食品与发酵工业 >

2026 , Vol. 52 >Issue 10: 373 - 381

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.043879

分析与检测

茶叶中31种吡咯里西啶类生物碱的检测方法研究

  • 李佳雯 ,
  • 吴微 ,
  • 冯德建 ,
  • 陶昕语 ,
  • 李学理 ,
  • 曾献春
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  • 1(成都医学院 检验医学院,四川 成都,610500)
    2(中国测试技术研究院 生物研究所,四川 成都,610000)
    3(成都医学院 动物源性食品兽药残留防控技术四川省工程研究中心,四川 成都,610500)
第一作者:硕士研究生(曾献春教授为通信作者,E-mail:1149125188@qq.com)

收稿日期: 2025-07-14

  修回日期: 2025-10-29

  网络出版日期: 2026-06-15

基金资助

四川省科技厅重点研发项目(2023YFS0398);四川省科技厅重点研发项目(2024YFFK0429);成都市重点研发支撑计划项目(2022-YF05-00994-SN);中国测试技术研究院“人才计划”项目(RC202407)

收起

Research on the detection method of 31 pyrrolizidine alkaloids in tea

  • LI Jiawen ,
  • WU Wei ,
  • FENG Dejian ,
  • TAO Xinyu ,
  • LI Xueli ,
  • ZENG Xianchun
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  • 1(School of Laboratory Medicine, Chengdu Medical College, Chengdu 610500, China)
    2(Institute of Biological Technology, National Institute of Measurement and Testing Technology, Chengdu 610000, China)
    3(Sichuan Provincial Engineering Laboratory for Prevention and Control Technology of Veterinary Drug Residue in Animal-origin Food, Chengdu Medical College, Chengdu 610500, China)

Received date: 2025-07-14

  Revised date: 2025-10-29

  Online published: 2026-06-15

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摘要

基于茶叶中吡咯里西啶类生物碱(pyrrolizidine alkaloids,PAs)污染引发的食品安全风险,该研究建立了一种超高效液相色谱-串联质谱同时检测茶叶中31种PAs及PAs氮氧化物(PAs N-oxides,PANOs) 的高灵敏度、高通量检测方法。样品经酸化乙醇溶液提取结合PXC(Phase Extraction Cartridges)固相萃取柱净化,有效消除了茶叶基质中多酚、色素及生物碱的干扰;选用Agilent Eclipse Plus C18色谱柱,梯度洗脱程序的流动相为甲醇、含5 mmol/L甲酸铵的0.1%(体积分数)甲酸水,在正离子多反应监测模式下检测;基质匹配外标法定量。31种PAs在浓度范围内相关系数r2＞0.997;定量限为0.2~2 μg/kg;检出限为0.06~0.66 μg/kg;低、中、高3个加标水平下的平均回收率为60.4%~101.6%;相对标准偏差为0.1%~6.0%。研究表明该方法具有良好的准确度与精密度,适用于茶叶中多种PAs及PANOs的同时检测。

关键词： 茶叶; 吡咯里西啶类生物碱; 检测分析; 超高效液相色谱-串联质谱; 固相萃取

本文引用格式

李佳雯 , 吴微 , 冯德建 , 陶昕语 , 李学理 , 曾献春 . 茶叶中31种吡咯里西啶类生物碱的检测方法研究[J]. 食品与发酵工业, 2026 , 52(10) : 373 -381 . DOI: 10.13995/j.cnki.11-1802/ts.043879

Abstract

In response to the food safety risks caused by pyrrolizidine alkaloids (PAs) contamination in tea, this study developed a highly sensitive detection method for simultaneously determining 31 hepatotoxic PAs and PAs N-oxides (PANOs) in tea using UHPLC-MS/MS.This method has the widest detection range among the relevant reported in the literature at present.Acidified ethanol extraction and subsequent Mixed-mode Strong Cation Exchange Reverse-phase Solid Phase Extraction Cartridges (PXC) purification of samples effectively eliminated polyphenol, pigment, and alkaloid interference in the tea matrix.The separation was carried out on an Agilent Eclipse Plus C18 column with a gradient elution of methanol and 0.1% formic acid water (containing 5 mmol/L ammonium formate) as the mobile phase.Detection was performed in positive ion MRM mode.The method was quantified by matrix-matched standard curve external standard method.The results showed that the 31 target compounds had good linearity within the concentration range (r2>0.997), and isomers could be baseline separated.The method's limit of quantification (LOQ) was 0.2-2 μg/kg, and the limit of detection (LOD) was 0.06-0.66 μg/kg.At low, medium and high spiked concentration levels, the average spiked recovery rate from 60.4% to 101.6%, with a relative standard deviation (RSD) of 0.1% to 6.0%.The above validation data indicate that the method has good accuracy and repeatability, and is suitable for the simultaneous detection of 31 PAs and PANOs in tea.It can provide technical support for the upgrading of the quality monitoring system of China’s tea trade.

Key words： tea; pyrrolizidine alkaloids; detection analysis; ultra high performance liquid chromatography-mass spectrometry; solid phase extraction

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