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基于TLC及UPLC-Q-TOF-MS/MS的铁棒锤毒效成分定性及HPLC定量研究

周蜜 何姬 刘妍如 唐志书 宋忠兴 王兴弛 张丽 张德柱

中国现代中药2026,Vol.28Issue(1):55-66,12.
中国现代中药2026,Vol.28Issue(1):55-66,12.DOI:10.13313/j.issn.1673-4890.20250809001

基于TLC及UPLC-Q-TOF-MS/MS的铁棒锤毒效成分定性及HPLC定量研究

Qualitative and Quantitative Study of the Toxicity Components of Aconitum pendulum Based on TLC,UPLC-Q-TOF-MS/MS and HPLC Technology

周蜜 1何姬 1刘妍如 1唐志书 2宋忠兴 1王兴弛 1张丽 3张德柱4

作者信息

  • 1. 陕西中医药大学 陕西中药资源产业化省部共建协同创新中心,陕西 咸阳 712083
  • 2. 陕西中医药大学 陕西中药资源产业化省部共建协同创新中心,陕西 咸阳 712083||北京中医药大学,北京 100700
  • 3. 陕西中医药大学 附属医院,陕西 咸阳 712000
  • 4. 陕西盘龙药业集团股份有限公司,陕西 商洛 711400
  • 折叠

摘要

Abstract

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 194.00-833.00 μg·mL-1(r≥0.999 6),respectively.The detection limits were 1.10 and 1.00 μg·mL-1,respectively,and the limits of quantification were 7.39 μg·mL-1 and 6.90 μg·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.

关键词

铁棒锤/超高效液相色谱-四极杆-飞行时间质谱法/薄层色谱法/高效液相色谱法

Key words

Aconitum pendulum Busch./UPLC-Q-TOF-MS/MS/thin layer chromatography/HPLC

分类

医药卫生

引用本文复制引用

周蜜,何姬,刘妍如,唐志书,宋忠兴,王兴弛,张丽,张德柱..基于TLC及UPLC-Q-TOF-MS/MS的铁棒锤毒效成分定性及HPLC定量研究[J].中国现代中药,2026,28(1):55-66,12.

基金项目

陕西省中医药科技创新提质扩能计划(TZKN-CXRC-23) (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) (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) (国中医药人教函[2023]96号)

中国现代中药

1673-4890

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