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

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.