Rapid Screening of Chemical Risk Substances in Honey by Sugar Extraction/Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

GAO Jia; LIU Meng-ying; REN Bei-bei; LU Yang; CHEN Fu-zun; WANG Li-ying; KANG Wei-jun

doi:10.19969/j.fxcsxb.23071402

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Rapid Screening of Chemical Risk Substances in Honey by Sugar Extraction/Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry

Scientific Papers | 更新时间：2023-10-18

- Rapid Screening of Chemical Risk Substances in Honey by Sugar Extraction/Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1233-1241(2023)
- 作者机构：
  
  1.河北医科大学公共卫生学院，河北石家庄 050017
  2.河北省疾病预防控制中心，河北石家庄　050021
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23071402
  CLC：
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高佳,刘梦颖,任贝贝等.糖析萃取/超高效液相色谱-四极杆/静电场轨道阱质谱快速筛查蜂蜜中的化学风险物质[J].分析测试学报,2023,42(10):1233-1241.

GAO Jia,LIU Meng-ying,REN Bei-bei,et al.Rapid Screening of Chemical Risk Substances in Honey by Sugar Extraction/Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1233-1241.
高佳,刘梦颖,任贝贝等.糖析萃取/超高效液相色谱-四极杆/静电场轨道阱质谱快速筛查蜂蜜中的化学风险物质[J].分析测试学报,2023,42(10):1233-1241. DOI： 10.19969/j.fxcsxb.23071402.

GAO Jia,LIU Meng-ying,REN Bei-bei,et al.Rapid Screening of Chemical Risk Substances in Honey by Sugar Extraction/Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1233-1241. DOI： 10.19969/j.fxcsxb.23071402.

摘要

基于糖析萃取/超高效液相色谱-四极杆/静电场轨道阱高分辨质谱技术，建立了蜂蜜中68种化学风险物质的分析方法。蜂蜜样品提取液经色谱柱分离，进入四极杆/静电场轨道阱高分辨质谱进行数据采集。通过对比样品与标准品一级质谱分子离子精确质量数、保留时间、同位素丰度比对所得数据进行初筛；初筛得到的阳性化合物采用二级碎片离子进一步确证。该方法实现了蜂蜜中68种风险物质的同时精准筛查，目标风险物质的检出限为0.03~2.73 μg/kg，定量下限为0.10~9.00 μg/kg，平均加标回收率为50.7%~122%，相对标准偏差为1.0%~15%。采用所建立的方法对32份市售蜂蜜样品进行检测，在12份样品中检出蝇毒磷，检出含量范围为0.74~24.87 µg/kg。该方法通量高、速度快、定量准确，可用于蜂蜜中风险物质的快速筛查。

Abstract

An analytical method for detection of 68 chemical risk substances in honey was established based on sugar extraction/ultra high performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry technology. The honey extracts were separated by a chromatographic column and then analyzed by quadrupole electrostatic field orbitrap high resolution mass spectrometry. The acquired sample information and the standard information were preliminary screening through the accurate mass number，retention time and isotope distribution ratio comparison. The positive compounds in the initial screening were further confirmed by comparing the secondary fragment ions. This method can accurately screen 68 risk substances in honey within 17 minutes，with the detection limits of 0.03-2.73 μg/kg，the quantification limits of 0.10-9.00 μg/kg，the recoveries of 50.7%-122% and the relative standard deviations（RSDs） of 1.0%-15%. This method was used to detect 32 honey samples，and coumaphos was detected in 12 samples，with the detection concentration ranging from 0.74 to 24.87 µg/kg. This method has high throughput，fast speed，and accurate quantification，and can be used for rapid screening of risk substances in honey.

关键词

超高效液相色谱高分辨质谱快速筛查糖析萃取蜂蜜

Keywords

ultra high performance liquid chromatography（UPLC）high resolution mass spectrometryrapid screeningsugar extractionhoney

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