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采用加速溶剂萃取法分析2-烷基环丁酮以检测辐照肉类和鱼类。

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

作者信息

Obana Hirotaka, Furuta Masakazu, Tanaka Yukio

机构信息

Osaka Prefectural Institute of Public Health, 1-3-69, Nakamichi, Higashinari, Osaka, 5370025, Japan.

出版信息

J Agric Food Chem. 2005 Aug 24;53(17):6603-8. doi: 10.1021/jf0506636.

DOI:10.1021/jf0506636
PMID:16104773
Abstract

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 GC/MS 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.

摘要

已开发出一种新的分析方法来分析2-烷基环丁酮,以检测经γ射线辐照的含脂肪食品。样品通过加速溶剂萃取系统,在细胞中用热的加压乙酸乙酯进行萃取。提取物中大量的脂肪在加入乙腈后,通过在-20℃下静置过滤沉淀并去除。提取物再用1g硅胶微型柱进一步净化,并用气相色谱-质谱联用仪(GC/MS)测定2-十二烷基环丁酮(2-DCB)和2-十四烷基环丁酮(2-TCB)的辐射分解产物。GC/MS之前的样品制备时间为7-8小时。首先,通过在八个添加了20ng/g 2-DCB和2-TCB的样品中进行回收率测试来评估该方法,回收率为70-105%,相对标准偏差大多小于10%。该方法进一步用在-19℃下经0.7至7.0kGyγ射线辐照的牛肉、猪肉、鸡肉和三文鱼样品进行评估。在所有剂量下,大多数样品中的2-DCB和2-TCB均被检测到,具有良好的剂量反应关系,而三文鱼在辐照剂量超过2kGy时被检测到。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射线辐照的冷冻样品中,2-TCB与硬脂酸的生成率比2-DCB与棕榈酸的生成率更明显。

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引用本文的文献

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J Toxicol Pathol. 2015 Apr;28(2):99-107. doi: 10.1293/tox.2015-0002. Epub 2015 Feb 16.