同位素内标-气相色谱质谱法测定海洋动物体中多溴联苯醚  

Simultaneous determination of PBDEs in marine organisms by gas chromatography-mass spectrometry based on stable isotope internal standards

作　　者：唐莉 孙秀梅[2] 金衍健 宋素平 郝青[2] 朱剑[2] 李铁军[2] 郭远明[2] TANG Li;SUN Xiumei;JIN Yanjian;SONG Suping;HAO Qing;ZHU Jian;LI Tiejun;GUO Yuanming(Marine and Fisheries Research Institute of Zhejiang Ocean University,Zhoushan 316012,China;Zhejiang Marine Fisheries Research Institute,Key Laboratory of Sustainable Utilization of Technology Research for Fisheries Resources of Zhejiang Province,Zhoushan 316021,China;Zhejiang Marine Ecology Environment Monitoring Center,Zhoushan 316021,China)

机构地区：[1]浙江海洋大学海洋与渔业研究所,浙江舟山316012 [2]浙江省海洋水产研究所,浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316021 [3]浙江省海洋生态环境监测中心,浙江舟山316021

出　　处：《农业环境科学学报》2025年第3期859-868,共10页Journal of Agro-Environment Science

基　　金：浙江省基础公益计划项目(LGF22B070004)。

摘　　要：为同时测定海洋动物体中13种多溴联苯醚(PBDEs),本研究建立了同位素内标-气相色谱-负化学源质谱方法。取2 g动物样品与13C12标记的8种同位素混合内标溶液混合,用正己烷-二氯甲烷(3∶1,V/V)混合溶剂进行超声提取,提取液酸化处理后经复合层析柱净化及正己烷-二氯甲烷(3∶1,V/V)混合溶剂洗脱,利用GC-NCI/MS的选择离子监测(SIM)模式分析测定13种PBDEs。结果表明13种PBDEs在0.1~20μg·L^(-1)内线性关系良好,相关系数(r^(2))>0.995(除BDE-206的r^(2)>0.98外),方法检出限(S/N=3)为0.01~0.46μg·kg^(-1),定量限(S/N=10)为0.02~1.52μg·kg^(-1)。应用该方法对采集的海洋动物样本进行分析检测,结果显示13种PBDEs均有不同程度检出,浓度范围为2.95~10.03μg·kg^(-1),中低溴代PBDEs含量较高。实际样品检测结果表明该方法适用于对海洋动物样品中包括BDE-209在内的13种PBDEs的准确定性定量分析。In order to simultaneously determine 13 polybrominated diphenyl ethers(PBDEs)in marine animals,an isotope internal standard-gas chromatography-negative chemical source mass spectrometry method was established.2 g of animal samples were mixed with 8 isotope mixed internal standard solutions labeled with 13C12,and 13 kinds of PBDEs were analyzed by GC-NCI/MS selective ion monitoring(SIM)mode by selective ion monitoring(SIM)mode.The results showed that the 13 PBDEs were effective in 0.1-20µg·L^(-1).The correlation coefficient(r^(2))was>0.995(except BDE-206,r^(2)>0.98),the detection limit(S/N=3)was 0.01-0.46µg·kg^(-1),and the quantitative limit(S/N=10)was 0.02-1.52µg·kg^(-1).The results showed that 13 kinds of PBDEs were detected in different degrees,with concentrations ranging from 2.95-10.03µg·kg^(-1) and the content of medium and low brominated PBDEs was high.The results of actual samples show that the method is suitable for the accurate qualitative and quantitative analysis of 13 PBDEs including BDE-209 in marine animal samples.

关 键 词：气相色谱-负化学源质谱 多溴联苯醚 海洋动物体 同位素内标 

分 类 号：X835[环境科学与工程—环境工程] O657.63[理学—分析化学]