摘要
建立不同类别茶叶中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-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)同时测定方法。茶叶样品经粉碎均匀后,用加速溶剂仪提取,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、2倍定量限和10倍定量限3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,相对标准偏差为0.1%~9.3%,方法的检出限在0.11~4.3μg/kg之间。方法实现对68种POPs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。
A method based on gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for the determination of 68 persistent organic pollutants(POPs)including 16 polycyclic aromatic hydrocarbons,19 phthalate esters,18 polychlorinated biphenyls and 15 organic chlorines in various teas.Tea samples were crushed and extracted by an accelerated solvent extractor,and the extract was cleaned up by a molecular imprinted polymer solid phase extraction column,and further purified by the QuEChERS method.The analytes were separated on a DB-5ms capillary column and analyzed by GC-MS/MS,where the triple quadrupole mass spectrometer was operated in the multi-reaction monitoring(MRM)mode,effectively reducing the background interference from the tea substrate.In 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 three spiked concentration levels of limit of quantification(LOQ),2-fold LOQ and 10-fold LOQ.The limits of detection(LOD)of the proposed method ranged from 0.11 to 4.3μg/kg.In conclusion,this method can be used for accurate qualitation and quantification of the 68 POPs in tea samples.Moreover,its stability and feasibility have been verified by testing 60 batches of tea samples.
作者
徐清
戴明
刘文菁
欧阳立群
林钦
王征
XU Qing;DAI Ming;LIU Wenjing;OUYANG Liqun;LIN Qin;WANG Zheng(Fujian Inspection and Research Institue for Product Quality,Fuzhou 350002,China)
出处
《食品科学》
EI
CAS
CSCD
北大核心
2022年第20期361-369,共9页
Food Science
基金
福建省监督管理局科技项目(FJMS2019010)
关键词
茶叶
持久性有机污染物
气相色谱-串联质谱
加速溶剂萃取
分子印迹固相萃取
tea
persistent organic pollutants
gas chromatography-tandem mass spectrometry
accelerated solvent extractor
molecular imprinted polymer solid phase extraction
