固相萃取-气相色谱质谱法检测水体中典型有机磷酸酯阻燃剂  

Determination of Organophosphorus Flame Retardants in Surface Water by Solid Phase Extraction Coupled with Gas Chromatography-Mass Spectrometry

作　　者：严小菊[1] 何欢[1] 彭英[1] 王晓萌[1] 高占啟[1] 杨绍贵[1] 孙成[1] 

机构地区：[1]南京大学环境学院,污染控制与资源化研究国家重点实验室,南京210046

出　　处：《分析化学》2012年第11期1693-1697,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.2127061);江苏省环境监测科研基金项目(No.1115);江苏省研究生创新计划(No.CXZZ11-0050)资助

摘　　要：建立了固相萃取(SPE)与气相色谱质谱(GC-MS)联用测定自然水体中8种有机磷酸酯阻燃剂(OPFRs)OPFRs的分析方法。通过对GC MS条件与SPE萃取条件的优化,采用Poly-Sery PSD固相萃取小柱对水样进行富集浓缩,用4 mL乙酸乙酯洗脱,以选择离子扫描方式对目标物进行定性和定量分析,并采用内标法定量。本方法在对应OPFRs线性范围内的线性相关系数为0.9937～0.9995;检出限为0.006～0.850 ng/L;定量限为0.015～2.0 ng/L。除磷酸三(2-乙基)己基酯(TEHP)外,其它OPFRs的加标回收率为70.3%～114.3%。TEHP加标10和50 ng/L时,回收率为64.0%～69.3%;加标100 ng/L时回收率为34.3%。将本方法应用于太湖梅梁湾水体中OPFRs分析,其总浓度值为1000～2700 ng/L。Organophosphorus flame retardants（OPFRs ）,as their increasing production and consumption,are almost ubiquitous in environmental compartments.In this study,a solid phase extraction（SPE） coupled with gas chromatography-mass spectrometric（SPE-GC-MS） method was developed for the determination of 8 typical OPFRs.The targets in water samples were concentrated by Poly-Sery PSD SPE cartridge,and then eluted by 4 mL ethyl acetate.The OPFRs were qualified and quantified by GC-MS in selective ion scan monitoring method（SIM）.Good linearity was observed in the range of 2 to 200 ng/L OPFRs with correlation coefficients varing between 0.9937 and 0.9995. The limits of detection and limits of quantification ranged from 0.006 to 0.850 ng/L and 0.015 to 2.000 ng/L,respectively.Spiked recoveries of pure water and river water samples ranged from 70.3%to 114.3%,with the relative standard deviations less than 15%,except for tri（2-ethylhexyl） phosphate（TEHP）.The satisfied recovery of TEHP was achieved when the spiked concentration was less than 50 ng/L.The results showed that the SPE-GC-MS analytical method established was sensitive and accurate for the determination of OPFRs in surface water samples.Then the method was applied to analyze OPFRs in the water collected in Meiliang Bay of Taihu Lake,and it was found that the total concentration of OPFRs was ranging from 1000 to 2700 ng/L.

关 键 词：有机磷酸酯阻燃剂 固相萃取 气相色谱-质谱 水体 

分 类 号：X832[环境科学与工程—环境工程] O657.63[理学—分析化学]