固相萃取—气相色谱—质谱测定再生水中邻苯二甲酸酯类物质

探讨了一种再生水中邻苯二甲酸酯类物质的测定方法——固相萃取—气相色谱—质谱,检测了相关再生水标准中涉及的邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)两类物质。在质量浓度为20～1 000μg/L时,两类物质的回归方程的相关系数均大于0.999,检出限分别是0.060、0.002μg/L,DBP、DEHP的相对标准偏差分别为4.1%～7.4%、5.1%～6.1%。利用固相萃取技术进行预处理,平均加标回收率为96.6%、89.6%。检测了北京市4座再生水厂出水中DBP和DEHP含量,其中,DBP在1.74～5.59μg/L,低于《城市污水再生利用景观环境用水水质》(GB/T 18921—2002)规定的限值(不超过0.1mg/L),但高于《城市污水再生利用地下水回灌水质》(GB/T 19772—2005)规定的限值(不超过3μg/L);DEHP在0.42～4.93μg/L,满足GB/T 19772—2005要求(不超过8μg/L)。

Determination of phthalates in reclaimed water by SPE-GC-MS

A method of solid phase extraction combined with chromatography-mass spectrometry(GC-MS) was established for determination of phthalate in reclaimed water.In this paper,the Dibutyl phthalate(DBP) and Di(2-ethylhexyl)phthalate(DEHP) that mentioned in some standards of reclaimed water was selected as typical phthalate to be detected by the established method.In the range of mass concentration 20-1 000 μg/L,the correlation coefficients of regression equations were above 0.999.The detection limits of DBP and DEHP were 0.060,0.002 μg/L.The RSD of DBP and DEHP were 4.1%-7.4% and 5.1%-6.1%.The average recoveries were 96.6%,89.6% by solid phase extraction(SPE) in the pretreatment.The contents of DBP and DEHP in effluents of four reclaimed water plants in Beijing were detected.The DBP concentration was among 1.74-5.59 μg/L,which below the limits value(0.1 mg/L) for scenic environment use(GB/T 18921-2002) but exceed the limits for groundwater recharge(3 μg/L).DEHP was in range of 0.42-4.93 μg/L,which met the demand of GB/T 19772-2005(below 8 μg/L).