[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].
Se Pu
; 37(3): 299-304, 2019 Mar 08.
Article
en Zh
| MEDLINE
| ID: mdl-30900859
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.
Palabras clave
Texto completo:
1
Banco de datos:
MEDLINE
Asunto principal:
Benzofenoneido
/
Contaminación de Alimentos
/
Contaminación de Medicamentos
/
Aditivos Alimentarios
Tipo de estudio:
Diagnostic_studies
/
Qualitative_research
Idioma:
Zh
Revista:
Se Pu
Año:
2019
Tipo del documento:
Article
País de afiliación:
China