悬浮固化液相微萃取-气相色谱联用测定水样中酰胺类除草剂残留  

Determination of Acetanilide Herbicides in Water Samples by Liquid Phase Microextraction Based on Solidification of Floating Organic Droplet Coupled with Gas Chromatography

作　　者：常青云[1] 周欣[1] 高书涛[1] 臧晓欢[1] 王春[1] 王志[1] 

机构地区：[1]河北农业大学理学院河北省生物无机化学重点实验室,保定071001

出　　处：《分析化学》2012年第4期523-528,共6页Chinese Journal of Analytical Chemistry

基　　金：河北省自然科学基金(No.B2010000657)资助项目

摘　　要：将悬浮固化液相微萃取技术(SFO-LPME)与气相色谱-电子俘获检测(GC-ECD)联用,建立了高灵敏分析水样中7种酰胺类除草剂残留的新方法。对影响萃取效率的诸因素,如萃取剂的种类及其体积、萃取时间和搅拌速率等进行了优化。在优化条件下,7种酰胺类除草剂的富集倍数达875～1546倍,以α-六六六为内标,甲草胺、乙草胺、异丙甲草胺、丁草胺和丙草胺浓度在0.50～100.0!g/L范围内,敌稗浓度在0.10～50.0!g/L范围内,杀草丹浓度在0.80～100.0!g/L范围内具有良好线性关系,线性相关系数在0.9965～0.9994之间,检出限在0.010～0.10!g/L(S/N=3)范围内。本方法已应用于河水、自来水和水库水等实际水样的分析,平均加标回收率在89.5%～112.5%之间,相对标准偏差在4.5%～7.3%之间。本方法操作简便、灵敏、富集倍数高,可满足水样中酰胺类除草剂残留的检测要求。A novel method was developed for the determination of seven acetanilide herbicides residues in water samples by liquid phase microextraction based on solidification of floating organic droplet （LPME-SFO） coupled with capillary gas chromatography with electron capture detection （GC-ECD）. Some important experimental parameters that influence the extraction efficiency, such as the type and volume of the extraction solvent, the extraction time and stirring rate, were investigated. Under the optimum conditions, as high as 875-to 1546-fold enrichment factors were achieved. Using a-benzene hexachloride as the internal standard, the linearity of the method ranged from 0.50 to 100.0μg/L for alachlor, acetochlor, metolachlor, butachlor and pretilachlor, from 0.10 to 50.0 μg/L for propanil, and from 0.80 to 100.0 μg/L for thiobencarb. The correlation coefficients （r） varied from 0. 9965 to 0. 9994 and the limits of detection were in the range between 0. 010 and 0.10 μg/L （S/N=3）. The method has been successfully applied for the determination of acetanilide herbicides residues in real water samples （tap, reservoir and river waters） with satisfactory results. The recoveries fell in the range from 89.5% to 112.5% and the relative standard deviations were between 4.5% and 7.3%.

关 键 词：气相色谱 悬浮固化液相微萃取 酰胺类除草剂 水样 

分 类 号：O661.1[理学—分析化学] X832[理学—化学] O657.71[环境科学与工程—环境工程]