固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中39 种植物源性毒素

doi:10.7506/spkx1002-6630-20240718-186

食品科学 ›› 2025, Vol. 46 ›› Issue (2): 231-239.doi: 10.7506/spkx1002-6630-20240718-186

固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中39 种植物源性毒素

刘川，陈燕秋，林浩，汪璐瑶，石培育，刘蓉，王义，吴文林，毛锐，肖全伟，宋娟，戴琴

（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）

出版日期:2025-01-25 发布日期:2024-12-30
基金资助:
“十四五”国家重点研发计划重点专项（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 39 Plant Toxins in Honey by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

LIU Chuan, CHEN Yanqiu, LIN Hao, WANG Luyao, SHI Peiyu, LIU Rong, WANG Yi, WU Wenlin, MAO Rui, XIAO Quanwei, SONG Juan, DAI Qin

(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)

Online:2025-01-25 Published:2024-12-30

摘要/Abstract

摘要： 为有效评估蜂蜜中可能残留多种植物源性毒素的食品安全风险，建立和验证固相萃取-超高效液相色谱-串联质谱测定蜂蜜中39 种植物源性毒素的检测方法。试样经0.1%甲酸水提取，HLB小柱净化，多反应监测模式检测，基质匹配外标法定量。本方法中39 种植物源性毒素在各自浓度范围内线性关系良好，平均回收率介于78.7%～112.8%，相对标准偏差介于1.6%～15.2%（n＝6）。该方法具有操作简单、检测通量大、灵敏度高等特点，能够满足蜂蜜中该类毒素监测的应用需求。在实际36 批次样品的检测过程中，部分样品分别检出了不同含量的吡咯里西啶生物碱和闹羊花毒素III，证明蜂蜜中确具有残留该类植物毒素的风险。

关键词: 固相萃取；超高效液相色谱-串联质谱；蜂蜜；植物源性毒素

Abstract: To effectively assess food safety risks associated with potential plant toxin residues present in honey, this study aimed to establish and validate a method for the detection of 39 plant toxins in honey using solid-phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The developed method involved sample extraction with 0.1% formic acid, purification using a hydrophilic-lipophilic balanced (HLB) cartridge, detection in the multiple reaction monitoring (MRM) mode, and quantification using the matrix-matched external standard method. The calibration curves exhibited good linearity for all the analytes. Average recoveries ranged from 78.7% to 112.8% with relative standard deviation (RSD) between 1.6% and 15.2% (n = 6). This method was characterized by ease of operation, high throughput and high sensitivity, and could be used for the monitoring these toxins in honey. Varying levels of pyrrolizidine alkaloids (PAs) and rhodojaponin III were detected in some of the 36 tested batches of honey, confirming the presence of phytotoxin residue risks in honey.

Key words: solid-phase extraction; ultra-high performance liquid chromatography-tandem mass spectrometry; honey; plant toxins

中图分类号:

O657.63

刘川，陈燕秋，林浩，汪璐瑶，石培育，刘蓉，王义，吴文林，毛锐，肖全伟，宋娟，戴琴. 固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中39 种植物源性毒素[J]. 食品科学, 2025, 46(2): 231-239.

LIU Chuan, CHEN Yanqiu, LIN Hao, WANG Luyao, SHI Peiyu, LIU Rong, WANG Yi, WU Wenlin, MAO Rui, XIAO Quanwei, SONG Juan, DAI Qin. Simultaneous Determination of 39 Plant Toxins in Honey by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction[J]. FOOD SCIENCE, 2025, 46(2): 231-239.

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固相萃取-超高效液相色谱-串联质谱法测定蜂蜜中39 种植物源性毒素

Simultaneous Determination of 39 Plant Toxins in Honey by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

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