引用本文:侯瑞,李逸,梁永津,赵彦龙,王旭涛.鱼类样品中有机磷阻燃剂分析方法的优化研究[J].环境监控与预警,2020,12(5):95-101
HOU Rui, LI Yi, LIANG Yong-jin, ZHAO Yan-long, WANG Xu-tao.Optimization of Determining Method for Organophosphate Flame Retardants (OPFRs) in Biological Tissues[J].Environmental Monitoring and Forewarning,2020,12(5):95-101
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鱼类样品中有机磷阻燃剂分析方法的优化研究
侯瑞,李逸,梁永津,赵彦龙,王旭涛
作者单位
侯瑞,李逸,梁永津,赵彦龙,王旭涛* 生态环境部珠江流域南海海域生态环境监督管理局生态环境监测与科学研究中心广东 广州 510610 
摘要:
建立了鱼类组织样品中有机磷阻燃剂(OPFRs)的分析方法,优化了萃取条件、净化条件、液相色谱条件和质谱检测参数。确定了生物样品经冷冻干燥后,以1∶1(V/V)的正己烷/二氯甲烷混合溶液进行加速溶剂萃取,利用氨基固相萃取柱进行净化,以1∶1(V/V)的正己烷/二氯甲烷、二氯甲烷和9∶1(V/V)的二氯甲烷/甲醇为洗脱液,最后用超高效液相色谱-串联质谱同时对9种OPFRs进行定性定量检测。结果表明,各物质的基质加标回收率均为56.5%~108%,方法的测定下限为0.016~0.104 ng/g (以脂重计),满足了生物样品中OPFRs的分析检测要求。利用该方法测定了北京和广州市养殖和野生鲫鱼肌肉组织样品,主要的OPFRs同族体为磷酸三正丁酯(TNBP)、磷酸三乙基己基酯(TEHP)、磷酸三(1-氯-2-丙基)酯(TCIPP)和磷酸三氯乙基酯(TCEP),质量比为5.94~33.7 ng/g(以脂重计),显示出良好的适用性。
关键词:  有机磷阻燃剂(OPFRs)  鱼类组织样品  超高效液相色谱串联质谱  固相萃取  净化
DOI:
分类号:X835
文献标识码:A
基金项目:国家自然科学基金青年项目基金资助项目(41907339)
Optimization of Determining Method for Organophosphate Flame Retardants (OPFRs) in Biological Tissues
HOU Rui, LI Yi, LIANG Yong-jin, ZHAO Yan-long, WANG Xu-tao
Abstract:
An optimized method for the cleanup and analysis of organophosphate flame retardants (OPFRs) in fish tissues was developed. The mixed solution of 1∶1 (V/V) n hexane/dichloromethane was used for accelerated solvent extraction of 9 OPFRs from biological samples which were freeze dried in advance, the extracts were then loaded onto the NH2 solid phase extraction cartridges which were then eluted with dichloromethane/n hexane mixture (1∶1,V/V), dichloromethane and the dichloromethane/methanol mixture (9∶1,V/V) subsequently. The obtained extract was then qualitatively and quantitatively analyzed by ultra high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The method provided recoveries between 56.5% and 108%, and the MLQs were in the range of 0.016~0.104 ng/g(lw). This method was applied to analyze OPFRs accumulation in crucian carp from Beijing and Guangzhou, tris n butyl phosphate (TNBP), tris(2-ethylhexyl) phosphate (TEHP), tris(2-chloroisopropyl) phosphate (TCIPP), and tris(2-chloroethyl) phosphate (TCEP) were most predominant OPFRs in fish, with concentrations in the range of 5.94~33.7 ng/g(lw), suggesting the robustness of this method in detecting OPFRs in biological tissues.
Key words:  Organophosphorus flame retardant (OPFRs)  Fish tissues  Ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS)  Solid phase extraction (SPE)  Cleanup