深共晶溶剂液液微萃取测定痕量苯系物的研究

Hydrophobic deep eutectic solvent-vortex assisted liquid-liquid microextraction for sensitively detecting trace benzene in water samples

本文以新型的疏水型深共晶溶剂(DES)作为萃取剂,建立了漩涡辅助液液微萃取-气相色谱法(VALLME-GC)的新方法,并应用于环境水样中6种痕量苯系物(苯、甲苯、乙苯、对二甲苯、间二甲苯、邻二甲苯)的高灵敏度分析检测.实验还对DES的单体配比、萃取剂的用量、旋涡时间等影响因素进行了探讨和优化,结果表明,本法最佳条件为:DES单体摩尔比1∶1,萃取剂用量1.00 mL,旋涡时间3.00 min.在最佳条件下,本法测定6种苯系物的线性范围0.500~500μg/L,相关系数r^(2)≥0.997,检出限(LOD)为1.80μg/L,相对标准偏差(RSD)为0.12%~7.73%.最后,本法成功应用于实际环境水样(福建省九龙江水,漳州市学校内湖湖水)6种痕量苯系物的分析检测,加标回收率为78.9%~93.7%.

In this work,we prepared a hydrophobic deep eutectic solvent(DES),which was used as extractant for vortex assisted liquid-liquid microextraction-gas chromatography(VALLME-GC)to the analysis of benzene,toluene,ethylbenzene,o-xylenes,m-xylenes and p-xylenes(BTEX)in environmental water samples.The parameters,mole ratio of DES,amount of extractant,and vortex time of DES,were systematically optimized.The best extraction conditions were obtained:molar ratio of DES 1∶1,amount of extractant 1 mL,and extraction time 3 min.Under these conditions,a good linearity ranges were between the range of 0.500 and 500μg/L,the low limit of detections(LODs)was 1.80μg/L,the relative standard deviation(RSD%)were obtained in the range from 0.12%to 7.73%.Finally,the proposed method was successfully used to analysize BTEX in real water samples,and the recoveries from spiked samples ranged from 78.9%~93.7%.