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

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10～1 000 μg/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、400 μg/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、6.0 μg/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。

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

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 = 383 709.18x ? 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.