论文部分内容阅读
目的建立凝胶渗透色谱净化.气相色谱.质谱.内标法测定焙烤食品中富马酸二甲酯残留量的方法。方法试样经乙酸乙酯超声提取,经凝胶渗透色谱(gel permeation chromatography,GPC)净化,采用选择离子监测模式(selective ion monitoring,SIM)进行气相色谱一质谱(gas chromatography-mass spectrometry,GC-MS)测定,采用丁二酸二甲酯作为内标,以内标法定量。结果富马酸二甲酯在0.02~5.00 mg/L内呈良好的线性关系,相关系数(r)大于0.9999;0.1、0.2和1.0 mg/kg水平的空白糕点加标回收实验的回收率为92.0%~107%,相对标准偏差(RSD)为3.2%~5.7%(n=6);方法的检出限(limit of detection,LOD)为0.012 mg/kg,定量限(limit of quantity,LOQ)为0.04 mg/kg。结论该方法准确、灵敏度高,适用于糕点等焙烤食品中富马酸二甲酯残留水平测定。
OBJECTIVE To establish a method for the determination of dimethyl fumarate residues in bakery products by gel permeation chromatography (GC-MS) and gas chromatography-mass spectrometry. Methods The samples were extracted with ethyl acetate and purified by gel permeation chromatography (GPC). Gas chromatography-mass spectrometry (GC-MS) was performed using selective ion monitoring (SIM) MS), using dimethyl succinate as internal standard and internal standard method. Results The linear relationship between dimethyl fumarate and 0.02 ~ 5.00 mg / L linear regression was obtained. The correlation coefficient (r) was greater than 0.9999. The recovery rate of spiked samples at 0.1, 0.2 and 1.0 mg / kg was 92.0 The limit of detection (LOD) was 0.012 mg / kg, and the limit of quantity (LOQ) was between 10% and 107% with a relative standard deviation (RSD) 0.04 mg / kg. Conclusion The method is accurate and sensitive. It is suitable for the determination of dimethyl fumarate residues in baked goods such as cakes.