UPLC-PDA同时测定三黄方药液10种成分含量

Simultaneous determination of ten ingredients in Sanhuangfang ethanol extract by UPLC-PDA

目的:建立UPLC-PDA法同时测定三黄方药液中黄柏碱、黄芩苷、小檗碱、黄芩素、芦荟大黄素、汉黄芩素、大黄酸、大黄素、大黄酚、大黄素甲醚10种成分的含量。方法:采用Waters ACQUITY BEH C18(2.1 mm×100 mm,1.7μm)色谱柱,以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速0.3 m L·min^(-1),柱温30℃,检测波长284 nm。结果:在一定浓度范围内,三黄方药液中10种成分均呈良好的线性关系(r>0.999);平均加样回收率为96.73%~101.7%(RSD<3%,n=6)。3批样品中黄柏碱、黄芩苷、小檗碱、黄芩素、芦荟大黄素、汉黄芩素、大黄酸、大黄素、大黄酚、大黄素甲醚含量分别在0.226~0.233、5.85~6.00、1.92~2.00、0.140~0.151、0.031 4~0.037 5、0.043 6~0.044 7、0.081 5~0.083 1、0.032 8~0.040 6、0.102~0.105、0.340~0.350 mg·mL^(-1)。结论:经方法学验证,本法可用于三黄方药液的质量控制。

Objective： To establish a UPLC-PDA method for simultaneous determination of ten ingredients, including phellodendrine, baicalin, berberine, baicalein, aioe-emodin, wogonin, rhein, emodin, chrysophanol and physcion, in Sanhuangfang ethanol extract. Methods： The chromatographic analysis was carried out on an ACQUITY BEH Clscolumn（ 2.1 mm × 100 mm, 1.7 μ m ）. The mobile phase consisted of aeetonitrile-0.1% phosphoric acid solution with gradient elution at a flow rate of 0. 3 mL . min^-1. The column temperature was 30 ℃, and the detection wavelengths were set at 284 nm. Results： Within a certain concentration range, the ten ingredients all showed good linear relationship C r〉0. 999 ） and the average recoveries were with the range of 96. 73%-101.7% （ RSD〈3%, n=6 ）. The contents of phellodendrine, baicalin, berberine, baicalein, aloe-emodin, wogonin, rhein, emodin, chrysophanol and physcion in 3 samples were 0.226-0.233,5.85-6.00, 1.92-2.00, 0.140-0.151, 0.031 4-0.037 5,0.043 6-0.044 7,0.081 5-0.083 1,0.032 8-0.040 6, 0.102-0.105, and 0.340-0.350 mg.mL^-1, respectively. Conclusion： The established method can be used for the quality control of Sanhuangfang ethanol extract.