高分辨质谱库和特征组分诊断比值法快速筛查鉴别食品中非法添加黄芪

Rapid screening and identification of illegally added Astragalus membranaceus in food by high resolution mass spectrometry library and diagnostic ratio of characteristic components

目的 建立一种基于高分辨质谱库和高效液相色谱特征组分诊断比值法筛查鉴别食品中非法添加黄芪的方法。方法 采用高效液相色谱-四极杆-飞行时间质谱仪构建黄芪4种特征组分高分辨质谱库进行初步筛查;将不同产地和采摘时间的黄芪中药材模拟配制酒、代用茶和饮料样品,构建3种基质中黄芪特征组分高效液相色谱-紫外检测器分析方法,以不同基质组间无显著性差异的特征组分的高效液相色谱峰面积诊断比值作为确证指标。结果 建立了黄芪4种特征组分高分辨质谱库,确定了黄芪中不同基质组间无显著性差异的1组高效液相色谱特征组分峰面积诊断比值DR1(毛蕊异黄酮苷/芒柄花苷),诊断比值非异常值范围分别为1.86~2.71;并对实际样品配制酒、代用茶及饮料进行分析, 1批次配制酒样品与黄芪4种特征组分高分辨质谱库匹配一致,且高效液相色谱特征组分诊断比值DR1为1.98,在规定区间内,推断该配制酒样品中加入了黄芪中药材。结论 该方法准确、快捷、稳定性好,可快速筛查和鉴别食品中非法添加黄芪,为打击食品中非法添加黄芪违法行为提供技术支撑。

Objective To establish a method for screening and identifying illegally added Astragalus membranaceus in food based on high resolution mass spectrometry library and high performance liquid chromatography characteristic component diagnostic ratio method.Methods High resolution mass spectrometry library of 4 kinds of characteristic components of Astragalus membranaceus was constructed by high performance liquid chromatography quadrupole time of flight mass spectrometry for preliminary screening;the samples of prepared wine,substitutional tea and beverages were prepared from Astragalus membranaceus of different producing areas and picking time,then the high performance liquid chromatography-ultraviolet detector analysis method was established for the characteristic components of Astragalus membranaceus in 3 kinds of different matrices,the diagnostic peak area ratio of the characteristic components with no significant difference between the different matrix groups in high performance liquid chromatography was used as the confirmatory index.Results A high resolution mass spectrometric database of 4 kinds of characteristic components of Astragalus membranaceus was establish,and a group of diagnostic peak area ratios DR1(calycosin/ononin) of characteristic components of high performance liquid chromatography without significant difference among different matrix groups in Astragalus membranaceus was identify,with non-abnormal values of that diagnostic ratio ranging from 1.86 to 2.71,respectively;the actual prepared wine,substitutional tea and beverages were analyzed,and the first batch of prepared wine sample was matched with the high resolution mass spectrometry library of the 4 kinds of characteristic components of Astragalus membranaceus,and the diagnostic ratio of the characteristic components DR1 of high performance liquid chromatography was 1.98,within the specified range,it was deduced that Astragalus membranaceus was added into the prepared wine sample.Conclusion This method is accurate,rapid and stable,and can quickly screen and identify the illegal addition of Astragalus membranaceus in food,provide technical support for combating illegal addition of Astragalus membranaceus in food.