcion in Huangshixiangsheng Pills simultaneously.