摘要
建立基于GC-MS/MS方法,采用稳定性同位素稀释法测定鱼肉中二噁英及二噁英类多氯联苯。样品经快速溶剂萃取仪提取3次,以酸化硅胶除脂,经多层硅胶柱、碱性氧化铝柱和活性炭柱净化,分别收集含PCDD/Fs和DL-PCBs组分,经浓缩复溶后供GC-MS/MS测定。结果表明:在净化步骤中,PCDD/Fs和DL-PCBs受洗脱液的体积以及收集步骤的影响较大,分开收集PCDD/Fs和DL-PCBs,先对PCDD/Fs的收集液进行测定,然后将其和DL-PCBs的收集液合并完成DL-PCBs的测定,从而对DL-PCBs进行准确定量。采用鱼肉为样品基质时,该方法PCDD/Fs和DL-PCBs的内标回收率为63.3%~106.8%,RSD为0.4%~9.6%;目标物的回收率为93.6%~114.5%,RSD为0.9%~9.2%,方法线性和检出限达到国家标准GB 5009.205的要求,适用于鱼肉样品中PCDD/Fs和DL-PCBs的测定。
Based on GC-MS/MS,a stable isotope dilution method was established for the determination of dioxins and dioxin like polychlorinated biphenyls in fish.The sample was extracted by rapid solvent extractor for 3 times,and the fat was removed by acidified silica gel.Then,after purification by multi-layer silica gel column,alkaline alumina column and activated carbon column,the elution samples containing PCDD/Fs and DL-PCBs were collected respectively.Finally,it is concentrated and redissolved for GC-MS/MS determination.In this experiment,the extraction,purification and determination steps of samples were optimized and discussed.The results show that in the purification step,PCDD/Fs and DL-PCBs are greatly affected by the volume of washing liquid and collection step.PCDD/Fs and DL-PCBs are collected separately.Firstly,the collection solution of PCDD/Fs was measured,and then it was combined with the collection solution of DL-PCBs to complete the determination of DL-PCBs,thereby accurately quantifying DL-PCBs.When the fish was detected,the internal standard recoveries of PCDD/Fs and DL-PCBs were 63.3%-106.8%and RSD was 0.4%-9.6%;The recovery rate of the target substance is 93.6%-114.5%,and the RSD is 0.9%-9.2%,which meets the relevant requirements of the national standard of GB 5009.205.It is suitable for the determination of PCDD/Fs and DL-PCBs in actual fish samples.
作者
陆静
申甜甜
焦艳娜
崔凤云
朱绍华
成婧
易锡
付善良
Lu Jing;Shen Tiantian;Jiao Yanna;Cui Fengyun;Zhu Shaohua;Cheng Jing;Yi Xi;Fu Shanliang(Technology Center of Changsha Customs,Hunan Key Laboratory of Food Safety Science&Technology,Changsha 410004;Science and Technology Research Center of China Customs,Beijing 100026)
出处
《中国食品学报》
EI
CAS
CSCD
北大核心
2023年第9期376-387,共12页
Journal of Chinese Institute Of Food Science and Technology
基金
海关总署科技计划项目(2021HK202)。
作者简介
第一作者:陆静,女,博士,工程师。;通信作者:付善良。E-mail:fsl432@163.com。
