摘要
应用自动化前处理设备和气相色谱串联四级杆质谱仪建立了淡水鱼体中10种有机磷阻燃剂的检测方法。该方法先采用自动索氏提取仪进行样品的提取,再应用凝胶渗透色谱净化仪和florisil柱对提取液进行两级净化,最后用气相色谱串联四级杆质谱法(多反应监测模式)对样品中的有机磷阻燃剂(OPFRs)定性定量。实验表明,凝胶渗透色谱净化系统在以乙酸乙酯∶环己烷(1∶1,V/V)为流动相,流速为5.0 m L·min-1的条件下,收集OPFRs的最佳时间为900~1 680 s;方法的检出限为0.002~0.192 ng·g^(-1)湿重,加标水平为5.000 ng·g^(-1)湿重时,平均加标回收率为48.7%~122%,相对偏差除磷酸三乙酯(TEP)(17.7%)和磷酸三(1,3-二氯异丙基)酯(TDCP)(11.9%)外均小于10%。应用该方法测定采集于东江某污水处理厂入河排污口的鱼类样品时,回收率指示物(d27-TBP)的回收率为82.4%~114%,鱼类样品中∑OPFRs的浓度范围为nd^6.41 ng·g^(-1)湿重。
An analytical method for the determination of 10 organophosphorus flame retardants （OPFRs） in freshwater fish samples was developed using automated equipment for pretreatment and gas chromatography-tandem mass spectrometry （GC-MS/MS） for quantification. In the present method, the samples were extracted using automatic soxhlet extraction system, and then a two-step clean-up （including automatic gel permeation chromatography （GPC） and florisil） was used to purify the extract. Finally, the GC-MS/MS was used for qualitation and quantitation by multi-reaction monitoring （MRM） mode. Experimental results showed that the best collection time of the automatic GPC system was from 900 to 1 680 seconds using ethyl acetate and hexane mixture （1：1, V/V） as mobile phase at a flow rate of 5.0 mL ·min^-1. The method detection limits ranged from 0.002 ng· g^-1 to 0.192 ng ·g^-1 wet weight, and the recoveries were in the range of 48.7%-122%, with relative standard deviations （RSDs） of less than 10% except for triethylphosphate （TEP） （17.7%） and tris（1,3-dichloropropyl） phosphate （TDCP） （11.9%）. The developed method was applied to determine the OPFRs in freshwater fish collected from an outlet of a sewage treatment plant in the East River. The recoveries of d27-TBP spiked in the samples ranged from 82.4% to 114%, and the total concentrations of OPFRs in the samples ranged from not detected to 6.41 ng ·g^-1 wet weight.
出处
《生态毒理学报》
CAS
CSCD
北大核心
2017年第3期604-610,共7页
Asian Journal of Ecotoxicology
基金
国家自然科学基金项目(41303082)
关键词
有机磷阻燃剂
自动化
串联质谱
淡水鱼体
organophosphorus flame retardants
automation
tandem mass spectrometry
freshwater fish
