悬浮固化液相微萃取-气相色谱法测定水中有机氯农药

李晓霞; 王宇; 雍莉等

悬浮固化液相微萃取-气相色谱法测定水中有机氯农药

Determination of Organochlorine Pesticides in Water using Solidification of Floating Organic Drop Liquid Phase

摘要

摘要: 目的建立悬浮固化液相微萃取技术结合气相色谱-电子捕获检测（GC-ECD）同时测定水中8种常见有机氯农药的新方法。方法详细考察悬浮固化液相微萃取的实验条件，以正十六烷为萃取剂，在pH 6.0和15.0 g/100 mL NaCl浓度条件下，55 ℃温浴10 min进行有机氯农药的微萃取，萃取液进气相色谱-电子捕获检测器分离分析。结果在优化条件下，8种农药在5～100 ng/L浓度范围线性良好，相关系数r≥0.996，方法检出限为0.24～0.78 ng/L。将所建立的方法用于自来水、河水和农田池塘水的检测，取得了较为满意的结果，平均回收率在76.0%~106.0%，方法精密度为3.24%~11.60%。结论方法快速灵敏，操作简单，绿色环保，适用于水中8种常见有机氯的批量分析。

Abstract: 【Abstract】 Objective To develop a new method for simultaneous determination of eight organochlorine pesticides (OCPs) in water samples using solidification floating organic drop liquid-phase microextraction (SFO-LPME) combined with gas chromatography-electronic capture detector (GC-ECD). Methods The experimental conditions of SFO-LPME were determined with n-Hexadecane as extractant, water samples adjusted to pH 6.0, inonic strength increased by adding 15.0 g/100 mL NaCl. The OCPs were extracted at 55℃ for 10 min and determined with GC-ECD. Results A good linearity (correlation coefficients ≥0.996) was obtained for eight target compounds from 5 ng/L to 100 ng/L. The method detection limits ranged from 0.24 ng/L to 0.78 ng/L. Satisfactory results were achieved with samples of river water, piped water and farmland water, with an average recovery of 76.0%-106.0% and \RSD of 3.24%-11.60%. Conclusion The proposed method is rapid, simple and sensitive. It is suitable for batch analyses of eight organic chlorine pesticides in water samples.

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