加速溶剂萃取-气相色谱-质谱法测定辐照猪肉中2-十二烷基环丁酮

Determination of 2-dodecylcyclobutanone in irradiated pork by accelerated solvent extraction followed by gas chromatography-mass spectrometry

目的建立简便、快速、准确的基于加速溶剂萃取技术的辐照猪肉中特异性辐解产物2-十二烷基环丁酮（2-dodecylcyclobutanone,2-DCB）提取方法,利用该方法结合气相色谱-质谱（GC-MS）联用技术测定辐照猪肉中2-DCB含量。方法以正己烷为萃取溶剂、中性氧化铝为粗脂肪吸附剂,在系统压力1500 psi、80℃条件下快速提取纯化猪肉中的2-DCB,采用GC-MS方法并以m/z 98为定量离子、m/z 1 12为定性离子进行分析检测。结果本方法对2-DCB的定量检出限为12.25 ng/g,回收率大于80%,相对标准偏差〈10%（n=3）,提取时间仅为20 min。采用该方法对辐照剂量为0~8 kGy的猪肉进行检测,浓度范围为0~75.17 ng/g。结论此法实现了2-DCB的快速提取纯化,操作简便、重现性好,且定量计算方法更为科学,可用于辐照食品中2-DCB的检测分析和辐照食品的判定。

Objective To establish a simple,rapid and accurate extraction method based on accelerated solvent extraction technology combined with gas chromatography-mass spectrometry（GC-MS） for quantitative determination of 2-dodecylcyclobutanone（2-DCB） in irradiated pork.Methods The samples were extracted with hexane as solvent and neutral alumina as crude fat adsorbent,and the 2-DCB of the purified pork was rapidly extracted under the system pressure of 1500 psi and the temperature of 80 ℃.The sample was then analyzed by GC-MS method with quantitative ion of mlz 98 and qualitative ion of mlz 112.Results The detection limit for 2-DCB by this method was 12.25 ng/g,and the recoveries were over 80%,with the relative standard deviations all below 10%（n=3）.The extraction time cost only 20 min.The method was applied to the determination of pork that were irradiated at the dose among 0~8 kGy,with the concentration range among0~75.17 ng/g.Conclusion This extraction and purification method for 2-DCB is simple,fast,with easy operation and good reproducibility,the quantitative calculation method is more scientific than literatures,and it can be used for the detection and analysis of 2-DCB in irradiated food.