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建立了磁固相萃取结合气相色谱/质谱联用测定环境水中邻苯二甲酸二丁酯(DBP)和邻苯二甲酸二(2-乙基己基)酯(DEHP)的方法。萃取的最佳条件为:在100 mL水样中加入20 mg磁性Fe3O4@SiO2-C18微球,振摇萃取10 min后,用2.0 mL二氯甲烷解析5 min。在优化条件下,DBP和DEHP的检出限分别为0.1μg/L和0.3μg/L(S/N=3),线性范围为1.0~100μg/L,线性相关系数分别为0.9992和0.9990。方法应用于河水、湖水和井水样的分析,DBP的加标回收率为83.2%~103%,相对标准偏差小于6.8%,DEHP的加标回收率为82.2%~107%,相对标准偏差小于7.9%。
A method for the determination of dibutyl phthalate (DBP) and di-2-ethylhexyl phthalate (DEHP) in environmental water by magnetic solid-phase extraction coupled with gas chromatography / mass spectrometry was established. The optimal conditions for extraction were as follows: 20 mg magnetic Fe3O4 @ SiO2-C18 microspheres were added to 100 mL water sample, and the solution was shaken for 10 min and then resolved with 2.0 mL dichloromethane for 5 min. Under optimized conditions, the detection limits of DBP and DEHP were 0.1μg / L and 0.3μg / L respectively (S / N = 3). The linear range was 1.0-100μg / L and the linear correlation coefficients were 0.9992 and 0.9990 respectively. The method was applied to the analysis of river water, lake water and well water samples. The spiked recoveries of DBP were 83.2% -103% with the relative standard deviations less than 6.8%. The spiked recoveries of DEHP ranged from 82.2% to 107% with relative standard deviations 7.9%.