气相色谱-质谱法测定食品中3-乙酰基-2,5-二甲基呋喃  

Determination of 3-acetyl-2,5-dimethylfuran in food by gas chromatography-mass spectrometry

作　　者：张瑾如 王韦达[1] 张洁吟 杨睿 卢灿鑫 蔡琳 刘晓晗 林长虹[1] ZHANG Jin-Ru;WANG Wei-Da;ZHANG Jie-Yin;YANG Rui;LU Can-Xin;CAI Lin;LIU Xiao-Han;LIN Chang-Hong(Shenzhen Academy of Metrology&Quality Inspection,Shenzhen 518131,China)

机构地区：[1]深圳市计量质量检测研究院,深圳518131

出　　处：《食品安全质量检测学报》2024年第11期84-89,共6页Journal of Food Safety and Quality

摘　　要：目的建立气相色谱-质谱法(gas chromatography mass spectrometry,GC-MS)测定食品中合成香料3-乙酰基-2,5-二甲基呋喃的方法。方法样品用正己烷涡旋提取后过滤,含油脂样品采用冷冻过滤技术去除油脂和其他杂质,选用TG-5MS毛细管色谱柱(30 m×0.25 mm,0.25μm),载气流速1 mL/min进行分离后进质谱分析。结果3-乙酰基-2,5-二甲基呋喃在0.005~10.000μg/L质量浓度范围内曲线线性良好,相关系数为0.9997;在不同基质及不同加标浓度下,加标回收率为80.16%~103.76%,相对标准偏差为1.83%~7.87%(n=6);3-乙酰基-2,5-二甲基呋喃在不同基质中的检出限均可达到1μg/kg,定量限均可达到3μg/kg。结论该方法简单、准确度高、灵敏度好,可以用于食品中3-乙酰基-2,5-二甲基呋喃含量的快速检测,为合成香料的安全使用和监管提供技术手段。Objective To establish a method for the determination of 3-acetyl-2,5-dimethylfuran in food by gas chromatography-mass spectrometry(GC-MS).Methods Samples were extracted with n-hexane vortex and filtered,and the oil-containing samples were filtered by freeze filtration to remove the oil and other impurities.The 3-acetyl-2,5-dimethylfuran was well separated using the TG-5MS capillary chromatographic column(30 m×0.25 mm×0.25μm)with a carrier gas flow rate of 1 mL/min before mass spectrometry analysis.Results The linear curves of 3-acetyl-2,5-dimethylfuran was good in the mass concentration range of 0.005–10.000μg/L,and the correlation coefficient was 0.9997.The recoveries were 80.16%–103.76%and the relative standard deviations(n=6)were 1.83%–7.87%under different substrates and spiked concentrations.The limits of detection of 3-acetyl-2,5-dimethylfuran in different substrates were up to 1μg/kg,and the limits of quantitation were up to 3μg/kg.Conclusion The method is simple,accurate and sensitive,and can be used for the rapid detection of 3-acetyl-2,5-dimethylfuran content in food,providing technical means for the safe use and supervision of synthetic flavors.

关 键 词：3-乙酰基-2 5-二甲基呋喃 气相色谱-质谱法 食品 合成香料 定性定量分析 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]