全二维气相色谱/飞行时间质谱快速定性筛查食品中32种防腐剂和抗氧化剂

Fast Qualitative Analysis of 32 Preservatives and Antioxidants in Food Sample by Comprehensive Two Dimensional Gas Chromatography Coupled Time of Flight Mass Spectrometry

建立了全二维气相色谱/飞行时间质谱法(GC×GC-TOFMS)快速定性筛查食品样品中19种防腐剂和抗氧化剂、13种超范围使用的非法添加物的方法。以40 mL乙腈为溶剂,对20 g均质样品进行液体萃取,萃取液经过离心过滤后,使用无水MgSO4脱水(含油样品使用40 mL正己烷去除油脂);萃取液再用乙腈稀释5倍进样。本方法采用GC×GC二维特征谱图、TOFMS谱图库检索的定性手段,能在20.5 min内快速分离和定性分析食品中19种防腐剂和抗氧化剂。使用GC×GC-TOFMS技术对含量大于0.3 mg/kg的样品有较好的灵敏度,而在食品添加剂领域,添加量一般都大于100 mg/kg。因此,本方法可以作为一种快速定性筛查的手段。

Comprehensive two dimensional gas chromatography（GC×GC-TOFMS） has been applied to fast qualitative analysis of 32 preservatives,antioxidants in food.GC×GC-TOFMS parameters were evaluated and optimized to yield complete separation for 32 analytes from interference,and to attain the high sensitivity.After optimization,all analytes were separated in 20.5 min and qualitativly analyzed by retention time of GC×GC and mass spectrum library.The method was used to analyze food sample,and the detection limit of most analytes was lower than 0.5 mg/kg,meanwhile,the addition level of food addictives in the field of food industry was usually higher than 100 mg/kg.The method could be used for the rapid qualitative analysis of food preservatives,antioxidants and illegal addictives in food.