凝胶渗透色谱-气相色谱/串联质谱法分析辐照肉松与乳粉中2-十二烷基环丁酮含量  

Determination of 2-dodecylcyclobutanone in irradiated dried meat floss and milk powder by gel permeation chromatography-gas chromatography-tandem mass spectrometry

作　　者：邵彪 周小兰[2] 尤嘉 王琳琳 陈刚 SHAO Biao;ZHOU Xiao-Lan;YOU Jia;WANG Lin-Lin;CHEN Gang(Nantong Products Quality Supervision and Inspection Institute,Nantong 226011,China;Nantong University Analysis&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,南通226011 [2]南通大学分析测试中心,南通226019 [3]南通市食品药品监督检验中心,南通226006

出　　处：《食品安全质量检测学报》2020年第14期4723-4731,共9页Journal of Food Safety and Quality

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

摘　　要：目的利用凝胶渗透色谱-气相色谱/串联质谱法分析不同辐照剂量处理的肉松与乳粉中2-十二烷基环丁酮含量。方法样品中目标组分经正己烷超声提取,使用凝胶渗透色谱净化去除大分子成分并结合在线浓缩处理后,利用气相色谱-串联质谱进行分析检测,其中质谱扫描采用多反应监测模式(multireaction monitoring mode,MRM),所监测离子对为(m/z)98.1>83.1、(m/z)98.1>70.1、(m/z)98.1>55.0、(m/z)112.2>97.1。结果在10~1000μg/L范围内2-十二烷基环丁酮标准曲线方程具有良好的线性关系,方法的检出限和定量限分别为2.3、7.7μg/kg,在20、100、500μg/kg3个水平下的平均加标回收率在73.5%~98.2%之间,相对标准偏差小于6.2%。结论该方法灵敏度高、准确性好、操作简单,可用于辐照肉松与乳粉中2-十二烷基环丁酮检测。Objective To analyze the content of 2-dodecyl cyclobutanone in meat floss and milk powder treated with different irradiation doses by gel permeation chromatography-gas chromatography/tandem mass spectrometry.Methods The target components were extracted by N-hexane ultrasound,purified by gel permeation chromatography to remove macromolecular components and concentrated on-line,and then analyzed by gas chromatography-tandem mass spectrometry.The mass spectrometry scanning adopted multi-reaction monitoring mode(MRM),and the monitored ion pairs were(m/z)98.1>83.1,(m/z)98.1>70.1,(m/z)98.1>55.0,(m/z)112.2>97.1.Results The standard curve equation of 2-dodecyl cyclobutanone had a good linear relationship in the range of 10–1000 g/L.The detection limit and quantitative limit of the method were 2.3 g/kg and 7.7 g/kg,respectively.The average recoveries of 2-dodecyl cyclobutanone were 73.5%–98.2%and the relative standard deviations were less than 6.2%at the levels of 20,100,500 g/kg.Conclusion This method has high sensitivity,good accuracy and simple operation,and can be used for the detection of 2-dodecyl cyclobutanone in irradiated meat floss and milk powder.

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

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]