摘要
目的 建立同时测定黄蛤培元膏中莫诺苷、马钱苷、升麻素苷、毛蕊异黄酮葡萄糖苷、5-O-甲基维斯阿米醇苷、淫羊藿苷、五味子醇甲7种抗炎活性成分含量的一测多评法.方法 黄蛤培元膏经50％甲醇提取.色谱柱为Agilent Eclipse XDB-C18柱(250 mm × 4.6 mm,5 μm),流动相为乙腈-0.2％磷酸水溶液(梯度洗脱),流速为1.0mL/min,检测波长为260 nm,柱温为30 ℃,进样量为5 µL.以淫羊藿苷为内标,计算其他6种成分的相对校正因子,分别以一测多评法和外标法测定含量,通过2种方法的相对误差验证结果的可靠性.结果 莫诺苷、马钱苷、升麻素苷、毛蕊异黄酮葡萄糖苷、5-O-甲基维斯阿米醇苷、淫羊藿苷、五味子醇甲的质量浓度分别在 14.21～454.71 μg/mL、6.65～212.89 μg/mL、1.36～43.54 μg/mL、1.18～37.64 µg/mL、1.64～52.42 µg/mL、3.38～108.11 μg/mL、0.57～18.17 μg/mL范围内与峰面积积分值线性关系良好(r＞0.999 5,n=6);精密度、稳定性、重复性试验结果的RSD均小于3.0％(n=6);平均加样回收率为95.68％～99.50％,RSD为0.55％～2.41％(n=6).以淫羊藿苷为内标,莫诺苷、马钱苷、升麻素苷、毛蕊异黄酮葡萄糖苷、5-O-甲基维斯阿米醇苷、五味子醇甲的相对校正因子分别为2.995 5,3.947 6,2.225 1,0.5843,2.154 9,1.255 7.一测多评法与外标法含量测定结果的相对偏差均在-1.3％～1.9％范围内.结论 该方法简单可靠、结果准确,可用于黄蛤培元膏中7种抗炎活性成分的含量测定.
Abstract
Objective To establish a quantitative analysis of multi-components by single-marker(QAMS)method for the simultaneous determination of seven anti-inflammatory active components(morroniside,loganin,prim-O-glucosylcimifugin,galycosin 7-O-β-D-glucopyranoside,5-O-methylvisammioside,icariin,schisandrin)in Huangge Peiyuan Ointment.Methods Huangge Peiyuan Ointment was extracted with 50％methanol.The chromatographic column was Agilent Eclipse XDB-C18 column(250 mm × 4.6 mm,5 µm),the mobile phase was acetonitrile-0.2％phosphoric acid aqueous solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 260 nm,the column temperature was 30 ℃,and the injection volume was 5 μL.With icariin as the internal standard,the relative correction factors of the other six components were calculated,and their contents were determined by the QAMS method and the external standard method.The reliability of the results was verified through the relative errors of the two methods.Results The linear ranges of morroniside,loganin,prim-O-glucosylcimifugin,galycosin 7-O-β-D-glucopyranoside,5-O-methylvisammioside,icariin,and schisandrin were 14.21-454.71 μg/mL,6.65-212.89 μg/mL,1.36-43.54 μg/mL,1.18-37.64 μg/mL,1.64-52.42 µg/mL,3.38-108.11 μg/mL,and 0.57-18.17 μg/mL(r＞0.999 5,n=6),respectively.The RSDs of precision,stability,and repeatability test results were all lower than 3.0％(n=6).The average recoveries of the above seven components were in the ranges of 95.68％-99.50％,with RSDs of 0.55％-2.41％(n=6).With icariin as the internal standard,the relative correction factors of morroniside,loganin,prim-O-glucosylcimifugin,galycosin 7-O-β-D-glucopyranoside,5-O-methylvisammioside,icariin,and schisandrin were 2.995 5,3.947 6,2.225 1,0.584 3,2.154 9,and 1.255 7,respectively.The relative deviation between the content determination result of the QAMS method and that of the external standard method was ranged from-1.3％to 1.9％.Conclusion The method is simple,reliable,and accurate,which can be used for the content determination of seven anti-inflammatory active components in Huangge Peiyuan Ointment.
维普
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