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目的:建立高效液相色谱法同时测定利胆排石片中大黄素、大黄酚及大黄素甲醚含量的方法。方法:采用高效液相色谱法,Agilent SB-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-甲醇-0.1%磷酸(42∶23∶35)为流动相,流速1.0 mL.min-1,检测波长254 nm。结果:大黄素、大黄酚和大黄素甲醚分别在3.4×10-3～1.14μg,5.3×10-3～1.06μg,1.9×10-3～0.49μg线性关系良好,r分别为0.999 9,0.999 9,0.999 6;平均加样回收率分别为101.1%,100.5%,99.3%,RSD(n=6)分别为1.1%,0.9%,1.1%。结论:方法简便快捷,结果准确、可靠,重复性好,可作为利胆排石片质量控制方法之一。
Objective: To establish a method for the simultaneous determination of emodin, chrysophanol and physcion in Laxan Paoban tablet by high performance liquid chromatography. METHODS: The mobile phase was acetonitrile-methanol-0.1% phosphoric acid (42:23:35) at a flow rate of 1.0 mL.min-1 on a Agilent SB-C18 column (4.6 mm × 250 mm, 5 μm) 1, detection wavelength 254 nm. RESULTS: Emodin, chrysophanol and emodin had good linearity in the ranges of 3.4 × 10-3 ~ 1.14μg, 5.3 × 10-3 ~ 1.06μg and 1.9 × 10-3 ~ 0.49μg with r of 0.999 9, 0.999 9,0.999 6 respectively. The average recoveries were 101.1%, 100.5% and 99.3%, respectively, and RSD (n = 6) were 1.1%, 0.9% and 1.1% respectively. Conclusion: The method is simple, rapid, accurate, reliable and reproducible. It can be used as one of the quality control methods for Ligustilide.