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

中文关键词:  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

英文关键词:3-acetyl-2,5-dimethylfuran  gas chromatography-mass spectrometry  food  synthesized flavor  qualitative and quantitative analysis

中文摘要:

      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, 0.25 μm), 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0.005~10.000 μg/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1 μg/kg, 定量限均可达到3 μg/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。

英文摘要:

      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×0.25 μm) 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 0.005–10.000 μg/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 1 μg/kg, and the limits of quantitation were up to 3 μg/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.