高分辨质谱库和特征组分诊断比值法快速鉴别食品中非法添加淫羊藿

建立了一种基于高分辨质谱库和特征组分诊断比值法鉴别食品中非法添加淫羊藿的方法。采用高效液相色谱-四极杆-飞行时间质谱仪构建淫羊藿6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淫羊藿中药材模拟配制酒、代用茶和饮料样品,构建3种基质中淫羊藿特征组分液相色谱分析方法,选取受产地、采摘时间、加工工艺等影响较小,不同基质组间无显著性差异的3组特征组分峰面积诊断比值DR1(朝藿定A/朝藿定B)、DR3(朝藿定A/淫羊藿苷)和DR7(朝藿定B/淫羊藿苷),合并后绘制箱图确定各诊断比值非异常值范围分别为0.60~0.96、0.26~0.64和0.35~0.91,以此作为鉴别指标。对实际样品配制酒、代用茶及饮料进行分析,1批次配制酒样品与淫羊藿6种特征组分高分辨质谱库匹配一致,且3组特征组分诊断比值DR1、DR3、DR7分别为0.73、0.28、0.38,均在规定区间内,推断该配制酒样品中加入了淫羊藿中药材。该方法准确、快捷、稳定性好,可快速鉴别食品中非法添加淫羊藿,为打击食品中非法添加淫羊藿违法行为提供技术支撑。

Rapid Identification of Illegally Added Epimedium in Food Based on High-resolution Mass Spectrometry Library and Diagnostic Ratio of Characteristic Components

A method based on high-resolution mass spectrometry library and characteristic component diagnostic ratio was established for identifying illegally added epimedium in food. A high resolution mass spectrometry library of six characteristic components of epimedium was constructed by high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (HPLC-TOF-MS) for preliminary screening. Simulated wine, substitute tea and drink samples were prepared using Chinese medicinal materials of epimedium obtained from different origins and picking times. A liquid chromatography analysis method was established for the characteristic components of epimedium in three different matrices. The characteristic component peak area diagnostic ratios, DR1 (epimedin A/ epimedin B), DR3 (epimedin A/ icariin) and DR7 (epimedin B/ icariin), which were less affected by the origin, picking time and processing technology, with no significant differences among different matrix groups, were selected and combined to draw box plots. . Then, the non-abnormal value ranges of diagnostic ratios were determined to be 0.60~0.96, 0.26~0.64 and 0.35~0.91, respectively, which were used as identification indicators. The actual samples of prepared wine, substitute tea and drink were analysed. The prepared wine samples of one batch matched with the high-resolution mass spectrometry library of the six characteristic components of epimedium. The diagnostic ratios of the three characteristic components DR1, DR3 and DR7 were 0.73, 0.28 and 0.38, respectively, which were all within the specified range, inferring that epimedium-containing Chinese medicinal materials had been added to the prepared wine samples. The method is accurate, fast and stable, and can quickly identify the illegal addition of epimedium to food and provide technical support for cracking down on the illegally added epimedium in food.