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液相色谱-串联质谱法测定曼陀罗中东莨菪碱、消旋山莨菪碱和阿托品

Determination of scopolamine, racanisodamine and atropine in Datura stramonium by liquid chromatography-tandem mass spectrometry

投稿时间：2025-02-28 修订日期：2025-05-09

DOI：

中文关键词: LC-MS/MS 曼陀罗东莨菪碱消旋山莨菪碱阿托品

英文关键词:LC-MS/MS Datura stramonium Scopolamine Racanisodamine Atropine

基金项目:江苏省重点研发计划(社会发展)项目(BE2023720)

作者	单位
邓淑铃	南京医科大学
朱峰	江苏省疾病预防控制中心
张昊	江苏省疾病预防控制中心
霍宗利	江苏省疾病预防控制中心
刘华良	南京医科大学，江苏省疾病预防控制中心
王联红	水污染控制与资源绿色循环全国重点实验室，南京大学环境学院，南京

Author	Institution
DENG Shu-Ling	School of Public Health,Nanjing Medical University
ZHU Feng	Jiangsu Provincial Center for Disease Control and Prevention
ZHANG Hao	Jiangsu Provincial Center for Disease Control and Prevention
HUO Zhong-Li	Jiangsu Provincial Center for Disease Control and Prevention
LIU Hua-Liang	School of Public Health,Nanjing Medical University and Jiangsu Provincial Center for Disease Control and Prevention
wang lian-hong	State Key Laboratory of Water Pollution Control and Green Resource Recycling, School of the Environment, Nanjing University, Nanjing

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中文摘要:

目的? 建立快速提取曼陀罗籽、曼陀罗花、曼陀罗壳、曼陀罗叶和曼陀罗茎的前处理法,采用液相色谱-串联质谱法(Liquid Chromatography-tandem Mass Spectrometry, LC-MS/MS)同时检测东莨菪碱、消旋山莨菪碱和阿托品。方法? 以甲醇提取曼陀罗籽,以1%甲酸水提取花、壳、叶、和茎,选用ACQUITY UPLC BEH C18(100 mm × 2.1 mm, 1.7 μm)为色谱柱,以甲酸水(0.1 %,体积分数)-甲醇溶液为流动相梯度洗脱,电喷雾离子源正离子扫描,多反应监测(multiple reaction monitoring, MRM)模式采集,外标法定量。结果? 在质量浓度0.1～10 ng/mL范围内,东莨菪碱、消旋山莨菪碱和阿托品呈现良好的线性关系(r≥0.999)；检出限(Method Detection Limit, MDL)为30~76 μg/kg,定量限(Method Quantification Limit, MQL)为80~253 μg/kg；三种生物碱在低、中、高三个加标浓度水平的平均回收率为80.1 % ~ 119.1 %,相对标准偏差(relative standard deviation, RSD)为0.7 %~7.2 %。结论? 该法操作简单、快速、准确,为测定曼陀罗多种组织中东莨菪碱、消旋山莨菪碱和阿托品提供了可靠的技术支持。

英文摘要:

ABSTRACT: Objective? To establish a method for the rapid extraction of Datura stramonium seeds, Datura stramonium flowers, Datura stramonium shells, Datura stramonium leaves and Datura stramonium stems and simultaneous determination of Scopolamine, Racanisodamine and Atropine by Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS). Methods? The Datura stramonium seeds were extracted with methanol solution and others were extracted with 1 % formic acid solution. An ACQUITY UPLC BEH C18 (100 mm × 2.1 mm, 1.7 μm) column was used for the qualitative and quantitative analysis of Scopolamine, Racanisodamine and Atropine by matrix matching curve external standard method in multiple reaction monitoring (MRM) mode using a methanol-formic acid (0.1%) aqueous solution as the mobile phase in a gradient elution and electrospray ionization (ESI) with a positive ion source. Results? Scopolamine, Racanisodamine and Atropine showed good linearity (R≥0.999) in the range of mass concentrations from 0.1 to 10 ng/mL. Method Detection Limit (MDL) was 0.03~0.76 μg/kg, Method Quantification Limit (MQL) was 0.08~2.53 μg/kg. The average recoveries of the three alkaloids at the low, medium and high spiked concentration levels ranged from 80.1 % ~ 119.1 %, and the relative standard deviations (RSDs) were from 0.7 %~7.2 % (n=6). Conclusion? The method is simple, rapid, accurate, can meet the rapid detection requirements of Scopolamine, Racanisodamine and Atropine in Datura stramonium.

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