HPLC测定不同来源决明子饮片中9个成分的含量

目的: 建立高效液相色谱法测定决明子饮片中红镰霉素龙胆二糖苷、决明子苷、橙黄决明素葡萄糖苷3个苷类成分和橙黄决明素、黄决明素、决明素、大黄素、大黄酚、大黄素甲醚6个苷元的含量。 方法: 采用Agilent ZORBAX SB-C₁₈色谱柱(4.6 mm×250 mm,5 μm)色谱柱,流速为1.0 mL·min^-1,柱温为室温。流动相Ⅰ为乙腈-四氢呋喃-1%冰醋酸水溶液(18:3:79),检测波长为278 nm;流动相Ⅱ为乙腈-0.1%磷酸水溶液,梯度洗脱,检测波长为284 nm,分别测定苷和苷元类成分的含量。 结果: 红镰霉素龙胆二糖苷、决明子苷、橙黄决明素葡萄糖苷、橙黄决明素、黄决明素、决明素、大黄素、大黄酚、大黄素甲醚的进样量分别在0.051~2.0、0.054~2.1、0.020~0.78、0.050~0.50、0.018~0.18、0.015~0.15、0.013~0.13、0.085~0.85、0.026~0.26 μg范围内与色谱峰面积呈良好的线性关系;加样回收率(n=6)在97.6%~101.6%,RSD在1.4%~ 2.4%。不同来源的决明子饮片中9个成分的含量差异显著。 结论: 本方法为决明子饮片的全面质量控制提供了参考。

Objective: To establish an HPLC method for determination of three glycosides(rubrofusarin-gentiobioside,aurantio-obtusin-6-O-β-D-glucopyranoside)and six aglycones (aurantio-obtusin,chryso-obtusin,obtusin,emodin,chrysophanol,physcion) in the processed products of Cassiae Semen. Methods: The samples were separated on an Agilent ZORBAX SB-C₁₈ (4.6 mm×250 mm,5 μm)column at a flow rate of 1.0 mL·min^-1 and the column temperature was at room temperature.The mobile phaseⅠ was acetonitrile-tetrahydrofuran-1% glacial acetic acid aqueous(18: 3: 79) for determination of glycosides with the detection wavelength of 278 nm.The mobile phase Ⅱ was acetonitrile-0.1% phosphoric acid aqueous for determination of aglycones with gradient elution,and the detection wavelength was 284 nm. Results: Rubrofusarin-gentiobioside,cassiaside,aurantio-obtusin-6-O-β-D-glucopyranoside,aurantio-obtusin,chryso-obtusin,obtusin,emodin,chrysophanol,physcion had good linearity in the ranges of 0.051-2.0,0.054-2.1,0.020-0.78,0.050-0.50,0.018-0.18,0.015-0.15,0.013-0.13,0.085-0.85,0.026-0.26 μg,respectively.The average recoveries of the nine constituents were 97.6%-101.6% and RSDs were 1.4%-2.4%.The contents of nine constituents in Cassiae Semen from different sources had significant differences. Conclusion: The method provides reference for comprehensive quality control of Cassiae Semen.