GC-MS/MS法测定茶叶中68种持久性有机污染物

摘要/Abstract

摘要： 建立了不同类别茶叶中16种多环芳烃、19种邻苯二甲酸酯、18种多氯联苯、15种有机氯农药共68种持久性有机污染物（Persistent Organic Pollutants，POPs）的气相色谱-三重四极杆质谱(gas chromatography- tandem mass spectrometry，GC-MS/MS)同时测定分析方法。茶叶样品经粉碎均匀后，用加速溶剂仪（accelerated solvent extractor， ASE）提取，先用分子印迹柱净化，再采用QuEchERs法进一步净化，采用 DB-5ms毛细管柱分离，三重四极杆质谱多反应监测(Multiple Reaction Monitoring，MRM)模式有效降低茶叶基质的背景干扰，GC-MS/MS分析检测。在各POPs的1倍定量限、2倍定量限和10倍定量限三个添加水平，在选定的绿茶、黑茶样品中的回收率在73.1%～109.5%之间，相对标准偏差(relative standard deviation，RSD)为 0.1%～9.3%，方法的检测限(detection of limit，LOD)在 0.11～4.3μg/kg 之间。方法实现对68种持久性有机污染物目标物的精准定性定量，并通过对市售的60批茶叶样品的检测，验证方法的稳定性和可行性。

关键词: 茶叶, 持久性有机污染物（POPs）, 气相色谱-三重四极杆质谱(GC-MS/MS), 加速溶剂萃取（ASE）, 分子印迹固相萃取

Abstract: A method based on gas chromatography-tandem mass spectrometry was developed for deternimation of 68 kinds of persistent organic pollutants (POPs) including 16 kinds of polycyclic aromatic hydrocarbons, 19 kinds of phthalate esters , 18 kinds of polychlorinated biphenyls and 15 kinds of organic chlorines in various teas. The crushed tea samples were extracted by accelerated solvent extractor， then cleaned up by molecular imprinted polymer solid phase extraction column , then further purified by QuEchERs method. The analytes were separated on a DB-5ms capillary column and analysed by GC-MS/MS which the triple quadrupole mass spectrometry multi-reaction monitoring (Multiple Reaction Monitoring,MRM) mode effectively reduced the background interference of the tea substrate.In the selected green tea and dark tea samples ,the recoveries for the analytes were from 73.1% to 109.5% with a relative standard deviation (RSD) from 0.1% to 9.3% at the spike levels of limits of quantification(LOQ), 2-fold LOQ and 10-fold LOQ. The limits of detection (LOD) of the method ranged from 0.11 to 4.3 μg/kg. In conclusion, this method was determinated to achieve accurate qualitative and quantification of 68 persistent organic pollutants in tea samples。The stability and feasibility of the method were verified by testing 60 batches of tea samples.

Key words: tea, persistent organic pollutants (POPs), gas chromatography-Triple quadrupole Pole Mass Spectrometry (GC-MS/MS), accelerated solvent extractor(ASE), molecular imprinted polymer solid phase extraction

中图分类号:

TS207.3

徐清戴明刘文菁欧阳立群林钦王征. GC-MS/MS法测定茶叶中68种持久性有机污染物[J]. 食品科学, 0, (): 0-0.

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