一体化QuEChERS净化-超高效液相色谱-串联质谱法测定茶叶中27种吡咯里西啶类生物碱

doi:10.13305/j.cnki.jts.2024.05.005

茶叶科学 ›› 2024, Vol. 44 ›› Issue (5): 831-842.doi: 10.13305/j.cnki.jts.2024.05.005

一体化QuEChERS净化-超高效液相色谱-串联质谱法测定茶叶中27种吡咯里西啶类生物碱

姚蕾珺^1,2,3,4, 陈燕秋^1,2,3,4, 林浩^1,2,3,4, 汪璐瑶^1,2,3,4, 石培育^1,2,3,4, 张阳阳^1,2,3,4, 黄婷^1,2,3,4, 宋娟^1,2,3,4, 王义^1,2,3,4, 戴琴^1,2,3,4,*, 刘川^1,2,3,4,*

1.成都市食品检验研究院,四川成都 611130;
2.国家市场监督管理总局重点实验室（新食品原料监测与评价）,四川成都 611130;
3.国家市场监督管理总局重点实验室（营养与健康化学计量及应用）,北京 100029;
4.辐照保藏四川省重点实验室,四川成都 611130

收稿日期:2024-07-19 修回日期:2024-09-13 出版日期:2024-10-15 发布日期:2024-11-08
通讯作者: *740747208@qq.com;liuchuanai@hotmail.com
作者简介:姚蕾珺,女,工程师,研究方向为食品安全与质量检测。
基金资助:
国家重点研发计划项目（2022YFF0710405）、四川省科技计划重点研发项目（2022YFS0511、2023YFS0402）、2023年成都市食品安全风险研究项目（2023spfx07）

Simultaneous Determination of 27 Pyrrolizidine Alkaloids in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Integrated QuEChERS Purification

YAO Leijun^1,2,3,4, CHEN Yanqiu^1,2,3,4, LIN Hao^1,2,3,4, WANG Luyao^1,2,3,4, SHI Peiyu^1,2,3,4, ZHANG Yangyang^1,2,3,4, HUANG Ting^1,2,3,4, SONG Juan^1,2,3,4, WANG Yi^1,2,3,4, DAI Qin^1,2,3,4,*, LIU Chuan^1,2,3,4,*

1. Chengdu Institute of Food Inspection, Chengdu 611130, China;
2. Key Laboratory of Monitoring and Assessment on Novel Food Raw Materials, State Administration for Market Regulation, Chengdu 611130, China;
3. Key Laboratory of Chemical Metrology and Applications on Nutrition and Health, State Administration for Market Regulation, Beijing 100029, China;
4. Irradiation Preservation Key Laboratory of Sichuan Province, Chengdu 611130, China

Received:2024-07-19 Revised:2024-09-13 Online:2024-10-15 Published:2024-11-08

摘要/Abstract

摘要： 针对茶叶中吡咯里西啶类生物碱（Pyrrolizidine alkaloids,PAs）的残留风险,并为进一步提高传统QuEChERS的检测效率,研究建立使用一体化QuEChERS净化-超高效液相色谱-串联质谱测定茶叶中27种PAs的检测方法。该方法中的试样经1%甲酸乙腈提取,使用离心管一体盐包盐析和下压式QuEChERS净化,多反应监测模式（MRM）检测,基质匹配外标法定量。结果表明,27种PAs在各自浓度范围内线性关系良好,平均回收率为73.0%~111.8%,相对标准偏差为1.6%~13.8%（n=6）。该方法具有操作简单、检测通量大、灵敏度高、减少传统QuEChERS反复开盖等特点,能够满足茶叶中PAs的监测需求。对实际60批次茶叶样品进行检测,部分茶叶样品分别检出了不同含量的PAs,证明茶叶中有残留该类植物毒素的风险,建议持续跟踪监测。

关键词: 茶叶, 超高效液相色谱-串联质谱, QuEChERS, 吡咯里西啶类生物碱

Abstract: In this study, an integrated QuEChERS purification-ultra-performance liquid chromatography-tandem mass spectrometry method was established to detect 27 pyrrolizidine alkaloids (PAs) in tea, taking into account the residual risk of PAs in tea and the challenges of traditional QuEChERS. The method involves extracting the sample with 1% formic acid in acetonitrile, salting out using the centrifuge tube integrated salt bag and Down-Pressure QuEChERS Cleanup, detecting by multiple reaction monitoring mode (MRM), and quantifying it using the matrix-matched external standard method. The 27 PAs exhibit a strong linear relationship within their concentration ranges, with average recovery rates ranging from 73.0% to 111.8% and relative standard deviations from 1.6% to 13.8% (n=6). This method has the characteristics of simple operation, large detection throughput, high sensitivity, and reduction of repeated opening of the traditional QuEChERS, meeting the monitoring requirements for PAs in tea. During the actual testing of 60 batches of samples, different levels of PAs were detected in some tea samples, proving that there is indeed a risk of these plant toxins in tea, and continuous monitoring and tracking is recommended.

Key words: tea, UPLC-MS/MS, QuEChERS, pyrrolizidine alkaloids

中图分类号:

S571.1

姚蕾珺, 陈燕秋, 林浩, 汪璐瑶, 石培育, 张阳阳, 黄婷, 宋娟, 王义, 戴琴, 刘川. 一体化QuEChERS净化-超高效液相色谱-串联质谱法测定茶叶中27种吡咯里西啶类生物碱[J]. 茶叶科学, 2024, 44(5): 831-842. doi: 10.13305/j.cnki.jts.2024.05.005.

YAO Leijun, CHEN Yanqiu, LIN Hao, WANG Luyao, SHI Peiyu, ZHANG Yangyang, HUANG Ting, SONG Juan, WANG Yi, DAI Qin, LIU Chuan. Simultaneous Determination of 27 Pyrrolizidine Alkaloids in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Integrated QuEChERS Purification[J]. Journal of Tea Science, 2024, 44(5): 831-842. doi: 10.13305/j.cnki.jts.2024.05.005.

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一体化QuEChERS净化-超高效液相色谱-串联质谱法测定茶叶中27种吡咯里西啶类生物碱

Simultaneous Determination of 27 Pyrrolizidine Alkaloids in Tea by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Integrated QuEChERS Purification

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