超快速高效液相色谱法测定普通白菜中16种氨基甲酸酯类农药残留  

Simultaneous Determination of Sixteen Carbamate Pesticide Residues in Cabbage with Ultra Fast High Performance Liquid Chromatography

作　　者：万凯[1] 刘家容[1] 陆莹[1] 杨炜君[1] 

机构地区：[1]广东省农业科学院农产品公共监测中心/农业部农产品质量安全风险评估实验室,广东广州510640

出　　处：《热带农业科学》2015年第7期57-62,68,共7页Chinese Journal of Tropical Agriculture

基　　金：农业部公益性行业(农业)科研专项(No.201303088);广东省专业镇中小微企业农产品质量安全检测服务平台建设(No.2013B091604005)

摘　　要：研究应用超快速高效液相色谱仪柱后衍生荧光检测器同时测定普通白菜中16种氨基甲酸酯类农药残留。对流动相组成、波长选择、梯度洗脱等条件进行比较研究,建立了样品经乙腈提取, SPE-NH2固相萃取柱净化,液相色谱柱后衍生分离,荧光检测（λex＝339 nm,λem＝445 nm）测定,外标法定量的检测方法。研究表明：基于液相色谱荧光检测条件,16种农药残留在0.025～1.0 mg/L浓度范围内线性关系良好；检出限0.002～0.010 mg/L；平均加标回收率73.0%～103.0%,相对标准偏差（RSD）1.5%～8.8%。该研究确定的方法具有检测范围广、快速、灵敏、准确、重现性好、易推广等特点。The study aims to establish a method for simultaneous determination of 16 pesticide residues which are Aldicarb-sulfoxide, Aldicarb-sulfone, oxamyl, Methomyl, Hydroxycarbofuran, toxic metabolite, Aldicarb, Tsumacide, Propoxu, Carbofuran, Carbary, XMC, Isoprocarb, Fenobcarb, Methiocarb, Thiodicarb, Promecarb in cabbage by ultra fast high performance liquid chromatograph column derivative fluorescence detector. Meanwhile, the study also aims to the comparison of the composition of mobile phase, wavelength selection, gradient elution at different levels. Samples were ectracted by acetonitrile and purified by SPE-NH2-dispersive solid phase extraction. The colleted solution was analyzed by UFLC-FLD with post-column derivation and quantified by external standard method. The wavelengths were set at 339 nm and 445 nm. The result indicates that the calibration curves of 16 pesticides showed good linear relationship in the concentration of 0.025~1.0 mg/L with correlation coefficients greater than 0.999. The detection limits ranged from 0.002~0.010 mg/L. The recoveries ranged from 73.0%~103.0% with the relative standard deviation （RSD） range of 1.5%~8.8% . The method is characterized as wide range of detection, rapid, sensitive, accurate, repeatable and ease of deployment.

关 键 词：超快速高效液相色谱法 荧光检测 氨基甲酸酯 农药残留 

分 类 号：S481.8[农业科学—农药学]