GPC-GC-MS测定糕点和麻辣食品中的富马酸二甲酯

Determination of Dimethyl Fumarate in Pastry and Spicy Snacks by GPC-GC/MS

建立快速凝胶柱的全自动凝胶净化系统(gel permeation chromatography,GPC)-气相色谱-质谱联用(gas chromatography-mass spectrometry,GC-MS)检测食品中防腐剂富马酸二甲酯。以环己烷:乙酸乙酯(1:1,V/V)为提取液,利用GPC对样品进行净化和浓缩,应用选择离子监测(selected ion monitoring,SIM)模式,以m/z 113、85、59为定量离子,GC-MS进行定性和定量分析,建立富马酸二甲酯的提取和检测方法。该方法回归方程为Y=4018974X-56743,线性范围为0.02～20.0mg/L,相关系数0.9991,检出限为0.02mg/kg,添加水平为0.05、0.5、1.5mg/kg时加标回收率为89.5%～94.0%、相对标准偏差为4.0%～5.7%(n=6)。结果表明,该法具有回收率高、检出限低、自动化程度高等优势。

Dimethyl fumarate is widely used in the food industry as an antifungal agent.Because of the high content of oil and spice in pastry and spicy snacks,extraction and determination of dimethyl fumarate from these matrices is challenging.In this study,a GPC-GC/MS method to determine dimethyl fumarate residues in pastry and spicy snacks was established.Samples were extracted with a mixture of cyclohexane and ethyl acetate（1：1,V/V） and the extract was cleaned up and concentrated in an automated GPC system.Dimethyl fumarate was analyzed by GC-MS in the selective ion monitoring mode using m/z 113,85,and 59 as qualitative ions.A regression equation was built for the method as follows： Y = 4018974X-56743,with a linear range of 0.02-20.0 mg/L and a correlation coefficient of 0.9991.The detection limitation of the method was 0.02 mg/kg.The average recoveries across the spike levels of 0.05,0.5 mg/kg and 1.5 mg/kg were between 89.5% and 94.0% with a relative standard derivation ranging from 4.0% to 5.7%（n = 6）.The method was of high recovery,low detection limit and high automation.