色谱

色谱 ›› 2019, Vol. 37 ›› Issue (3): 299-304.DOI: 10.3724/SP.J.1123.2018.10025

• 研究论文 • 上一篇    下一篇

高效液相色谱-离子阱-飞行时间质谱法鉴定碱性嫩黄中的杂质及高效液相色谱法制备碱性嫩黄标准物质

车芬芳1, 路艳珍1, 席兴军2, 兰韬2, 魏芸1   

  1. 1. 北京化工大学, 化工资源有效利用国家重点实验室, 北京 100029;
    2. 中国标准化研究院, 北京 100191
  • 收稿日期:2018-10-19 出版日期:2019-03-08 发布日期:2015-01-21
  • 通讯作者: 魏芸 Tel:+86-10-64442928,E-mail:weiyun@mail.buct.edu.cn.
  • 基金资助:

    National Key Research and Development Program of China (No. 2017YFF0207800); National Natural Science Foundation of China (Nos. 81671411, 21075007); SINOPEC Research and Development Program (No. 217015-6).

Identification of the impurity in auramine O by high performance liquid chromatography-ion trap-time of flight mass spectrometry and preparation of the auramine O reference standard by preparative high performance liquid chromatography

CHE Fenfang1, LU Yanzhen1, XI Xingjun2, LAN Tao2, WEI Yun1   

  1. 1. State Key Laboratory of Chemical Resource Engineering, Beijing University of Chemical Technology, Beijing 100029, China;
    2. China National Institute of Standardization, Beijing 100191, China
  • Received:2018-10-19 Online:2019-03-08 Published:2015-01-21
  • Supported by:

    National Key Research and Development Program of China (No. 2017YFF0207800); National Natural Science Foundation of China (Nos. 81671411, 21075007); SINOPEC Research and Development Program (No. 217015-6).

PDF

82

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。

关键词: 标准物质, 高效液相色谱-离子阱-飞行时间质谱, 碱性嫩黄, 杂质鉴定, 制备高效液相色谱

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 10 μm and 5 μm were used for the separation and purification with injection volumes of 1 mL and 500 μL, 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.

Key words: auramine O, high performance liquid chromatography-ion trap-time of flight mass spectrometry (HPLC-IT-TOF-MS), impurity identification, preparative high performance liquid chromatography (prep-HPLC), reference standard

中图分类号: