乌头类双酯型生物碱水解转化规律及含量计算方法研究  

Study on Hydrolysis of Aconitum Alkaloids and Quantitative Analysis Method of Their Hydrolysates

作　　者：郑琴[1] 陆浩伟[1] 郝伟伟[1] 刘嘉宇[1] 王粟莙[1] 杨明[1] 

机构地区：[1]江西中医学院现代中药制剂教育部重点实验室,南昌330004

出　　处：《中国药学杂志》2011年第9期652-656,共5页Chinese Pharmaceutical Journal

基　　金：国家自然科学基金资助项目(81060347);江西省教育厅科学技术研究项目(GJJ08333)

摘　　要：目的研究乌头类双酯型生物碱水解转化规律,建立LC-MS定性分析及HPLC定量分析乌头类双酯型生物碱及其水解产物方法。方法通过控制乌头碱、新乌头碱、次乌头碱3种双酯型生物碱的水解条件,分别获得不同阶段的水解产物,从而推导各水解产物的精确质量浓度。结果根据LC-MS定性分析结果,乌头类生物碱水解规律为乌头类双酯型生物碱先水解生成焦乌头碱类生物碱,再继续水解生成苯甲酰乌头原碱类生物碱;并根据水解规律分别计算出焦乌头碱类生物碱、苯甲酰乌头原碱类等乌头类生物碱水解产物的精确质量浓度。HPLC方法学表明,焦乌头碱、焦新乌头碱、焦次乌头碱、苯甲酰乌头原碱、苯甲酰新乌头原碱、苯甲酰次乌头原碱分别在0.70～44.64μg.mL-1(r=0.999 7);0.34～21.77μg.mL-1(r=0.999 9);0.38～24.37μg.mL-1(r=0.999 9);0.48～30.74μg.mL-1(r=0.999 9);0.41～26.38μg.mL-1(r=0.999 9);0.42～27.08μg.mL-1(r=0.999 7)内线性关系良好。结论本实验得出了乌头类双酯型生物碱水解转化规律,并建立了计算不同水解阶段水解产物的方法,其专属性高、定量简便,为乌头类生物碱及其水解产物的定量分析和乌头类中药材炮制、质量控制等提供了简便可行的方法。OBJECTIVE To investigate the hydrolysis rule of aconitum alkaloids,and to establish a quantitative HPLC analysis method and a qualitative LC-MS analysis method of aconitum alkaloids and their hydrolysates.METHODS By controlling the condition of hydrolysis reactions of aconitine,mesaconitine and hypaconitine,different hydrolysates were obtained.The accurate concentrations of the hydrolysates were deduced according to their relationship in hydrolysis reaction formula.RESULTS LC-MS analysis indicated that diester aconitum alkaloids were first hydrolyzed to pyraconitine alkaloids,then hydrolyzed to benzoylaconine alkaloids.The formulas for calculating the accurate concentrations of the different hydrolysates were deduced.The HPLC methodology investigation showed that the calibration curves were linear in the range of 0.70-44.64 μg·mL-1（r=0.999 7） for pyraconitine,0.34-21.77 μg·mL-1（r=0.999 9） for pyrmesaconitine,0.38-24.37 μg·mL-1（r=0.999 9） for pyrhypaconitine,0.48-30.74 μg·mL-1（r=0.999 9） for benzoylaconine,0.41-26.38 μg·mL-1（r=0.999 9） for benzoylmesaconine,and 0.42-27.08 μg·mL-1（r=0.999 7） for benzoylhypaconine,respectively.CONCLUSION This experiment provides an accurate,simple and convenient method for determination of aconitum alkaloids and their hydrolysates generated during the processing of Radix Aconiti and Radix Aconiti.

关 键 词：乌头类双酯型生物碱 焦乌头碱类生物碱 苯甲酰乌头原碱类生物碱 水解转化 

分 类 号：R284[医药卫生—中药学]