Determination of 4-methylimidazole in soy sauce, vinegar and beverage by ultra high-performance liquid chromatography-tandem mass spectrometry

目的：建立酱油、醋和饮料中4-甲基咪唑(4-methylimidazole,4-MeI)的超高效液相色谱-串联质谱检测方法。方法酱油、醋和饮料样品通过MCX固相萃取柱进行净化处理,采用乙腈-水(含0.05%氨水)作为色谱分离条件,在MRM模式下采集4-MeI的信号,同位素内标法定量。结果目标化合物的线性范围为10~1000μg/L,相关系数R为0.9995,三个添加水平的平均回收率为90.5%~101.6%,相对标准偏差(RSD)<6.6%。所有被检测的样品中均含有4-MeI,酱油样品中含有的4-MeI的浓度范围为23.3~4310.8μg/L,平均值为823.3μg/L；醋样品中含有的4-MeI 的浓度范围为111.2~2077.8μg/L,平均值为622.5μg/L；饮料样品中含有的4-MeI 的浓度范围为10.8~307.1μg/L,平均值为94.8μg/L。结论本方法简单、快速、灵敏度高,适用于检测酱油、醋和饮料中4-MeI。Objective To establish a method to determine the 4-methylimidazole (4-MeI) concentrations in soy sauce, vinegar and beverage by ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Methods Soy sauce, vinegar and beverage samples were purified by MCX solid phase extraction column. Then acetonitrile-water (containing 0.05% ammonia) was used as chromatographic separation conditions, the 4-MeI signal was collected in MRM mode and quantified by isotope internal standard. Results The linear relationship was good from 10 μg/L to 1000 μg/L and the correlation coefficient was 0.9995. The recovery of low, medium and high levels was 90.5%~101.6%and the relative standard deviation was less than 6.6%. 4-MeI was contained in all samples. The concentration level of 4-MeI ranged from 23.3~4310.8 mg/kg with a mean of 823.3 μg/L, 111.2~2077.8 μg/L with a mean of 622.5 μg/L and 10.8~307.1 μg/L with a mean of 94.8 μg/L in soy sauce, vinegar and beverage samples, respectively. Conclusion This method is simple, rapid and of high sensitivity, which is suitable for detection of 4-MeI in soy sauce, vinegar and beverages.中国科技核心期刊(ISTIC)03962-96