分析化学2012，Vol.40Issue(12)：1919-1923,5.DOI:10.3724/SP.J.1096.2012.20428
直接溶剂萃取/气相色谱-质谱检测辐照牛肉中的2-十二烷基环丁酮
Determination of 2-Dodecylcyclobutanone in Irradiated Beef by Direct Solvent Extraction and Gas Chromatography-Mass Spectrometry
摘要
Abstract
x A new rapid analytical method based on direct solvent extraction (DSE)/gas chromatogra-phy-mass spectrometry (GC-MS) was developed to analyze 2-dodecyclobutanone (2-DCB) to detect y-ray irradiated beef. A 5 g sample of ground beef patties was homogenized with 7 g of anhydrous sodium sulfate and blended with 150 mL acetonitrile using a blender for 2 min. The extract solvent was carefully transferred to a 500 mL round-bottom flask through filter paper. And the procedure repeated for two times. Then, the extraction solutions were evaporated to dryness using a rotary evaporator. The round-bottom flask was washed with hexane, and the solution was collected into a 50 mL volumetric flask. The 10 mL hexane aliquot was dried to 1 mL via nitrogen stream and then purified with a silica cartridge (1 g, 6 mL). The elution was concentrated to 1 mL with a nitrogen stream, and 1 uL was injected into the gas chromatography-mass spectrometer. The limit of detection and quantitation was 0. 004 and 0. 01 mg/kg, respectively. The procedure was evaluated with a recov?ery test in six samples spiked with 2-DCB at 0. 01 and 0. 5mg/kg of ground beef, resulting in 87. 9% — 91. 6% recoveries with mostly less than 7% RSD. The operation time for sample preparation was about 60 to 90 min. The method was used to detect 2-DCB in ground beef irradiated at 5 targeted absorbed doses of 0. 5, 1.0, 3. 0, 5. 0 and 7. 0 kGy and the concentration of 2-DCB increased linearly with dose (y = 0.0608χ-0.0004, R2 =0. 9899).关键词
2-十二烷基环丁酮/辐照牛肉/直接溶剂萃取/气相色谱-质谱联用Key words
2-Dodecyclobutanone/ Irradiated beef/ Direct solvent extraction/ Gas chromatography- mass spectrometry引用本文复制引用
赵月亮,王锋,周洪杰,李伟明,李安,刘海静,哈益明..直接溶剂萃取/气相色谱-质谱检测辐照牛肉中的2-十二烷基环丁酮[J].分析化学,2012,40(12):1919-1923,5.基金项目
本文系"十二五"国家科技支撑计划(Nos.2012BAK17B13 （）
2012BAD29B03)和农业部公益性行业科研专项(No.201103007)资助项目 （No.201103007）
