MSPD-HPLC同时测定枸杞中3种氨基甲酸酯类农药  

Simultaneous Determination of Three Carbamate Pesticides in Fructus lycii by MSPD-HPLC

作　　者：郝凤霞[1] 李学晴 齐瑾[1] 杨金会[1] 

机构地区：[1]宁夏大学能源化工重点实验室,银川750021

出　　处：《农药》2015年第7期525-527,共3页Agrochemicals

基　　金：宁夏大学自然科学研究基金(ZR1435)

摘　　要：[目的]建立基质固相分散净化、高效液相色谱测定枸杞中速灭威、克百威、抗蚜威的残留量。[方法]用乙腈提取,C18基质固相分散净化,甲醇-二氯甲烷(体积比1颐1)洗脱,Agilent TC-C18色谱柱,流动相为甲醇-水梯度洗脱,流速1.0 m L/min,柱温30℃,进样量20滋L。[结果]速灭威和抗蚜威质量浓度1.0~100 mg/L、克百威质量浓度0.20~20 mg/L时,线性关系良好;添加水平为10~60滋g时,速灭威、克百威、抗蚜威的加标回收率分别为95.5%、92.4%、96.3%,RSD分别为2.34%、2.28%、3.46%。[结论]该方法准确、快速、简便,符合农药残留分析要求。[Aims] A MSPD-HPLC method for simultaneous determination of metolcarb, carbofuran and pirimicarb residues in Fructus lycii was established. [Methods] The carbamate pesticide residues were extracted with acetonitrile, purified with C18 by MSPD, eluted with the mixture of dichloromethane and methanol （1：1, by vol）, determined on Agilent TC-C18 chromatographic column. The mixture of methanol and water was used as mobile phasewith the flow of 1.0 mL/min at 30 ~C, in addition, UV detection was conducted for 20 I^L of test sample. [Results] The results showed that when the contents of tsumacide and pirimicarb were in the range of 1.0-100 mg/L, and the content of carbofumn was 0.20-20 mg/L, the linear relationship of calibration curve was good. When the addition levels were 10-60 μg, the recovery rates of metolcarb, carbofuran and pirimicarb were 95.5, 92.4 and 96.3% with the RSD of 2.34, 2.28 and 3.46%, respectively. [Gonclusions] This method is accurate, rapid, convenient and qualified for pesticide residue analysis.

关 键 词：枸杞 氨基甲酸酯 基体固相分散 反相高效液相色谱 

分 类 号：S481.8[农业科学—农药学] O657.72[农业科学—植物保护]