摘要
利用气相色谱-电子捕获检测器(GC-ECD),建立了牡蛎中11种多溴联苯醚(PBDEs)同时测定方法。优化了气相法与质谱联用法仪器条件,考察了不同提取溶液、固相萃取柱、净化方式等前处理条件对提取和净化效果的影响。结果表明,GC-ECD对高溴组分更灵敏;牡蛎加标样品经正己烷-二氯甲烷(1:1,V/V)提取,弗洛里硅土柱-浓硫酸净化,GC-ECD测定,PBDEs各组分标准曲线线性良好(r>0.998),二至九溴联苯醚和十溴联苯醚方法检出限分别为0.05 ng/g和0.1 ng/g,回收率范围为80.3%~104%,相对标准偏差范围为3.0%~12%。方法可用于牡蛎中二至十溴联苯醚同时检测。
A simplified analytical method was developed for the determination of 11 polybrominated diphenyl ethers(PBDEs)congeners in oyster samples by gas chromatography with electron-capture detection(GC-ECD).The instrument conditions of gas chromatography and gas chromatography coupled with triple quadrupole mass spectrometry(GC-MS/MS)were optimized.The preparation parameters were investigated,including extraction solvents,solid-phase extraction(SPE)columns and purification procedure.The results showed that GC-ECD had the higher sensitivity to high brominated congeners and the best results were obtained using the solution mixed with hexane and dichloromethane at the ration of 1:1,followed by Florisil SPE and H2 SO4 digestion during GC-ECD analysis in oyster samples spiked with PBDEs.The calibration curves had good linearity with correlation coefficients(r)higher than 0.998.The method detection limits of 2-9 brominated congeners and deca-BDE were0.05 and 0.1 ng/g,respectively.The recoveries ranged from 80.3%to 104%and the RSDs ranged from 3.0%to 12%.The method can be used to detect 2-10 brominated diphenyl ethers in oyster samples simultaneously.
作者
刘奇
柯常亮
莫梦松
陈洁文
刘卓坚
黄珂
LIU Qi;KE Chang-liang;MO Meng-song;CHEN Jie-wen;LIU Zhuo-jian;HUANG Ke(South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Key Laboratory of Aquatic Product Processing,Ministry of Agriculture and Rural Affairs,Guangzhou 510300)
出处
《分析试验室》
CAS
CSCD
北大核心
2019年第11期1339-1344,共6页
Chinese Journal of Analysis Laboratory
基金
中国水产科学研究院南海水产研究所中央级公益性科研院所基本科研业务费专项资金(2016TS22)
国家农产品质量安全风险评估重大专项(GJFP20180903)资助
关键词
多溴联苯醚
气相色谱
牡蛎
Polybrominated diphenyl ethers(PBDEs)
Gas chromatography
Oyster
