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

引用本文: 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. doi: 10.3724/SP.J.1096.2012.20428 shu

Citation: ZHAO Yue-Liang, WANG Feng, ZHOU Hong-Jie, LI Wei-Ming, LI An, LIU Hai-Jing, HA Yi-Ming. Determination of 2-Dodecylcyclobutanone in Irradiated Beef by Direct Solvent Extraction and Gas Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2012, 40(12): 1919-1923. doi: 10.3724/SP.J.1096.2012.20428 shu

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

通讯作者: 哈益明

基金项目:
本文系"十二五"国家科技支撑计划(Nos.2012BAK17B13,2012BAD29B03) (Nos.2012BAK17B13,2012BAD29B03)

农业部公益性行业科研专项(No.201103007)资助项目 (No.201103007)

摘要: 应用直接溶剂萃取/气相色谱-质谱技术,建立了辐照牛肉中2-十二烷基环丁酮(2-Dodecylcyclobutanone,2-DCB)的快速检测方法。5 g牛肉糜与7 g无水Na₂SO₄混合均匀后,加入150 mL乙腈,搅拌提取2 min,提取液过滤转移至500 mL圆底烧瓶中,提取重复2次,将提取液旋转蒸干,用正己烷清洗烧瓶并收集,定容至50 mL,取10 mL氮吹浓缩至1 mL,用硅胶固相萃取小柱(1 g,6 mL)净化,淋洗液经氮气吹干后用正己烷定容至1 mL,取1 μL供气相色谱-质谱测定。本方法检出限为0.004 mg/kg,定量限为0.01 mg/kg;牛肉糜中2-DCB添加浓度在0.01-0.50 mg/kg范围内的回收率为87.9%-91.6%,相对标准偏差小于7%,样品前处理仅需60-90 min。采用本方法对辐照剂量为0.5-7.0 kGy的牛肉进行检测,表明辐照剂量与牛肉中2-DCB含量存在线性相关关系(y=0.0608x-0.0004,相关系数R²=0.9899)。

关键词:

English

Determination of 2-Dodecylcyclobutanone in Irradiated Beef by Direct Solvent Extraction and Gas Chromatography-Mass Spectrometry

1.
Institute of Agro-food Science & Technology Chinese Academy of Agricultural Sciences, Key Opening Laboratory of Agricultural Products Processing and Quality Control, Ministry of Agriculture, Beijing 100193, China

Corresponding author: 哈益明

Received Date: 22 April 2012
Fund Project:
本文系"十二五"国家科技支撑计划(Nos.2012BAK17B13,2012BAD29B03)

农业部公益性行业科研专项(No.201103007)资助项目

Abstract: A new rapid analytical method based on direct solvent extraction (DSE)/gas chromatography-mass spectrometry (GC-MS) was developed to analyze 2-dodecyclobutanone (2-DCB) to detect γ-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 μL 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 recovery 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=0.0608x-0.0004, R²=0.9899).

Key words:

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 哈益明

English

Determination of 2-Dodecylcyclobutanone in Irradiated Beef by Direct Solvent Extraction and Gas Chromatography-Mass Spectrometry

Corresponding author: 哈益明

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 哈益明

English

Determination of 2-Dodecylcyclobutanone in Irradiated Beef by Direct Solvent Extraction and Gas Chromatography-Mass Spectrometry

Corresponding author: 哈益明

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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通讯作者: 陈斌, bchen63@163.com

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