摘要
目的 建立同时测定冰川滴丸中 6 个成分含量的一测多评法.方法 色谱柱为Waters Symmetry C18 柱(250 mm×4.6 mm,5µm),流动相为乙腈-0.5%冰醋酸溶液(梯度洗脱),流速为 1.0 mL/min,检测波长为 285 nm(肉桂酸)、330 nm(阿魏酸和藁本内酯)、430 nm(姜黄素、去甲姜黄素、双去甲姜黄素),进样量为 10µL.以肉桂酸为内参物,计算阿魏酸、藁本内酯、姜黄素、去甲姜黄素、双去甲姜黄素的相对校正因子,并与外标法含量测定结果进行比较.结果 阿魏酸、藁本内酯、肉桂酸、姜黄素、去甲姜黄素、双去甲姜黄素的进样量分别在 0.025 86～0.142 8 mg、0.275 2～2.752 mg、0.045 4～0.454 mg、0.178 8～1.788 mg、0.063 6～0.636 mg、0.057 2～0.572 mg范围内与峰面积积分值线性关系良好(R2=0.999 9,n=6);精密度、稳定性、重复性试验结果的RSD均小于 3.0%(n=6);平均加样回收率分别为 96.85%,99.54%,99.75%,99.34%,98.65%,100.44%,RSD分别为 1.38%,2.32%,2.82%,2.56%,2.91%,1.46%(n=6).相对校正因子分别为 0.177 5,0.225 6,0.711 2,0.903 5,1.033 6.各成分一测多评法的含量测定结果与外标法接近.结论 该方法操作简便、结果准确、重复性好,可用于同时测定冰川滴丸制剂中 6 个成分的含量.
Abstract
Objective To establish a quantitative analysis of multi-components with a single-marker(QAMS)method for the simultaneous determination of six components in Bingchuan Dropping Pills.Methods The chromatographic column was the Waters Symmetry C18 column(250 mm×4.6 mm,5 µm),the mobile phase was acetonitrile-0.5%glacial acetic acid solution(gradient elution),the flow rate was 1.0 mL/min,the detection wavelengths were 285 nm(cinnamic acid),330 nm(ferulic acid,ligustrolactone)and 430 nm(curcumin,demethoxy curcumin,bis-demethoxy curcumin),and the injection volume was 10 µL.With cinnamic acid as the internal reference,the relative correction factors(RCFs)of ferulic acid,ligustrolactone,curcumin,demethoxy curcumin and bis-demethoxy curcumin were calculated,and the content determination was compared with that by the external standard method.Results The linear ranges of ferulic acid,ligustrolactone,cinnamic acid,curcumin,demethoxy curcumin,and bis-demethoxy curcumin were 0.025 86-0.142 8 µg,0.275 2-2.752 µg,0.045 4-0.454 µg,0.178 8-1.788 µg,0.063 6-0.636 µg,0.057 2-0.572 µg(R2=0.999 9,n=6)respectively.The RSDs of precision,stability and repeatability tests were all lower than 3.0%(n=6).The average recovery rates of the above six components were 96.85%,99.54%,99.75%,99.34%,98.65%,100.44%with RSDs of 1.38%,2.32%,2.82%,2.56%,2.91%,1.46%(n=6)respectively.The relative correction factors of the above five components were 0.177 5,0.225 6,0.711 2,0.903 5,1.033 6 respectively.The result of content determination by the QAMS method for each component was similar to that of by the external standard method.Conclusion This method is easy,accurate and repeatable,which can be used for the simultaneous determination of six components in Bingchuan Dripping Pills.
维普
万方数据