多壁碳纳米管做吸附剂富集水中有机磷农药残留  

Enrichment of Organophosphorus Pesticides with Multi-walled Carbon Nanotubes as Efficient Solid-phase Extraction Material from Water

作　　者：袁丁[1] 孙艳红[1] 贾艳霞[1] 孙大江 塔秀成[1] 赵海香[1,2] 

机构地区：[1]河北北方学院农林科技学院,河北张家口075000 [2]北京锦绣大地技术检测分析中心有限公司,北京100049

出　　处：《河北北方学院学报（自然科学版）》2011年第2期59-64,共6页Journal of Hebei North University:Natural Science Edition

基　　金：北京市海淀区科委企业博士后科研专项(k2008198)

摘　　要：目的研究多壁碳纳米管（MWCNTs）做固相萃取吸附剂对水中的16种有机磷农药残留的吸附富集效果.方法 MWCNTs SPE柱采用水相净化体系,有机磷农药采用双柱双检测器GC/FPD法测定.结果优化的净化条件为：水样采用HAc-NaAc缓冲溶液调节pH=5.0,MWCNTs SPE柱用5 mL甲醇和5 mLHAc-NaAc缓冲溶液（pH 5.0）活化,处理好的水样通过MWCNTs SPE柱富集有机磷农药,真空抽干10 min除水,10 mL二氯甲烷洗脱有机磷农药,洗脱液静置10 min分层,除去水层,有机层在氮气下吹干,残余物用丙酮定容至2 mL,进样GC/FPD分析测定.0.25 g MWCNTs（长度为515μm,直径为2040 nm）处理水样体积为50100 mL.在此净化条件下,水样中添加16种有机磷农药的测定结果表明：甲胺磷在MWC-NTs SPE柱上存在穿漏现象,9种农药（甲拌磷、二嗪农、久效磷、乐果、甲基嘧啶磷、水胺硫磷、喹硫磷、杀扑磷和亚胺硫磷）的回收率大于75%,RSD小于9%;6种农药（敌百虫、甲基毒死蜱、毒死蜱、倍硫磷、乙硫磷和伏杀硫磷）的回收率小于64%.结论研究表明：MWCNTs SPE柱可以有效地从水样中富集净化部分有机磷农药,是一种具有较好应用前景的去除水中有机磷农药的吸附材料.Objective The enriching effect of 16 rganophosphorus pesticides with multi-walled carbon nanotubes as efficient solid-phase extraction adsorbent from water was studied.Methods The determination and quantitation of 16 organophosphorus pesticides in water sample were carried out by gas chromatography-flame photometric detector（GC/FPD）.The GC/FPD method used two columns（HP-50 and HP-1） and two FPD detectors.Results The clean-up conditions were optimized.The pH of water sample was adjusted 5.0 with HAc-NaAc buffer solution.MWCNTs SPE cartridge was pre-washed with 5 mL methanol and 5 mL HAc-NaAc buffer solution（pH 5.0）.The water sample was transferred to the SPE cartridge.The cartridge was dried for 10 min under vacuum.The rganophosphorus pesticides were eluted with 10 mL dichlormethane into a graduated 10 mL centrifuge tube with ground-glass stopper and stand for 10 min.The upper water layer was transferred and threw away.The organic layer was dried under nitrogen.The remainder was re-dissolved with 2 mL acetone and determined by GC/FPD.The experimental results showed the methamidaphos was broken through,the recoveries of 9 organophosphorus pesticides（including phorate,diazinon,monocrotophos,dimethoate,pirimiphos-methyl ester,isocarbophos,quintiofos,methidathion,phthalophos） in water sample were over 75% and RSD were under 9%,and the recoveries of 6 organophosphorus pesticides（including trichlorphon,chlorpyrifos-methyl,chlorpyrifos,fenthion,ethion,phosalone） were under 64%.Conclusion This study indicates the MWCNTs SPE cartridge was an efficient clean-up and enrichment method to water and it can remove the contamination of the rganophosphorus pesticides in water.

关 键 词：多壁碳纳米管(MWCNTs) 有机磷农药 水 气相色谱-火焰光度法(GC/FPD) 

分 类 号：O658.1[理学—分析化学]