摘要
目的:建立液液萃取-顶空气相色谱法快速测定饮用水中九种卤乙酸的方法。方法:样品中的卤乙酸与硫酸二甲酯进行衍生反应,在正戊烷-水两相系统中,以四丁基硫酸氢铵作为相转移催化剂发生质量转移,卤乙酸甲酯和有机相在顶空系统中达到汽液平衡,经CP-S il8毛细管色谱柱分离,ECD内标法定量。结果:九种卤乙酸在0.1μg/L^300μg/L范围内具有良好线性关系,相关系数>0.99,检出限在0.05μg/L^0.61μg/L。在1μg/L、30μg/L、100μg/L三个水平添加时,各被测物的回收率在88.4%~105%,相对标准偏差在4.6%~3.9%。结论:该法操作简单、快速、准确度和灵敏度高,是一种饮用水中卤乙酸测定的快速分析方法。
Objective：A method was developed for rapid determination of nine haloacetic acids in drinking waters by liquid-liquid extraction and HS-GC.Methods： Derivatisation of haloacetic acids with dimethylsulphate was completed.Mass transfer was accomplished in n-pentane-water two-phase system with tetrabutylammonium hydrogen sulphate as phase transfer catalyst.Vapor-liquid equilibrium of the methyl ester derivatives and the organic phase were completed by static headspace technique.The separation was performed on CP-Sil8 capillarity column and detected by ECD.Results： Calibration curves for the nine haloacetic acids were linear within the range of 0.1 μg/L^300 μg/L.The correlation coefficients were higher than 0.99.The limits of detection were between 0.05 μg/L^0.61 μg/L.The extraction recoveries ranged from 88.4% to 105% at three spiked levels of 1 μg/L,30 μg/L,100 μg/L for each haloacetic acid,and the RSDs ranged from 4.6% to 3.9%.Conclusion： The proposed method is simple,rapid,accurate,sensitive and suitable for the determination of haloacetic acids in drinking waters.
出处
《中国卫生检验杂志》
CAS
2011年第6期1338-1340,共3页
Chinese Journal of Health Laboratory Technology
基金
上海市宝山区科委2009年立项项目(2009-E-30)
