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

文章建立了气相色谱-质谱法测定食品中3-乙酰基-2,5-二甲基呋喃的分析方法。样品用正庚烷超声提取,提取液离心后进行冷冻除脂处理,上清液经分散固相萃取净化,净化液用气相色谱-质谱法检测分析,采用选择离子监测模式,外标法定量。结果表明,3-乙酰基-2,5-二甲基呋喃浓度在0.005~0.250μg/mL范围内线性良好(r>0.999),检出限和定量限分别为0.010 mg/kg和0.030 mg/kg。4种不同食品基质的3个加标水平下的平均回收率为93.1%~106.0%,相对标准偏差(n=6)为0.74%~3.47%。该方法操作相对简单,具有较高的准确度和精密度,适用于食品中3-乙酰基-2,5-二甲基呋喃的测定。

A method for the determination of 3-acetyl-2,5-dimethylfuran in food by gas chromatography-mass spectrometry was established.Samples were extracted by ultrasound with n-heptane,and the extraction liquid was frozen to remove fat after centrifugation,and then the supematant was purified using dispersive solid-phase extraction.Finally,the purified liquid was analyzed by gas chromatography-mass spectrometry in the selected ion monitoring(SIM)mode.For quantification of 3-acetyl-2,5-dimethylfuran,the external standard method was utilized.The results showed that the method had a good linearity(r>0.999)within the concentration range of 0.005–0.250μg/mL for 3-acetyl-2,5-dimethylfuran,and the limits of detection and quantitation were determined to be 0.010 mg/kg and 0.030 mg/kg,respectively.The average recoveries of four food substrates were 93.1%–106.0%in the three levels of spiked food matrices with relative standard deviations(RSD,n=6)ranging from 0.74%to 3.47%.The results showed that the method was simple,sensitive and accurate,which could be used for the determination of 3-acetyl-2,5-dimethylfuran in food.