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Analysis of 2-alkylcyclobutanones with accelerated solvent extraction to detect irradiated meat and fish

机译:加速溶剂萃取法分析2-烷基环丁酮以检测辐照的肉和鱼

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A new analytical procedure has been developed to analyze 2-alkylcyclobutanones to detect gamma-ray-irradiated fat-containing foodstuffs. Samples were extracted with an accelerated solvent extraction system via hot and pressurized ethyl acetate in cells. A large amount of fat in the extract was precipitated and removed with filtration by standing at -20 degrees C after the addition of acetonitrile. The extract was further cleaned with a 1 g silica gel mini column, and the radiolytic compounds of 2-docecylcyclobutanone (2-DCB) and 2-tetradecylcyclobutanone (2-TCB) were determined with gas chromatography with mass spectrometry (GC/MS). Sample preparation time before GUMS was 7-8 h. At first, the procedure was evaluated with a recovery test in eight samples spiked with 2-DCB and 2-TCB at 20 ng/g, resulting in 70-105% recoveries with mostly less than 10% relative standard deviations. The procedure was further evaluated with beef, pork, chicken, and salmon samples irradiated with gamma-rays from 0.7 to 7.0 kGy at - 19 degrees C. Both 2-DCB and 2-TCB in most samples were detected with good dose-response relations at all doses, while salmon was detected more than 2 kGy irradiation. The amounts of 2-alkylcyclobutanones produced reflected precursor fatty acids levels in samples, especially for the combination of 2-TCB and stearic acid. The results indicated that the production rate of 2-TCB to stearic acid was more obvious than that of 2-DCB to palmitic acid in frozen samples with gamma-ray irradiation.
机译:已经开发出一种新的分析程序来分析2-烷基环丁酮,以检测伽马射线辐照的含脂肪食品。用加速溶剂萃取系统通过热加压的乙酸乙酯萃取样品。加入乙腈后,在-20°C下静置沉淀,使提取物中的大量脂肪沉淀并过滤除去。将萃取物进一步用1 g硅胶微型柱清洗,并通过气相色谱质谱法(GC / MS)测定2-docyl环丁酮(2-DCB)和2-十四烷基环丁酮(2-TCB)的放射性化合物。 GUMS之前的样品制备时间为7-8小时。首先,该程序通过回收测试评估了20个ng / g掺有2-DCB和2-TCB的八个样品,得到的回收率为70-105%,相对标准偏差大多小于10%。用在-19摄氏度下从0.7至7.0 kGy的伽玛射线辐照的牛肉,猪肉,鸡肉和鲑鱼样品进一步评估了该程序。在大多数样品中检测到2-DCB和2-TCB都具有良好的剂量反应关系在所有剂量下,检测到的鲑鱼辐射均超过2 kGy。产生的2-烷基环丁酮的量反映了样品中前体脂肪酸的水平,特别是对于2-TCB和硬脂酸的组合。结果表明,在γ射线照射下的冷冻样品中,2-TCB转化为硬脂酸的产率比2-DCB转化为棕榈酸的产率更为明显。

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