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.
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)
出处
《食品科技》
CAS
北大核心
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)。
