气相色谱法结合悬浮固化有机滴液液相微萃取测定水中有机氯农药
[Determination of organochlorine pesticides in water using solidification of floating organic drop liquid phase microextraction by gas chromatography].
作者信息
Li Xiao-Xia, Wang Yu, Yong Li, Zou Xiao-Li, Zhao Yue-Ping
出版信息
Sichuan Da Xue Xue Bao Yi Xue Ban. 2014 Mar;45(2):324-7.
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 NaCI. The OCPs were extracted at 55 degrees C for 10 mm and determined with GC-ECD.
RESULTS
A good linearity (correlation coefficients > or = 0.996) was obtained for eight target compounds from 5 ng/I. 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 hatch analyses of eight organic chlorine pesticides in water samples.
目的
建立一种采用固化漂浮有机滴液相微萃取（SFO-LPME）结合气相色谱-电子捕获检测器（GC-ECD）同时测定水样中8种有机氯农药（OCPs）的新方法。
方法
以正十六烷为萃取剂，将水样pH调至6.0，加入15.0 g/100 mL氯化钠提高离子强度，以此确定SFO-LPME的实验条件。在55℃下萃取10分钟后，用GC-ECD对OCPs进行测定。
结果
8种目标化合物在5 ng/L至100 ng/L范围内具有良好的线性关系（相关系数≥0.996）。方法检出限为0.24 ng/L至0.78 ng/L。对河水、自来水和农田水样品的检测结果令人满意，平均回收率为76.0% - 106.0%，相对标准偏差为3.24% - 11.60%。
结论
该方法快速、简便、灵敏，适用于水样中8种有机氯农药的痕量分析。
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