超声辅助-高分子表面活性剂增强乳化微萃取测定水中多种痕量芳香胺

Application of an Ultrasound-assisted Polymer Surfactantenhanced Emulsification Microextraction for Determination of Aromatic Amines in Water Sample

建立了超声辅助-高分子表面活性剂增强乳化微萃取测定水中痕量2,4,5-三甲基苯胺、3,3＇-二氯联苯胺以及4-氨基偶氮苯等8种芳香胺的测试方法。对分散液相微萃取的条件进行了优化,实验得到的最佳萃取条件为：萃取剂为二氯乙烷,萃取剂的体积为150μL,活性剂为海藻酸钠,其浓度为0.20 g/L,超声时间为1 min,pH=7.0,盐浓度为3%。在优化实验条件下,测得3,3＇-二氯联苯胺的线性范围为0.1-200μg/L,2,4,5-三甲基苯胺等5种芳香胺为0.3-200μg/L,4-氨基偶氮苯等2种芳香胺为0.5-200μg/L,相关系数为0.9961-0.9997,检出限为0.08-0.3μg/L,日内精度RSD〈10.3%,日间精度RSD〈11.9%。实际水样加标实验表明,本方法可用于不同基质水样中的芳香胺的测定。与常规活性剂增强的超声辅助分散乳化微萃取相比,本方法使用的活性剂为水溶性高分子表面活性剂,无污染且不溶于萃取试剂,可扩展分析仪器的范围；与其它固相萃取方法相比,本方法萃取时间更短,操作更简单,费用更低。

A simple and efficient method, based on ultrasound-assisted polymer surfactant-enhanced emulsification microextraction followed by gas chromatography-mass spectrometry（ GC-MS） , was developed for the determination of eight aromatic amines （ AAs ） in aqueous sample. The main parameters affecting the performance of the purposed method were optimized, and the optimized conditions were obtained as follows：150 μL of extractive solvent （ dichloroethane ） , polymer surfactant （ sodium alginate ） concentraction of 0. 20 g/L, pH 7. 0, salt addition of 3%, and ultrasound time of 1 min. Under the optimal conditions, the linear ranges of the method were 0. 1-200 μg/L for 3,3’-dichlorobenzidine, 0. 3-200 μg/L for 2,4,5-trimethylaniline, 4-chloro-o-toluidine, 3,3’-dimethyl-4,4’-diaminodiphenylmethane, 3,3’-dimethylbenzidine and 4 , 4’-methylene-bis-（ 2-chloroaniline ） , 0 . 5-200 μg/L for 4-aminoazobenzene and 3 , 3’-dimethoxy-benzidine. The correlation coefficients （R2） and the detection limits were 0. 9961-0. 9997 μg/L and 0. 08-0. 3 μg/L, respectively. The intra- and inter-day RSDs were less than 10. 6% and 11. 0%. The purposed method could be applied to the analysis of AAs in water sample collected from tap water and river water. In comparison with the common SA-USAEME, conventional surfactant was replaced with water-soluble polymer surfactant to solve the problems of potential pollution, and the polymer surfactant was natural and insoluble in extractive solvent. Compared with other solid-phase extractions, the proposed method had the advantages such as simple operation and low cost.