加速溶剂萃取/GC-MS法对辐照肉类食品中2-十二烷基环丁酮的检测

Determination of 2-Dodecylcyclobutanone in Irradiated Foods by Accelerated Solvent Extractor Coupled with GC-MS

应用加速溶剂萃取(ASE)/气相色谱-质谱(GC-MS)技术建立了辐照肉类食品中2-十二烷基环丁酮(2-DCB)的检测方法。采用加速溶剂萃取法从辐照过的肉类样品中提脂,萃取液加入乙腈后冰箱冷冻去除脂肪,LC-Si固相萃取小柱净化,氮气吹干后加入内标定容,于GC-MS仪上测定,在0.1～0.4μg/g(以脂肪计)范围内的回收率为78%～92%,RSD小于11%,定量下限为0.1μg/g(以脂肪计)。同时采用该方法对辐照剂量为1～8kGy的猪肉、鸡肉和鱼肉进行检测,再次证明了辐照剂量与脂肪中2-DCB含量存在线性相关关系。

A gas chromatography -mass spectrometry method was developed for analysis of 2-dode- cylcyclobutanone（2-DCB） in irradiated meat. The fat of irradiated meat was removed by accelerated solvent extractor（ASE） using ethyl acetate as extraction solvent. The extract was cleaned up by pass- ing through LC-Si solid phase extraction cartridge. The elute was evaporated to dryness under nitrogen and redissolved with internal standard solution. The quantitative detecting was performed by GC - MS. The calibration curve showed a good linearity over 2-DCB concentration in the range of 0. 1 - 0.4 μg/g（fat）. The limit of quantitation（LOQ） was 0. 1 μg/g（fat） and the recoveries were in the range of 78% -92% with RSD of less than 11%. The method was used to the determination of pork, chicken and fish that irradiated at dose of 1 -8 kGy. The result also indicated that the irradiated dos- age is linear with the concentration of 2-DCB in fat.