液液萃取-甲醇衍生-气相色谱-质谱法测定饮用水中卤乙酸  

Determination of haloacetic acids in drinking water by gas chromatography-mass spectrometry with liquid-liquid extraction-methanol derivatization

作　　者：侯逸众[1] 胡浩军[1] 黄方取 严继东[1] 

机构地区：[1]金华市疾病预防控制中心,浙江金华321002

出　　处：《中国卫生检验杂志》2015年第16期2663-2665,共3页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立液液萃取、酸化甲醇衍生、气相色谱-质谱法测定饮用水中的3种卤乙酸(一氯乙酸Mc AA、二氯乙酸Dc AA、三氯乙酸Tc AA)的方法,为饮用水中卤乙酸检测提供参考。方法样品酸化后只加入无水硫酸钠以促使水相和有机相分离,采用含内标1,2-二溴丙烷(1,2-DBP)的甲基叔丁基醚(Mt BE)萃取卤乙酸后,用新配制的硫酸酸化甲醇溶液衍生成卤乙酸甲酯,再用气相色谱-质谱仪测定,内标法定量。结果 3种卤乙酸在5.0μg/L^100μg/L时保持良好线性关系,检出限(3S/N)为0.06μg/L^0.21μg/L,加标回收率为78.8%~103.9%,相对标准偏差(RSD)为4.8%~5.1%(n=6)。结论该方法操作简便、试剂消耗少、回收率稳定、结果准确,适合饮用水中3种卤乙酸的检测。Objective To establish a method for the determination of three haloacetic acids（ Mc AA,Dc AA,Tc AA） in drinking water by gas chromatography- mass spectrometry with liquid- liquid extraction and methanol derivatization to provide reference for the detection of haloacetic acid in drinking water. Methods After acidified,only anhydrous Na2SO4 was added in the sample to separate organic and water phase,the haloacetic acids was abstracted by Mt BE included 1,2- DBP as internal standard,derivatizated by freshly prepared acidic methanol,then analyzed by gas chromatography- mass spectrometry,quantified with internal calibration curve. Results A good linear relationship of three haloacetic acids was maintained in the range of 5. 0 μg / L-100 μg / L. The detection limits（ 3S / N） were 0. 06 μg / L- 0. 21 μg / L,the additive recovery rates were 78. 8%- 103. 9%,and relative standard deviation（ RSD） was 4. 8%- 5. 1%（ n = 6）. Conclusion The method is simple with few reagent consumption,stable recovery,accurate and suitable for the determination of three haloacetic acids in drinking water.

关 键 词：液液萃取 甲醇衍生 气相色谱-质谱法 饮用水 卤乙酸 

分 类 号：O657.63[理学—分析化学]