水产品中氯霉素残留量测定方法的研究  

Study on the determination method of chloramphenicol residues in aquatic products

作　　者：白艳玲[1] 陈剑刚[1] 张彩虹[1] 王丽玲[1] 冯翠霞[1] 谭爱军[1] 瞿进文[2] 

机构地区：[1]广东省珠海市疾病预防控制中心,广东珠海519000 [2]珠海出入境检验检疫局,广东珠海519015

出　　处：《中国卫生检验杂志》2005年第6期672-674,共3页Chinese Journal of Health Laboratory Technology

基　　金：珠海市科技计划项目(PC200310045)

摘　　要：目的:研究了水产品中氯霉素残留量的ECD-气相色谱分析方法。方法:水产品中的氯霉素用乙酸乙酯提取、浓缩后用正己烷抽提脱脂。样液经C18固相萃取小柱净化,BSTFA+TMCS衍生后,用配有电子捕获检测器(ECD)的气相色谱仪测定,外标法定量,气相色谱-质谱法进行确证。结果:方法的最低检出浓度达到0.02μg/kg(S/N=3),在2.5～5000.0ng/ml浓度范围内,线性关系良好,相关系数r=0.9995,加标水平为1.0～10.0μg/kg时,回收率在86.3%～95.3%,相对标准偏差(RSD)为5.02%～9.04%。结论:该方法具有灵敏度高,样品提取简单等特点。Objective:To study the method for the determination of chloramphenicol (CAP) residues in aquatic products by ECD gas chromatography.Methods:The CAP residue was extracted from aquatic products which with ethyl acetate and defatted by n-hexane after concentrated.The sample solution was cleaned up by solid phase extraction C 18 column, derived with BSTFA+TMCS(99+1) and analyzed by electron capture detector gas chromatography using external standard quantitation. At last validated by GC/MS.Results:The detection limit of this method was 0.02 μg/kg(S/N=3).The results showed a good linear (r=0.9995) in the concentration range of 2.5～ 5 000.0 ng/ml,the average recoveries(n=3) for spiked standards(1.0～ 10.0 μg/kg) were 86.3%～95.3%,the relative standard deviations were 5.02%～9.04%.Conclusion:The method is sensitive and simple.

关 键 词：氯霉素残留量 水产品 测定方法 气相色谱-质谱法 电子捕获检测器 色谱分析方法 相对标准偏差 气相色谱仪 外标法定量 乙酸乙酯 固相萃取 浓度范围 线性关系 相关系数 正己烷 回收率 灵敏度 提取 

分 类 号：R155.55[医药卫生—营养与食品卫生学] R284.1[医药卫生—公共卫生与预防医学]