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柱切换液相色谱法快速定量检测参附注射液中乌头碱类生物碱和人参皂苷
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作者单位
张艳海,李玲,张大伟,鲁锐 1. 安捷伦科技(中国)有限公司上海 200080 2. 黑龙江农垦总局总医院黑龙江 哈尔滨 150088 
中文摘要:利用柱切换液相色谱,建立了参附注射液中苯甲酰新乌头原碱、苯甲酰乌头原碱、苯甲酰次乌头原碱、新乌头碱、次乌头碱和乌头碱6种乌头碱类生物碱,以及Rg1、Re、Rf、Rb1、Rc、Ro、Rb2、Rb3、Rd 9种人参皂苷的分析方法。首先利用强阳离子交换的在线固相小柱选择性富集和净化样品中生物碱类成分,优化了色谱条件;并采用EC-C18柱作为人参皂苷的分析柱,通过优化实验条件,结合柱切换方式,去除了样品中辅料等大极性基质成分对色谱柱的污染,实现了生物碱分析和人参皂苷分析的自动切换。结果显示,样品中的生物碱和人参皂苷分离良好,线性相关系数(r2)均大于0.999,连续进样精密度的相对标准偏差(RSD) < 2.0%,重复性的RSD < 2.0%;其中6种生物碱的平均回收率为95.1%~98.6%,检出限为4.0~8.2 ng/mL;9种人参皂苷的平均回收率为91.7%~104%。所构建的基于柱切换液相色谱技术的在线固相萃取方法能够有效去除样品中的基质干扰,快速完成参附注射液中3种单酯型生物碱和9种人参皂苷的快速定量,同时也可对3种双酯型生物碱进行限量检测,可应用于药物的质量评价。
中文关键词:柱切换液相色谱法  在线固相萃取  苯甲酰新乌头原碱  乌头碱  人参皂苷Ro  参附注射液
 
Rapid Quantitative Analysis of Aconitine-type Alkaloids and Ginsenosides in Shenfu Injection by Column Switching Liquid Chromatography
Abstract:A column switching liquid chromatography was developed for the analysis of aconitine-type alkaloids including aconitine(AC),mesaconitine(MA),hypaconitine(HA),benzoylaconine(BAC),benzoylmesaconine(BMA),benzoylhypaconine(BHA) and nine ginsenosides in Shenfu injection(SFI).Aconite-type alkaloids were enriched on an online SPE column by the interaction of strong cation exchange,and purified by the optimized eluting program.Eluting conditions were confirmed through investigating the transferring solvent and eluting time.A Zorbax SB-C18 was chosen as the analytical column,with acetonitrile and ammonium acetate as mobile phases.Meanwhile,an EC-C18 belonged to core-shell particles was used to analyze ginsenoside in SFI.Through the investigation of column oven and gradient program,the optimized conditions were confirmed.The matrix interference was removed to improve the relative response in chromatogram by column switching.The analytical processes for alkaloids and ginsenosides were switched automatically via valve switching.The satisfactory resolutions could be achieved for the aconitine-type alkaloids and ginsenosides in SFI sample.The methodology investigation showed good linearity(r2 > 0.999),precision(RSD < 2.0%) and better reproducibility(RSD < 2.0%).The limits of detection(LODs) for six target alkaloids were from 4.0 to 8.2 ng/mL.The average recoveries for six target alkaloids ranged from 95.1% to 98.6%.For nine ginsenosides,the recoveries were from 91.7% to 104%.It was an effective way to remove a large amount of matrix interference by the constructed online SPE method based on column switching LC,which could complete the rapid quantitation of three monoester alkaloids and nine active ginsenosides in SFI.The proposed method also realized the limit inspection of three diester alkaloids,and it could be used in practical quality evaluation on SFI.
Key Words:column switching liquid chromatography  online SPE  benzoylmesaconine  aconitine gensinoside Ro  Shenfu injection
引用本文:张艳海,李玲,张大伟,鲁锐.柱切换液相色谱法快速定量检测参附注射液中乌头碱类生物碱和人参皂苷[J].分析测试学报,2022,41(7):1022-1029.
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