摘要
目的:建立铁棒锤中5个有效成分(新乌头碱、欧乌头碱、苯甲酰乌头原碱、次乌头碱、乌头碱)的定性方法与其主要毒效成分的定量分析方法。方法:采用超高效液相色谱-四极杆-飞行时间质谱法(UPLC-Q-TOFMS/MS)对铁棒锤的化学成分进行表征。根据其主要成分的表征结果,通过优化薄层色谱法(TLC)条件建立铁棒锤定性分析方法。进一步针对其毒效成分苯甲酰乌头原碱和乌头碱,建立高效液相色谱法(HPLC)同时定量的方法学。结果:UPLC-Q-TOF-MS/MS结果鉴别并确定出5个主要生物碱成分:新乌头碱、欧乌头碱、苯甲酰乌头原碱、次乌头碱和乌头碱。TLC分析结果显示,基于上述主要生物碱成分所建立的鉴别方法可对铁棒锤与其混淆品仙茅进行区分。同时定量分析结果显示,苯甲酰乌头原碱和乌头碱分别在质量浓度为194.00~833.00μg·mL^(-1)时线性关系良好(r≥0.9996),检测限分别为1.10、1.00μg·mL^(-1),定量限分别为7.39、6.90μg·mL^(-1),平均加样回收率分别为97.51%、102.21%,RSD均小于3.0%。结论:建立的定性与定量方法可用于区分铁棒锤与混淆品仙茅,并为其质量控制及临床用药安全提供参考。
Objective:To establish a qualitative method for the five active components(neoaconitine,napelline,benzoyl aconitine,hypaconitine,and aconitine)in Aconitum pendulum Busch.and to quantitatively analyze their primary toxicity components.Methods:Ultra-high-performance liquid chromatography-quadrupole-time-of-flight tandem mass spectrometry(UPLC-Q-TOF-MS/MS)was used to characterize the chemical composition of A.pendulum.Based on the characterization results of its main components,a qualitative analysis method was established by optimizing the conditions of thin-layer chromatography(TLC).Furthermore,the methodology of simultaneous quantification by high-performance liquid chromatography(HPLC)was established for the toxicity components benzoyl aconitine,and aconitine.Results:The UPLC-Q-TOF-MS/MS analysis identified five main alkaloid components:neoaconitine,napelline,benzoyl aconitine,hypaconitine and aconitine.The results of TLC analysis showed that the identification method established based on these main alkaloid components could effectively distinguish A.pendulum from its adulterant Curculigo orchioides.The quantitative analysis results showed that benzoyl aconitine and aconitine had a good linear relationship within the concentration range of 194.00-833.00μg·mL^(-1)(r≥0.9996),respectively.The detection limits were 1.10 and 1.00μg·mL^(-1),respectively,and the limits of quantification were 7.39μg·mL^(-1)and 6.90μg·mL^(-1),respectively.The average spiked recovery rates were 97.51%and 102.21%,respectively,with relative standard deviations(RSD)both below 3.0%.Conclusion:The qualitative and quantitative methods established in this study can be used to distinguish between A.pendulum and C.orchioides,and provide references for their quality control and supporting clinical drug safety.
作者
周蜜
何姬
刘妍如
唐志书
宋忠兴
王兴弛
张丽
张德柱
ZHOU Mi;HE Ji;LIU Yanru*;TANG Zhishu;SONG Zhongxing;WANG Xingchi;ZHANG Li;ZHANG Dezhu(Shaanxi University of Chinese Medicine,Shaanxi Collaborative Innovation Center of Chinese Medicinal Resources Industrialization,Xianyang 712083,China;Beijing University of Chinese Medicine,Beijing 100700,China;The Affiliated Hospital of Shaanxi University of Traditional Chinese Medicine,Xianyang 712000,China;Shaanxi Panlong Pharmaceutical Group,Shangluo 711400,China)
出处
《中国现代中药》
2026年第1期55-66,I0009,共13页
Modern Chinese Medicine
基金
陕西省中医药科技创新提质扩能计划(TZKN-CXRC-23)
秦创原中医药产业创新聚集区项目&陕西中医药大学联合基金项目(L2024-QCY-ZYYJJQ-X203)
全国中药特色技术传承人才培训项目(国中医药人教函[2023]96号)。
