發(fā)布時間：2019-01-30 07:51

【摘要】：目的:建立黃楊寧片原料中環(huán)維黃楊星D準(zhǔn)確定量和全面反映雜質(zhì)色譜信息的分析方法。方法:選擇可使主成分和所有雜質(zhì)衍生化反應(yīng)的試劑進(jìn)行柱前衍生化反應(yīng),采用RP-HPLC法對衍生產(chǎn)物進(jìn)行分析,C8柱分離,乙腈-0.01%甲酸水溶液(71∶29)洗脫,流速1 m L·min 1,檢測波長230 nm,柱溫25℃。結(jié)果:新建立的方法能使環(huán)維黃楊星D與有關(guān)生物堿的最低分離度達(dá)1.5,檢測到的12個雜質(zhì)峰,其中9個可被定量。環(huán)維黃楊星D檢測限為0.35 ng(RSD=2.2%,n=5),定量限為1.37ng(RSD=4.6%,n=5);平均回收率為102.4%,RSD為1.4%(n=6)。來自4個廠家的10批樣品中環(huán)維黃楊星D含量范圍為78.28%~85.48%;9個雜質(zhì)總含量范圍為10.14%~15.57%。結(jié)論:該法既可使主成分與雜質(zhì)完全分離,又可全面反映雜質(zhì)色譜信息,能同時用于準(zhǔn)確測定原料中主成分含量和雜質(zhì)檢查。
[Abstract]:Objective: to establish an accurate quantitative and comprehensive method for the determination of impurity chromatographic information in Huangyangning tablets. Methods: precolumn derivatization reaction was carried out with the reagent which could make the principal component and all impurity derivatization reaction. The derivative was analyzed by RP-HPLC, separated on C 8 column, and eluted by acetonitrile-0.01% formic acid solution (71:29). The flow rate was 1 m L min / 1, the detection wavelength was 230 nm, and the column temperature was 25 鈩，

本文編號：2417916