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
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 112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 m/z 98 and qualitative ion of m/z 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 among 0~75.17 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.
标题：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
英文标题：Determination of 2-dodecylcyclobutanone in irradiated pork by accelerated solvent extraction followed by gas chromatography-mass spectrometry
作者：
张秀彤 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
李安 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
潘立刚 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
王冬 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
靳欣欣 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
满燕 北京农业质量标准与检测技术研究中心,农业部农产品质量安全风险评估实验室北京
中文关键词:辐照猪肉,2-十二烷基环丁酮,加速溶剂萃取,
英文关键词:irradiated pork,2-Dodecylcyclobutanone,accelerated solvent extraction,
发表日期：2015-12-05
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