【摘要】 该文建立了一种高效液相色谱-离子阱-飞行时间质谱(HPLC-IT-TOF-MS)分析非法食品添加剂碱性嫩黄样品中杂质成分的方法。对碱性嫩黄样品中的杂质进行多级质谱分析,根据各碎片离子的精确质量数推测出该杂质的具体组成,确定这个杂质为4-(亚氨基(4-(甲基氨基)苯基)甲基)-N,N-二甲基苯胺盐酸盐,从而推断出碱性嫩黄的合成方法及杂质的可能来源。同时建立了制备碱性嫩黄标准物质的方法,分别选用了粒径为10μm和5μm的制备液相色谱柱进行两次制备高效液相色谱分离纯化,进样量分别为1 mL和500μL,最终采用分析型高效液相色谱峰面积归一化法得到纯度为99.52%的碱性嫩黄标准物质。扣除0.34%水分含量,0.13%灰分含量,采用质量平衡法确定制备的物质最终纯度为99.05%,并通过UV、IR、LC-MS和NMR四大谱图进行化学结构的确认。该方法简单、高效,可拓展应用于其他非法食品添加剂标准物质的制备。更多还原

【Abstract】 A novel and effective method was established for the qualitative analysis of impurities in auramine O samples of illegal food additives using high performance liquid chromatography-ion trap-time of flight mass spectrometry(HPLC-IT-TOF-MS).An impurity was identified in the auramine O sample using the optimized HPLC-IT-TOF-MS method.According to the exact mass of each fragment ion measured by multistage MS,the structure of the impurity was determined to be that of 4-(imino(4-(methylamino)phenyl)methyl)-N,N-dimethylaniline hydrochloride.The synthetic route of the auramine O and the source of the identified impurity were proposed.Simultaneously,a preparative high performance liquid chromatography(prep-HPLC)technique was successfully applied for the purification of the auramine O from complex samples.Prep-HPLC columns with particle sizes of 10μm and 5μm were used for the separation and purification with injection volumes of 1 mL and500μL,respectively.Finally an auramine O reference standard with 99.52%purity was obtained by secondarily purification and determined by the analytical HPLC area normalization method.Deducting the 0.34%moisture content and 0.13%ash content,the final purity of the sample was 99.05%,as determined by mass balance method.The chemical structure was examined using UV,IR,LC-MS,and NMR.The developed method is simple and efficient,and can be applied for the preparation of reference standard materials for other illegal food additives.更多还原