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利用乌头类双酯型生物碱水解规律测定醇胺型乌头碱的含量
Determination of Alcohol Amine diterpene Alkaloids by Hydrolysis Rule of Diester Aconitum Alkaloids
投稿时间:2017-02-10  
DOI:
中文关键词:  乌头类生物碱  双酯型生物碱  醇胺型生物碱  水解规律  含量测定
英文关键词:Aconitum alkaloid  Diester aconitum alkaloids  Alcohol amine diterpene alkaloids  Hydrolysis rule  Content determination
基金项目:江苏省中医药局科技项目(编号:YB2015121)
作者单位
张小龙1陈洪岩1孙晓2姚晨旭1姜燕1 1.连云港市食品药品检验检测中心 江苏连云港 2220062.连云港市第一人民医院 
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中文摘要:
      摘 要 目的:研究乌头类双酯型生物碱水解转化为醇胺型生物碱的转化率,水解乌头类双酯型生物碱对照品,利用水解转化率计算出水解原液中醇胺型生物碱的量,以此量作为醇胺型生物碱对照品的量,建立测定制川乌中乌头原碱、次乌头原碱、新乌头原碱含量的方法。方法: 通过控制乌头碱、次乌头碱、新乌头碱3种双酯型生物碱的水解条件,得到乌头原碱、次乌头原碱、新乌头原碱。采用高效液相色谱四级杆飞行时间串联质谱(HPLC-QTOF-MS)法,使用Agilent ZORBAX Extend C18 RRHT(2.1 mm×50 mm,1.8 μm)色谱柱,流速为0.21 ml·min-1,柱温为30 ℃,流动相为甲醇 水(含0.1%甲酸和2.5 mmol·L-1醋酸铵)系统梯度洗脱,采用电喷雾离子(ESI)源,正离子方式检测。结果: 在本文的水解条件下,乌头碱对于乌头原碱的转化率为99.64%;次乌头碱对于次乌头原碱的转化率为99.94%;新乌头碱对于新乌头原碱的转化率为99.57%。HPLC-QTOF-MS方法学表明,乌头原碱、次乌头原碱、新乌头原碱在一定范围内具有较好的线性关系,r值均大于0.999 1,精密度、重复性和稳定性的RSD都小于5%,加样回收率均在99.43%~100.10%之间。结论:本方法操作简便、专属性和重复性较好,在缺乏对照品的情况下,可以为乌头类中药材质量控制提供依据。
英文摘要:
      ABSTRACT Objective: To investigate the hydrolysis conversion rate of alcohol amine diterpene alkaloids from aconitum alkaloids, hydrolyze aconitum alkaloids reference substance, calculate the amount of alcohol amine diterpene alkaloids in the hydrolysis solution by the hydrolysis conversion rate, which is used as the amount of alcohol amine diterpene alkaloids reference substance, and establish a content determination method for aconine, hypaconitine and aconine in Aconiti radix cocta. Methods: Through controlling the hydrolysis conditions of aconitine, hypaconitine and mesaconitine, aconine, hypaconitine and aconine were obtained. The determination was performed on an Agilent ZORBAX Extend C18 RRHT(2.1 mm×50 mm,1.8 μm) column with the mobile phase consisting of methanol(A) water(B containing 0.1% formic acid and 2.5 mmol·L-1 ammonium acetate) with gradient elution by HPLC QTOF MS. The flow rate was 0.21 ml·min-1.The column temperature was 30 ℃. MS instrument was equipped with an ESI+ ion source. Results:Under the hydrolysis conditions of this study, the conversion rate of aconine from aconitine was 99.64%; the conversion rate of hypaconitine from hypaconine was 99.94%; the conversion rate of mesaconitine from mesaconine was 99.57%. The HPLC QTOF MS methodological investigation showed the 3 kinds of alcohol amine diterpene alkaloids were with good linearity (r>0.999 1). The RSD of the precision, repeatability and stability tests were less than 5%. The average recoveries were within the range of 99.43% 100.10%. Conclusion: The validated method is simple, specific, reliable and reproducible. In the absence of reference substance, it can be used for the quality control of the herbs of Aconitum L. species.
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