甲基化衍生-高效液相色谱法检测代森锰锌在花生中的残留量  

Determination of Residual Mancozeb in Peanuts Sample by Methylation Derivation-High Performance Liquid Chromatography

作　　者：马婧玮[1] 董姝君[1] 游文宇[1] 张敬平[2] 钮伟民[2] 潘灿平[1] 

机构地区：[1]中国农业大学理学院,北京100094 [2]无锡市疾病预防控制中心,江苏无锡214023

出　　处：《农药学学报》2007年第3期297-300,共4页Chinese Journal of Pesticide Science

基　　金：卫生部科研基金课题(WKJ2006-2-10).

摘　　要：建立了简单、快速测定花生中杀菌剂代森锰锌的残留检测方法。花生样品用L-半胱氨酸盐酸盐和EDTA-2Na的混合溶液振荡提取,在pH=6.5～8.5时,用0.05mol/L的碘甲烷与三氯甲烷-正己烷(3∶1,体积比)的混合溶液进行甲基化反应。有机层经浓缩后,用乙腈定容,采用高效液相色谱仪在272nm处进行检测。色谱柱为AgilentTC-C18,流动相为乙腈-水(50∶50,体积比),以1.0mL/min的流速等梯度洗脱。结果表明,代森锰锌的添加浓度在0.05～2.00mg/kg范围内,平均回收率为76.1%～86.2%,变异系数分别为0.7%～10.2%,均在农药残留测定所允许的范围内。该方法的最低检出限(LOD)为0.02mg/kg,最低检测浓度(LOQ)为0.05mg/kg。A simple and rapid method was developed for the residue determination of mancozeb. Mancozeb in peanuts sample was extracted by the mixed solution of L-cysteine and EDTA-2Na. After that,0.05 mol/L methyl iodide in trichloromethane-hexane（3：1 , V/V） was added into the extracts. Then the organic layer was took out and concentrated and dissolved in acetonitrile for HPLC by A272 nm. In the method, mancozeb was analyzed on a Agilent TC-C18column, using a mixture of acetonitrile-water （50： 50, V/V） as the mobile phase at the ambient temperature with a flow rate of 1.0 mL/min. The average recoveries of mancozeb in peanuts at 0.05,0.5 and 2.0 mg/kg fortification level were 76.1% - 86.2%, and the coefficient of variation were 0.7%- 10.2%. The limit of detection （LOD） was 0.02 mg/kg,and the limit of quantitation （LOQ） was 0.05 mg/kg.

关 键 词：甲基化 代森锰锌 花生 高效液相色谱 农药残留 

分 类 号：O657.72[理学—分析化学] X592[理学—化学]