HPLC法同时测定荨麻疹丸中9个有效成分

Simultaneous determination of nine constituents in urticaria pills by HPLC

目的:建立HPLC法同时测定荨麻疹丸(赤芍、防风、当归、黄芩、白芷、何首乌)中芍药苷、升麻素苷、阿魏酸、5-O-甲基维斯阿米醇苷、黄芩苷、欧前胡素、异欧前胡素、大黄素、大黄素甲醚的含量。方法:采用高效液相色谱法。色谱柱为JADE-PAK ODS-AQ C18,流动相为甲醇-0.2%磷酸水溶液,梯度洗脱,流速1.0 mL·min^(-1),检测波长230 nm(芍药苷)、254 nm(升麻素苷、5-O-甲基维斯阿米醇苷、大黄素、大黄素甲醚)、280 nm(黄芩苷)、300 nm(欧前胡素、异欧前胡素)、321 nm(阿魏酸),柱温25℃,进样量10μL。结果:9个成分在各自范围内线性关系良好(r≥0.999),平均加样回收率为95.2%~101.0%,RSD为1.2%~2.0%。3批样品中芍药苷、升麻素苷、阿魏酸、5-O-甲基维斯阿米醇苷、黄芩苷、欧前胡素、异欧前胡素、大黄素、大黄素甲醚含量范围分别为2.014~2.161、0.205~0.220、0.032~0.038、0.241~0.251、0.048~0.050、0.785~0.811、0.042~0.049、0.095~0.102、0.037~0.041 mg·g^(-1)。结论:该方法准确,重复性好,可用于荨麻疹丸的质量控制。

Objective:To establish a method for the simultaneous determination of paeoniflorin,prim-Oglucosylcimifugin,ferulic acid,5-O-methylvisammioside,baicalin,imperatorin,isoimperatorin,emodin and physcion in urticaria pills.Methods:HPLC was performed on the column of JADE-PAK ODS-AQ C18 with the mobile phase of methanol-phosphoric acid at a flow rate of 1.0 mL·min-1.The detection wavelength was 230 nm for paeoniflorin,254 nm for cimifugin,5-O-methylvisammioside,emodin and parietin,280 nm for baicalin and 300 nm for imperatorin and isoimperatorin,321 nm for ferulic acid,respectively.Column temperature was 25℃,and the volume injection was 10μL.Results:Nine constituents showed good linear relationships within their own ranges(r≥0.999),and the average recoveries were 95.2%-101.0%with the RSDs of 1.2%-2.0%.The content ranges of paeoniflorin,prim-O-glucosylcimifugin,ferulic acid,5-O-methylvisammioside,baicalin,imperatorin,isoimperatorin,emodin,physcion in 3 samples were 2.014-2.161,0.205-0.220,0.032-0.038,0.241-0.251,0.048-0.050,0.785-0.811,0.042-0.049,0.095-0.102,0.037-0.041 mg·g-1,respectively.Conclusion:This simple,accurate and reproducible method can be used for the quality control of urticaria pills.