对虾中4种磺胺类药物残留的超声辅助-基质固相分散提取-柱前衍生高效液相色谱荧光测定法  

Determination of four sulfonamides residues in prawn by ultrasound-assisted matrix solid phase dispersive extraction combined with pre-column derivation high performance liquid chromatography-fluorescence

作　　者：谢进[1] 张宏峰[1] 胡国媛[1] 彭荣飞[1] 罗晓燕[1] 潘心红[1] 于鸿[1] XIE Jin;ZHANG Hong-feng;HU Guo-yuan;PEN Rong-fei;LUO Xiao-yan;PAN Xin-hong;YU Hong(Physical and Chemical Laboratory,Guangzhou Center for Disease Control and Prevention,Guangzhou Guangdong,510440,China)

机构地区：[1]广州市疾病预防控制中心理化检验科,广东广州510440

出　　处：《职业与健康》2020年第9期1200-1204,共5页Occupation and Health

基　　金：广东省医学科学技术研究基金项目(A2019060);广州市卫生健康科技项目(20191A011065)。

摘　　要：目的建立同时测定対虾中磺胺嘧啶、磺胺噻唑、磺胺甲基嘧啶、磺胺二甲嘧啶4种磺胺类药物残留的超声辅助-基质固相分散提取-柱前衍生高效液相色谱方法。方法通过萃取条件的优化,选取乙酸乙酯为萃取剂,弗罗里硅土为固相分散剂,用超声辅助基质固相分散的方式提取对虾中的磺胺类药物。选取荧光胺柱前衍生,高效液相色谱荧光法进行检测。结果在2~100μg/L范围内有较好的线性关系,相关系数>0.999,方法检出限为0.5μg/kg,定量限为2μg/kg。采用该方法对空白对虾样品进行加标回收实验,在2和20μg/kg 2个添加水平下加标回收率为84.4%~93.9%,相对标准偏差(n=3)<7.7%。结论该方法操作简单,耗时少,精密度高,符合残留分析的要求。Objective To establish a method for the simultaneous determination of four sulfonamides residues in prawn,including sulfadiazine,sulfathiazole,sulfamerazine and sulfamethazine,by ultrasound-assisted matrix solid phase dispersion extraction coupled with pre-column derivation high performance liquid chromatography(HPLC).Methods Through the optimization of extraction conditions,ethyl acetate was selected as the extraction agent and florisil as the solid dispersion agent,and the sulfonamides in prawn were extracted with the method ultrasound-assisted matrix solid phase dispersion.The sulfonamides were pre-column derived by fluorescamine and detected by HPLC-fluorescence method.Results All sulfonamides showed good linearity in the concentration range of 2-100μg/L,with the correlation coefficient>0.999.The limit of detection and limit of quantification was 0.5 and 2μg/kg,respectively.The spike recoveries of blank prawn samples were 84.4%-93.9%at two levels of 2 and 20μg/kg,with the relative standard deviation(n=3)less than 7.7%.Conclusion The method is simple,time-consuming and high precision,which meets the requirements of residue analysis.

关 键 词：超声辅助基质固相分散 柱前衍生 高效液相色谱 对虾 磺胺 

分 类 号：R115[医药卫生—公共卫生与预防医学]