固相萃取-加压毛细管电色谱法测定水体中8种农药残留  被引量:12

Determination of Eight Pesticide Residues in Water by Solid Phase Extraction-Pressurized Capillary Electrochromatography

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作  者:山梅 李静[1,2] 茹鑫[1,2] 郑署 王晓曦[1] 闫超[1] 

机构地区:[1]上海交通大学药学院,上海200240 [2]上海通微分析技术有限公司,上海201203

出  处:《分析科学学报》2015年第4期445-449,共5页Journal of Analytical Science

基  金:国家自然科学基金(No.21175092;21105064);国家重大科学仪器设备开发项目(No.2011YQ150072;2011YQ15007204;2011YQ15007210);上海市自然科学基金(No.12ZR1313600);苏州市科技支撑计划(No.SG201214);国家科技型中小企业创新基金(No.12C26213202212)

摘  要:采用固相萃取-反相加压毛细管电色谱-紫外检测技术,建立了水体中乐果、敌敌畏、克百威、甲萘威、莠去津、甲基对硫磷、马拉硫磷、百菌清8种农药残留的同时检测方法。在最佳条件下,8种目标农药的线性范围分别为:3.4~100μg/mL、8.1~120μg/mL、1.2~50μg/mL、0.2~50μg/mL、0.1~50μg/mL、3.7~100μg/mL/。11.2~150μg/mL,2.1~100μg/mL,相关系数为0.9961~0.9997;检出限(S/N=3)在0.03~3.7μg/mL之间,加标回收率在71.09/6~114.1%范围,相对标准偏差(RSD)为1.1%~9.8%。该方法简单、可靠、适用于水中多种农药残留的同时分析测定。By combining solid phase extraction,pressurized capillary electrochromatography(pCEC)equipped with ultra-violet detector was used to determine eight pesticide residues including dimethoate,dichiorvos,carbofuran,carbaryl,atrazine,methyl parathion and malathion and chlorothalonil in water via a reversed-phase C18 column.Under the optimal separation condition,the linear ranges of the eight pesticides were 3.4-100μg/mL,8.1-120μg/mL,1.2-50μg/mL,0.2-50μg/mL,0.1-50μg/mL,3.7-100μg/mL,11.2-150μg/mL and 2.1-100μg/mL,repectively.Correlation coefficients were between0.9961 and 0.9997,and limits of detection were between 0.03 and 3.7μg/mL.Average recoveries between71.0% and 114.1%and relative standard deviations between 1.1%and 9.8% were obtained.It is demonstrated that the pCEC-UV can be used for the determination of pesticides in water sample.

关 键 词:加压毛细管电色谱 紫外检测 固相萃取 农药残留 毛细管电色谱柱 

分 类 号:O657.8[理学—分析化学]

 

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