同位素稀释超高效液相色谱-串联质谱法测定 酱油、醋和饮料中的4-甲基咪唑
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10~1000 μg/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23.3~4310.8 μg/L, 平均值为823.3 μg/L; 醋样品中含有的4-MeI的浓度范围为111.2~2077.8 μg/L, 平均值为622.5 μg/L; 饮料样品中含有的4-MeI的浓度范围为10.8~307.1 μg/L, 平均值为94.8 μg/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.
标题：同位素稀释超高效液相色谱-串联质谱法测定 酱油、醋和饮料中的4-甲基咪唑
英文标题：Determination of 4-methylimidazole in soy sauce, vinegar and beverage by ultra high-performance liquid chromatography-tandem mass spectrometry
作者：
王丽英 河北省疾病预防控制中心
任贝贝 河北省疾病预防控制中心
杨立新 河北省疾病预防控制中心
路杨 河北省疾病预防控制中心
常凤启 河北省疾病预防控制中心
刘印平 河北省疾病预防控制中心
中文关键词:高效液相色谱-串联质谱,4-甲基咪唑,酱油,醋,饮料,
英文关键词:ultra high-performance liquid chromatography-tandem mass spectrometry,4-methylimidazole,soy sauce,vinegar,beverage,
发表日期：2015-01-26
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