液相色谱法同时测定火锅底料中11种氨基甲酸酯类农药残留  

Simultaneous Determination of 11 Carbamate Pesticide Residues in Hotpot Condiments by High Performance Liquid Chromatography

作　　者：唐柏彬[1,2] 郗存显[2] 邹芸 王国民[2] 李贤良[2] 张雷[2] 陈冬东[4] 张进忠[1] 

机构地区：[1]西南大学资源环境学院,三峡库区生态环境教育部重点实验室,重庆400715 [2]重庆出入境检验检疫局,重庆市进出口食品安全工程技术研究中心,重庆400020 [3]重庆市市政环卫监测中心,重庆401121 [4]中国检验检疫科学研究院,北京100123

出　　处：《食品科学》2013年第10期191-196,共6页Food Science

基　　金：国家公益性行业(质检)科研专项(201010073);国家质检总局科技计划项目(2009IK185);重庆市科技攻关项目(CSTC2009CB1012)

摘　　要：建立同时测定火锅底料中11种氨基甲酸酯类农药的高效液相色谱方法。样品经层析硅胶固相分散、乙腈提取,凝胶渗透色谱和氨基固相萃取柱净化后,C18柱分离,柱后衍生和荧光检测。在0.01～0.50mg/L的范围内,11种氨基甲酸酯类农药的色谱峰面积与其质量浓度之间的线性关系良好,相关系数均大于0.999,检测限(RSN=3)为0.3～1.2 g/kg,定量限(RSN=10)均为10 g/kg。当添加量水平为10、20 g/kg和50 g/kg时,11种氨基甲酸酯类农药的加标回收率为76.2%～95.5%,相对标准偏差(n=6)为3.4%～11.9%。本方法灵敏、可靠,能够满足火锅底料中11种氨基甲酸酯类农药残留检测的需要。A simultaneous method has been developed for the determination of 11 carbamate pesticide residues in hotpot condiments.Samples were dispersed by silica gel chromatography and extracted with acetonitrile,purified by gel permeation chromatography（GPC） and aminopropyl solid phase extraction column,separated on C18 column,and determined by high performance liquid chromatography（HPLC） with post-column derivatization and fluorescence detection.The results showed good linear relationships between chromatographic peak areas and the concentrations of 11 pesticide residues in the range of 0.01–0.50 mg/L with correlation coefficients more than 0.999.The limits of detection（LOD） and quantitation（LOQ） were 0.3–1.2 μg/kg and 10 μg/kg,respectively.The mean recovery rates for samples with spiked standard at levels of 10,20,50 μg/kg were in the range of 76.2%–95.5% with relative standard deviation（RSD,n = 6） of 3.4%–11.9%.This method is sensitive and reliable and can be used to simultaneously detect 11 carbamate pesticide residues in hotpot condiments.

关 键 词：火锅底料 氨基甲酸酯类农药 高效液相色谱 柱后衍生化 多残留检测 

分 类 号：TS207.53[轻工技术与工程—食品科学]