摘要
目的:建立采用高效液相色谱-二极管阵列检测器(HPLC-DAD)波长切换法同时定量分析三黄片中黄芩苷、盐酸小檗碱、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚7种化学成分含量的方法。方法:色谱柱为Diamonsil C18(4.6 mm×250 mm,5μm),流动相为乙腈-0.1%磷酸水溶液,梯度洗脱,流速1.0 ml/min;柱温30℃。采用DAD检测器,检测波长:0~5 min、280 nm(黄芩苷),5~10 min、265 nm(盐酸小檗碱),10~60 min、254 nm(芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚)。结果:黄芩苷、盐酸小檗碱、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚线性范围分别为0.0518~0.5180μg(r=0.9992)、0.0246~0.2459μg(r=0.9998)、0.0020~0.0202μg(r=0.9996)、0.0020~0.0200μg(r=0.9990)、0.0020~0.0201μg(r=0.9999)、0.0020~0.0201μg(r=0.9995)和0.0010~0.0102μg(r=0.9998);平均加样回收率为95.41%~100.59%(n=6),RSD均小于3.11%。结论:本文建立的HPLC-DAD法符合方法学验证要求,可用于三黄片7种化学成分的同时测定。
Objective To establish a method that could determine 7 chemical components including baicalin,berberine hydrochloride,aloe-emodin,rhein,emodin,chrysophanol and physcion in San huang tablet by high performance liquid chromatography-diode array detector(HPLC-DAD)method simultaneously with quantitative analysis method.Methods The Diamonsil C18 column(4.6 mm×250 mm,5μm)was adopted.The mobile phase was acetonitrile(A)-0.1%phosphoric acid solution(B)with gradient elution at a flow rate of 1.0 ml/min.The column temperature was set at 30℃.The detector was DAD.The detection wavelengths were 280 nm(baicalin),265 nm(berberine hydrochloride),254 nm(aloe-emodin,rhein,emodin,chrysophanol and physcion).Results The linear ranges of baicalin,berberine hydrochloride,aloe-emodin,rhein,emodin,chrysophanol and physcion were within the ranges of 0.0518-0.5180μg(r=0.9992),0.0246-0.2459μg(r=0.9998),0.0020-0.0202μg(r=0.9996),0.0020-0.0200μg(r=0.9990),0.0020-0.0201μg(r=0.9999),0.0020-0.0201μg(r=0.9995),and 0.0010-0.0102μg(r=0.9998),respectively.The average recoveries(n=6)were 95.41%-100.59%,with RSDs less than 3.11%.Conclusions This HPLC-DAD method is consistent with methodology and could simultaneously determine 7 chemical components in San huang tablet.
作者
张莹
阎岩
刘团会
和燕
李浪
Zhang Ying;Yan Yan;Liu Tuanhui;He Yan;Li Lang(Sun Simiao Medical School,Tongchuan Vocational and Technical College,Tongchuan 727031,China;School of Life Science,Yan’an University,Yan’an 716000,China;Shaanxi Origin Agricultural Technology Co.,Ltd.,Tongchuan 727031,China)
出处
《国际中医中药杂志》
2020年第10期996-1000,共5页
International Journal of Traditional Chinese Medicine
基金
陕西省重点研发计划项目(2018TSCXL-SF-01-03)
陕西省教育厅专项科学研究计划(19JK0271)。
关键词
三黄片
含量测定(中药)
高效液相色谱
波长切换法
San huang tablet
Assay(TCD)
High performance liquid chromatography
Wavelength switching
