液液萃取气相色谱法同时测定饮用水中的11种卤代酸  

Determination of eleven halogenated acids in drinking water by liquid-liquid extraction and gas chromatography with electron capture detector

作　　者：肖惠贞[1] 徐小作[1] 陆碧茹[1] 李静[1] 

机构地区：[1]深圳市宝安区疾病预防控制中心,广东深圳518101

出　　处：《中国卫生检验杂志》2015年第9期1332-1335,1356,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立液液萃取气相色谱法测定饮用水和水源水中9种卤代乙酸和2种除草剂共11种卤代酸的方法。方法采用甲基叔丁基醚为萃取溶剂,1,2-二溴丙烷为内标溶剂,在酸性条件下加氯化钠萃取水中的卤代酸。取甲基叔丁基醚层加入硫酸酸化的甲醇溶液,在酸性条件下,50℃酯化反应1 h,采用气相色谱法进行检测。结果方法的线性范围为2.0μg/L^100.0μg/L,线性相关系数为0.999 0~0.999 9,检出限为0.09μg/L^0.65μg/L;在2.0μg/L、20.0μg/L、100.0μg/L 3个添加水平范围内的平均加标回收率分别为83.5%~106.2%、89.0%~104.1%、87.1%~99.3%;相对标准偏差(RSD)为0.36%~6.23%。结论该方法在测定饮用水和水源水中的11种卤代酸时,具有操作简单、干扰少、快速、准确可靠等特点,适合用于居民生活饮用水和水源水的日常监控。Objective A method was established for rapid determination of the eleven halogenated acids（ nine haloacetic acids and two herbicides） in drinking waters by liquid - liquid extraction and gas chromatography with electron capture detector. Methods Methyl tert - butyl ether and 1,2 - dibromide propane were used as extraction solvent and an internal standard, re- spectively. Under acidic conditions, the esterification reaction was conducted for 1 h at 50 ℃ in acidic conditions. The obtained product was detected by gas chromatography. Results The calibration curves of eleven halogenated acids showed good linearity in the range of 2.0 μg/L - 100.0 μg/L with the correlation coefficient in the range of 0. 999 0 -0. 999 9. The detection limit of the method was from 0.09μg/L to 0.65 μg/L. The spiked at three levels ranged 83.5% - 106.2% （2.0μg/L）, 89.0% - 104.1%（20.0 μg/L） and87.1% -99.3%（100.0 μg/L）, andRSDwasO. 36% -6.23%. Conclusion The method for determination of eleven halogenated acids in drinking water and source water by gas chromatography with electron capture detec- tor was of operation convenience, less interference from impurities and good accuracy, which could used in monitoring quality of drinking water and source water.

关 键 词：卤代酸 除草剂 液液萃取 气相色谱法 饮用水 

分 类 号：O657.71[理学—分析化学]