王丽英,任贝贝,杨立新,路 杨,常凤启,刘印平.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[J].食品安全质量检测学报,2015,6(3):962-967
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
Determination of 4-methylimidazole in soy sauce, vinegar and beverage by ultra high-performance liquid chromatography-tandem mass spectrometry
投稿时间:2015-01-26  修订日期:2015-03-09
DOI:
中文关键词:  高效液相色谱-串联质谱  4-甲基咪唑  酱油    饮料
英文关键词:ultra high-performance liquid chromatography-tandem mass spectrometry  4-methylimidazole  soy sauce  vinegar  beverage
基金项目:
作者单位
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 
AuthorInstitution
WANG Li-Ying Hebei Provincial Center for Disease Control and Prevention 
REN Bei-Bei Hebei Provincial Center for Disease Control and Prevention 
YANG Li-Xin Hebei Provincial Center for Disease Control and Prevention 
LU Yang Hebei Provincial Center for Disease Control and Prevention 
CHANG Feng-Qi Hebei Provincial Center for Disease Control and Prevention 
LIU Yin-Ping Hebei Provincial Center for Disease Control and Prevention 
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中文摘要:
      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。
英文摘要:
      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.
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