快速衍生-全自动固相萃取液质联用法测定食品中硝基呋喃代谢物  

Determination of nitrofuran metabolites in food by rapid derivatization-Auto SPE and LC/MS/Ms methods

作　　者：王勤[1] 刘辉 李秋霞[1] 朱国婵 邹国燊 WANG Qin;LIU Hui;LI Qiu-xia;ZHU Guo-chan;ZOU Guo-shen(Maoming Center for Disease Control and Prevention,Maoming,Guangdong 525000,China)

机构地区：[1]茂名市疾病预防控制中心,广东茂名525000 [2]茂名海关,广东茂名525000

出　　处：《中国卫生检验杂志》2019年第13期1547-1550,共4页Chinese Journal of Health Laboratory Technology

基　　金：茂名市科技计划(201552)支撑项目

摘　　要：目的建立食品中硝基呋喃代谢物快速衍生的全自动固相萃取-液质联用检测方法。方法采用混合标准溶液衍生后峰面积的响应值对衍生溶液、衍生剂用量、衍生温度和时间进行优化,以确定最佳衍生条件。衍生完成后,调节pH值至7.2±0.2,然后上全自动固相萃取仪,过HLB小柱净化。结果以5%三氯乙酸为衍生溶液,在60℃下,加入50μl快速衍生剂,4种硝基呋喃代谢物在10 min内可以完成衍生。经HLB小柱净化后,方法检出限达0.50μg/kg,加标回收率为86.7%~113.9%,RSD为2.0%~15.8%。结论快速衍生方法具有检测速度快、灵敏度低、前处理简单、回收率高等优点,能较好地满足食品中硝基呋喃代谢物检测的需求。Objective To establish a testing method for the nitrofuran metabolites in foods by rapid derivatization and automatic solid phase extraction-liquid chromatography-mass spectrometry.Methods The response of peak area after derivatization with the mixed standard solution was optimized for derivatization solution,amount of derivatizing agent,derivatization temperature and time to derivatization.After derivatization was completed,pH was adjusted to 7.2±0.2,then purified by the HLB cartridge through the automatic solid phase extraction apparatus.Results With 5% trichloroacetic acid as the derivatization solution,50 μl of the fast derivatizing agent was added and the temperature was set at 60 °C.The four kinds of nitrofuran metabolites were derivatized in 10 min.After purification by HLB cartridge,the detection limit of the method was 0.50 μg/kg and the recoveries range was 86.7%-113.9% and the RSD range was 2.0%-15.8%.Conclusion The rapid derivatization method had the advantages of fast detection speed,low sensitivity,simple pretreatment and high recovery rate,which can better meet the needs of nitrofuran metabolite detection in foods.

关 键 词：硝基呋喃 代谢物 快速 衍生 固相萃取 

分 类 号：O657.63[理学—分析化学]