固相萃取—超高效液相色谱—质谱法测定食用香精中3种甲基咪唑类物质  

Determination of three methylimidazole compounds in food flavors by solid phase extraction coupled with ultra-performance liquid chromatography-mass spectrometry

作　　者：周艳华[1] 李涛 向俊 徐文泱 ZHOU Yan-hua;LI Tao;XIANG Jun;XU Wen-yang(Changsha Environmental Protection College,Changsha,Hunan 410004,China;Hunan Institute of Commodity Quality Inspection,Hunan Provincial Key Laboratory of Food Safety Monitoring and Early Warning,Changsha,Hunan 410011,China)

机构地区：[1]长沙环境保护职业技术学院,湖南长沙410004 [2]湖南省产商品质量检验研究院食品安全监测与预警湖南省重点实验室,湖南长沙410111

出　　处：《食品与机械》2022年第10期82-86,200,共6页Food and Machinery

基　　金：湖南创新型省份建设专项项目(编号:2020SK2128);湖南省科技创新平台与人才计划项目(编号:2019TP1058)。

摘　　要：目的:同时、快速检测食用香精中3种甲基咪唑化合物。方法:利用5%三氯乙酸溶液提取食用香精,再利用PCX混合阳离子固相萃取柱净化提取液,最后利用超高效液相色谱—质谱法和内标法进行定性和定量分析。结果:3种甲基咪唑化合物在5.0~400.0 ng/mL内呈良好线性关系,相关系数R 2≥0.997。3种甲基咪唑检出限为0.030~0.450μg/kg,定量限(LOQ)为0.10~1.50μg/kg。3种甲基咪唑的加标回收率在82.8%~111.7%,相对标准偏差RSD在1.3%~9.3%。结论:该方法简单高效、准确度高,可作为食用香精中甲基咪唑的定量检验方法。Objective:This study aimed to establish a method for quick determination of 3 kinds ofmethylimidazole compounds in food flavor.Methods:The food flavor was extracted with 5%trichloroacetic acid solution and purified with PCX mixed cationic solid phase extraction column.Finally,the qualitative and quantitative analysis was carried out by ultra-performance liquid chromatography-mass spectrometry(UPLC-MS/MS)and internal standard method.Results:The linear relationship between the three methyl imidazole compounds was good in the range of 5.0~400.0 ng/mL,with correlation coefficient R 2≥0.997.The limits of detection were 0.030~0.450μg/kg and the limits of quantification(LOQ)were 0.10~1.50μg/kg.The recoveries of three methylimidazole ranged from 82.8%to 111.7%,and the relative standard deviations(RSDS)ranged from 1.3%to 9.3%.Conclusion:The method is simple,efficient and accurate,and can be used for the quantitative determination of 1-methylimidazole,2-methylimidazole,4-methylimidazole in food flavor.

关 键 词：固相萃取 超高效液相色谱—质谱法 甲基咪唑化合物 食用香精 

分 类 号：O657.63[理学—分析化学] TS264.3[理学—化学]