凝胶渗透色谱净化-气相色谱-串联质谱法测定辐照肉制品中2-十二烷基环丁酮  

Detection of 2-Dodecylcyclobutanone in Irradiated Meat Products by Gel Permeation Chromatography Followed by Gas Chromatography-Tandem Mass Spectrometry

作　　者：邵彪 周小兰[2] 王琳琳 尤嘉 陈刚 SHAO Biao;ZHOU Xiaolan;WANG Linlin;YOU Jia;CHEN Gang(Nantong Products Quality Supervision and Inspection Institute,Nantong 226011,China;Nantong University Analysis and Testing Center,Nantong 226019,China;Nantong Food and Drug Supervision and Inspection Center,Nantong 226006,China)

机构地区：[1]南通市产品质量监督检验所,江苏南通226011 [2]南通大学分析测试中心,江苏南通226019 [3]南通市食品药品监督检验中心,江苏南通226006

出　　处：《肉类研究》2020年第4期53-56,57,共5页Meat Research

基　　金：国家质量监督检验检疫总局科技计划项目(2015QK060);江苏省质量技术监督“352专业技术人才培养工程”资助项目;南通市“226高层次人才培养工程”资助项目。

摘　　要：基于凝胶渗透色谱(gel permeation chromatography,GPC)净化处理,建立辐照肉制品中2-十二烷基环丁酮(2-dodecylcyclobutanone,2-DCB)的气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)检测方法。样品经正己烷超声提取、GPC净化及氮吹浓缩等步骤处理后,利用GC-MS/MS多反应监测模式进行分析。结果表明:2-DCB在质量浓度10~1 000μg/L范围内线性良好,线性方程为y=383 709.18x-4 686.41,相关系数为0.998 3;25、100、400μg/kg 3个加标水平的平均回收率为78.2%~105.5%,相对标准偏差小于7.3%;检出限和定量限分别为1.8、6.0μg/kg。该方法前处理操作简单、可实现自动化批量处理,同时具有较高灵敏度。Based on clean-up by gel permeation chromatography(GPC), a method for the determination of 2-dodecylcyclobutanone(2-DCB) in irradiated meat products by gas chromatography-tandem mass spectrometry(GC-MS/MS) was established. Samples were subjected to sequential ultrasonic extraction with n-hexane, purification by GPC, concentration and nitrogen blowing evaporation to dryness before being analyzed by GC-MS/MS. The results showed that a linear calibration curve in the concentration range of 10–1 000 μg/L was obtained as follows y = 383 709.18 x-4 686.41, with correlation coefficient of 0.998 3. The average recoveries of 2-DCB at three spiked concentration levels of 25, 100 and 400 μg/kg ranged from 78.2% to 105.5%, with relative standard deviation(RSD) lower than 7.3%. The detection limit and quantitation limit were 1.8 and 6.0 μg/kg, respectively. The method had the advantages of simple pretreatment, largescale automated detection and high sensitivity.

关 键 词：凝胶渗透色谱 辐照肉制品 气相色谱-串联质谱 2-十二烷基环丁酮 

分 类 号：O657.6[理学—分析化学]