食品与发酵工业 >

2025 , Vol. 51 >Issue 12: 319 - 326

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.040667

分析与检测

基于分散固相萃取-高效液相色谱串联质谱技术快速测定食品中十种钩吻生物碱

  • 曾羲 ,
  • 徐振林 ,
  • 胡凌 ,
  • 毛新武 ,
  • 刘春生 ,
  • 刘昕 ,
  • 王宇 ,
  • 于洋
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  • 1(广州市食品检验所,广东 广州,511400)
    2(华南农业大学 食品学院,广东省食品质量安全重点实验室,广东 广州,510642)
    3(黄埔海关技术中心,广东 东莞,510700)
第一作者:博士研究生,高级工程师(徐振林教授为通信作者,E-mail:jallent@163.com)

收稿日期: 2024-08-14

  修回日期: 2024-10-22

  网络出版日期: 2025-07-11

基金资助

国家自然科学基金项目(32372448);广东省基础与应用基础研究基金项目(2023A1515012605);广东省市场监督管理局科技项目(2023CS01)

收起

Rapid determination of ten alkaloids of Gelsemium elegans with dispersed solid phase extraction-high performance liquid chromatographytandem mass spectrometry technique

  • ZENG Xi ,
  • XU Zhenlin ,
  • HU Ling ,
  • MAO Xinwu ,
  • LIU Chunsheng ,
  • LIU Xin ,
  • WANG Yu ,
  • YU Yang
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  • 1(Guangzhou Institute for Food Inspection, Guangzhou 511400, China)
    2(College of Food Science, South China Agricultural University, Guangdong Provincial Key Laboratory of Food Quality and Safety, Guangzhou 510642, China)
    3(Huangpu Customs Technology Center, Dongguan 510700, China)

Received date: 2024-08-14

  Revised date: 2024-10-22

  Online published: 2025-07-11

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摘要

钩吻生物碱是引起钩吻中毒的主要成分,严重威胁人民群众的生命健康。该文建立了分散固相萃取-高效液相色谱串联质谱(high performance liquid chromatography tandem mass spectrometry, HPLC-MS/MS)法同时快速分析食品中10种钩吻生物碱的方法。食品样品经1%(体积分数)HCl超声提取后调pH值至11~12,加入乙腈涡旋振荡提取后,以NaCl辅助分层离心,上清液经无水Na2SO4和C18脱水净化后,离心所得上清液吹干复溶,在电喷雾正离子模式(ESI+)下,采用多反应监测模式,以0.1%氨水-10 mmol/L乙酸铵溶液和乙腈为流动相,经Hilic (2.1 mm×100 mm×1.7 μm)柱梯度洗脱分离测定,采用基质标曲外标法定量。结果表明,钩吻生物碱的基质效应为13.1%~3 692.7%,在0.5~10.0 ng/mL线性良好,相关系数(R)在0.995以上,检出限和定量限分别为0.075~0.225 ng/g和0.250~0.750 ng/g,在4种食品基质中3个水平的加标回收率为79.3%~118.7%,相对标准偏差为0.1%~12.1%(n=6)。该方法操作简单、高效、灵敏度高,对误食钩吻引起的急性中毒事件诊断并采取必要措施保障生命安全具有重要现实意义。

关键词： 高效液相色谱-串联质谱; 分散固相萃取; 钩吻中毒; 断肠草误食; 大茶药; 生物碱; 钩吻碱

本文引用格式

曾羲 , 徐振林 , 胡凌 , 毛新武 , 刘春生 , 刘昕 , 王宇 , 于洋 . 基于分散固相萃取-高效液相色谱串联质谱技术快速测定食品中十种钩吻生物碱[J]. 食品与发酵工业, 2025 , 51(12) : 319 -326 . DOI: 10.13995/j.cnki.11-1802/ts.040667

Abstract

The alkaloids in Gelsemium elegans are the main components leading to acute poison, which threat to the public health seriously.This work established a method for simultaneously analysis of ten alkaloids in G.elegans using dispersed solid phase extraction-high performance liquid chromatography tandem mass spectrometry technique.Food samples were extracted and ultrasound by 1%HCl before the pH was adjusted to 11-12.And then acetonitrile were added to vortex, latter NaCl were added to assisted centrifugation and stratification.The supernatant was dehydrated and purified by Na2SO4 and C18, respectively.After centrifugation, the supernatant was dried by nitrogen and then redissolved by acetonitrile.The sample was conducted in positive electrospray ionization (ESI+) mode under multiple reaction monitoring mode, coupled with gradient elution by 0.1% NH4OH-10 mmol/L CH3COONH4 solvent and acetonitrile as mobile phase and Hilic (2.1 mm×100 mm×1.7 μm) chromatographic column.The quantification of alkaloids were conducted by matrix standard method.As a result, the matrix effect were 13.1%-3 692.7%, which can be eliminated by corresponding matrix standard.The linearity were good in the range of 0.5-10.0 ng/mL, with the regression coefficients (R) all above 0.995.The limit of detection (LOD) and the limit of quantitation (LOQ) were 0.075-0.225 ng/g and 0.250-0.750 ng/g, respectively.The recoveries were 79.3%-118.7%, and the relative standard deviations were 0.1%-12.1% (n=6) in four different sorts of food samples at three spiked levels.This method is easy, effective and high-sensitive, laid the foundation of rapid detection technique of acute G.elegans poison and owned critical significance of guarantee the public health.

Key words： high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS); dispersed solid phase extraction; Gelsemium elegans poisoning; Gelsemium elegans mistaken; graceful jesamine; alkaloids; Gelsemium elegans alkaloids

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