摘要
目的:采用QAMS测定一清颗粒中4种蒽醌类成分的含量。方法:采用RP-HPLC,Accurasil C18色谱柱(4.6 mm×250 mm,5μm),流动相甲醇-0.4%磷酸水溶液(85∶15),流速1 mL·min-1,检测波长254 nm,柱温30℃。以大黄素为内参物,采用QAMS测定11批一清颗粒中大黄蒽醌类成分含量,并与外标法实测值进行比较。结果:大黄酸、大黄素、大黄酚和大黄素甲醚的加样回收率分别为103.6%,98.8%,99.5%,99.4%,RSD分别为0.29%,1.8%,2.7%,3.8%。f254 nm大黄酸/大黄素=1.14,f254 nm大黄酚/大黄素=1.47 f254 nm大黄素甲醚/大黄素=1.04,r大黄酸/大黄素=0.64,r大黄酚/大黄素=1.38,r大黄素甲醚/大黄素=1.88,两种含量测定方法的结果无明显差异。结论:该方法简便、可靠,可用于控制一清颗粒中大黄蒽醌类成分含量。
Objective：To develop a HPLC for determining the contents of four anthraquinones in Yiqing granules by a single marker（QAMS）.Method：RP-HPLC was performed on an Accurasil C 18 column（4.6 mm × 250 mm,5 μm）,eluted with a mobile phase of methanol-0.4% phosphoric acid solution（85∶ 15）.The flow rate was 1.0 mL·min-1.The column temperature was set at 30 ℃ and the detection wavelength was 254 nm.Using emodin as an internal reference substance,the contents of four anthraquinones in 11 batches of Yiqing granules was authentically determined by QAMS,and compared with the measured values by external standard method.Result：Recoveries of rhein,emodin,chrysophanol and physcion were 103.6%,98.8%,99.5%,99.4% with RSD were 0.29%,1.8%,2.7%,3.8%,respectively.f rhein/emodin = 1.14,f chrysophanol/emodin = 1.47,f physcion/emodin = 1.04,r rhein/emodin = 0.64,r chrysophanol/emodin = 1.38,r physcion/emodin = 1.88,there were no significant differences between results determined by the two standard method.Conclusion：This method was simple and reliable,it could be used for determination of the four anthraquinones inYiqing granules.
出处
《中国实验方剂学杂志》
CAS
北大核心
2013年第17期53-56,共4页
Chinese Journal of Experimental Traditional Medical Formulae
基金
国家"重大新药创制"科技重大专项(2009ZX09301-005
2009ZX09308-003)
2007年国家中医药管理局中医药行业科技专项(200707009)
关键词
高效液相色谱
一测多评法
一清颗粒
蒽醌
相对校正因子
相对保留值
HPLC
a quantitative method for simultaneous assay（QAMS）
Yiqing granules
anthraquinone
relative correction factor
relative retention value
