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固相萃取/气相色谱-质谱联用技术快速测定水中有机磷酸酯阻燃剂与增塑剂

固相萃取/气相色谱-质谱联用技术快速测定水中有机磷酸酯阻燃剂与增塑剂

ISSN:1004-4957
2013年第32卷第4期
研究简报
何丽雄1, 2, 3, 4;曹曙霞1, 2, 3, 4;曾祥英1, 2, 3, 4;于志强1, 2, 3, 4;盛国英1, 2, 3, 4;傅家谟1, 2, 3, 4 HE Li-xiong[1] , CAO Shu-xia[1] , ZENG Xiang-ying[2] , YU Zhi-qiang[2] , SHENG Guo-ying[2] , FU Jia-mo[2]

利用固相萃取(SPE)技术快速富集表层水中的有机磷酸酯类化合物,并结合气相色谱-质谱联用(GC-MS)分析技术,建立了快速测定水中7种常用磷酸酯类化合物的方法。考察了SPE小柱和洗脱溶剂的影响,最终选择OasisHLB(200mg)作为固相萃取小柱,乙酸乙酯为洗脱溶剂。对实验室纯水加标实验、实际环境水样加标实验的研究表明,该方法具有良好的回收率和重现性。在实验室纯水加标实验中,目标化合物的回收率为(74±12)%~(118±3.0)%;在实际环境水样加标实验中,目标化合物的回收率为(62±6.9)%~(121±2.2)%。仪器检出限为4~15μg/L。采用该方法考察了珠江表层水、东江表层水和广州某污水处理厂出水中7种常用磷酸酯类化合物的分布现状和含量水平。

Organophosphate esters(OPs) are widely used as flame retardants and plasticizers.A rapid method for the determination of seven OPs in water was developed based on enrichment via solid-phase extraction(SPE) and determination by gas chromatography-mass spectrometry(GC-MS).The SPE cartridge and elution solvent were optimized,consequently,Oasis HLB(200 mg) cartridge was chose as extractive cartridge and ethyl acetate was selected as elution solvent.Under the optimized conditions,the developed method was verified using the blank spiked and the matrix spiked,and acceptable recoveries and good reproducibilities were achieved,with recoveries of(74±12)%-(118±3.0)% and(62±6.9)%-(121±2.2)% for the blank spiked and the matrix spiked,respectively.The instrumental detection limits(IDLs) for specific chemicals were in the range of 4-15 μg/L.The established method was proved to be efficient via measurement on the occurrence and concentrations of the 7 OPs in two surface water samples collected from the Pearl River,and effluent from a waste water treatment plant (WWTP) in Guangzhou.

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ISSN:1004-4957
2013年第32卷第4期
研究简报

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