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
刘川 1陈燕秋 1林浩 1汪璐瑶 1石培育 1刘蓉 1王义 1吴文林 1毛锐 1肖全伟 1宋娟 1戴琴1
作者信息
- 1. 成都市食品检验研究院,四川 成都 611130;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;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;辐照保藏四川省重点实验室,四川 成都 611130
- 折叠
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.
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.
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Key words
solid-phase extraction/ultra-high performance liquid chromatography-tandem mass spectrometry/honey/plant toxins引用本文复制引用
出版年
2025
国家科技期刊平台
NSTL
万方数据