全自动固相萃取-气相色谱法检测水中的2,4-滴  

Determination of 2,4-dichlorophenoxyacetic acid by automatic solid phase extraction-gas chromatography in drinking water

作　　者：张念华[1] 王军淋[1] 应英[1] 冯靓[1] 赵永信[1] 沈向红[1] 

机构地区：[1]浙江省疾病预防控制中心,浙江杭州310051

出　　处：《中国卫生检验杂志》2016年第1期26-27,共2页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立全自动固相萃取-气相色谱法检测水中2,4-滴的方法。方法取1 L水样,加浓硫酸使水样p H<1,通过全自动固相萃取仪以15 ml/min将水样过HLB固相萃取柱(Waters,500 mg,Oasis)萃取,用0.1 mol/L Na OH甲醇溶液洗脱HLB固相萃取柱上吸附的待测物,氮气吹干,用三氟化硼甲醇溶液衍生后,加纯水用正己烷提取,经气相色谱仪进行检测。结果水样中2,4-滴的浓度为0μg/ml^1.0μg/ml时,与峰面积呈良好的线性关系,相关系数(r)均>0.999,最低检出浓度为0.01μg/L(1 L水样)。0.1μg/L加标水样组2,4-滴的回收率为110.0%,相对标准偏差(RSD)为6.9%;1.0μg/L加标水样组2,4-滴的回收率为106.0%,RSD为2.3%。结论该方法简便、准确,适用于水中2,4-滴的检测。Objective To establish a method for the determination of 2,4 -dichlorophenoxyacetic acid（2,4 -D） by automatic solid phase extraction - gas chromatography （ SPE - GC ） in drinking water. Methods i L of drinking water were added into sulfuric acid to make pH 〈 1, by automatic solid - phase extraction, water samples flew through solid phase extraction column at 15 ml/min （Waters, 500 mg, Oasis） for extraction, to elute analyte adsorpted on the HLB SPE column with 0.1 mol/L NaOH methanol, then dried with nitrogen, and after derivatized with three boron trifluoride methanol solution, adding water to extract with hexane, and detected with gas chromatography. Results The experimental results indicated that the coefficients efficiency of 2,4 -D 〉0. 999 with the concentration of 2,4 -D among 0 μg/ml - 1.0μg/ml, and showed good linearity. The limit concentration of 2,4 - D was 0.01 μg/L （ 1 L water sample）. The recovery rate of spiked water sample group with 0.1μg/L was 110.0% , with the relative standard deviations of 6.9% ; and the recovery rate of spiked water sample group with 1.0 μg/L was 106.0%, with the relative standard deviations of 2.3%. Conclusion The method is a quick and accurate for the detection of 2,4 - D in drinking water.

关 键 词：2 4-滴 气相色谱仪 生活饮用水 固相萃取 三氟化硼 

分 类 号：O657.71[理学—分析化学]