固相萃取-气相色谱质谱法测定焙烤食品中富马酸二甲酯的含量  

Determination of Dimethyl Fumarate in Bakery Food by Supported Phase Extraction(SPE)-Gas Chromatography Mass Spectrometry

作　　者：钟丽君 赵文霞 王春玉 蔡慧敏 赵利 ZHONG Lijun;ZHAO Wenxia;WANG Chunyu;CAI Huimin;ZHAO Li(Bejing Center for Food Safety Monitoring and Risk Assessment,Beijing 100094,China)

机构地区：[1]北京市食品安全监控和风险评估中心,北京100094

出　　处：《食品科技》2022年第8期277-281,共5页Food Science and Technology

基　　金：国家重点研发计划项目(2019YFC1606503)。

摘　　要：目的:建立焙烤食品中富马酸二甲酯含量测定的固相萃取-气相色谱质谱法。方法:试样加水分散后,加无机盐以利于分层,经乙腈涡旋振荡提取,提取液浓缩,并经C_(18)/PSA固相萃取小柱净化,以去除样品中的油脂,试样采用选择离子监测模式进行气相色谱质谱测定,外标法定量。结果:富马酸二甲酯在0.05~1.00μg/mL呈良好的线性关系,相关系数不小于0.999。空白流心奶黄月饼3个水平(0.1、0.2、1.0 mg/kg,n=6)加标回收实验的回收率为88.6%~93.3%、94.0%~98.9%和83.8%~102.3%,相对标准偏差(RSD,n=6)为2.8%~7.3%。空白桃酥样品3个水平(0.1、0.2、1.0 mg/kg,n=6)加标回收实验的回收率为90.4%~95.7%、92.0%~97.8%和89.6%~99.5%,相对标准偏差(RSD,n=6)为2.8%~7.6%。方法的检出限为0.03 mg/kg,定量限为0.1 mg/kg。结论:该方法准确性好、灵敏度高,适用于月饼、糕点等焙烤食品中富马酸二甲酯含量的测定。Objective:To establish a method for the determination of dimethyl fumarate in baked food by Supported Phase Extraction(SPE)-gas chromatography mass spectrometry(GC-MS).Methods:Samples added with inorganic salts were dispersed in water,then extracted with acetonitrile by vortex vibration,and concentrated and purified by C_(18)/PSA solid phase extraction cartridge to remove fat and oils.Dimethyl fumarate was determined by GC-MS under selected ion monitoring(SIM)and quantified by external standard method.Results:Dimethyl fumarate showed a good linear relationship in the range of 0.05~1.00μg/mL with the correlation coefficients not less than 0.999.The recovery of the spiked blank lava custard moon cake with three levels(0.1,0.2,1.0 mg/kg,n=6)were 88.6%~93.3%,94.0%~98.9% and 83.8%~102.3%,with the relative standard deviation(RSD,n=6)were 2.8%~7.3%.The recovery of the spiked blank walnut cookies with three levels(0.1,0.2,1.0 mg/kg,n=6)were 90.4%~95.7%,92.0%~97.8% and 89.6%~99.5%,with the relative standard deviation(RSD,n=6)were 2.8%~7.6%.The detection limit of the method was 0.03 mg/kg,and the limit of quantification was 0.1 mg/kg.Conclusion:The method is accurate and sensitive,and is suitable for the determination of dimethyl fumarate in baked foods such as moon cakes and cakes.

关 键 词：富马酸二甲酯 固相萃取 气相色谱质谱法 焙烤食品 

分 类 号：TS207.55[轻工技术与工程—食品科学]