采用二维液相色谱-质谱联用技术鉴定间苯三酚注射液中的有关物质。以HSS T3(250 mm × 4。6 mm，5 μm)为色谱柱，1。36 g·L-1磷酸二氢钾(稀磷酸调节pH调至3。0)-乙腈为一维流动相进行梯度洗脱，实现间苯三酚注射液有关物质的分离。各分离成分经多通道切换阀分别被捕集于截留管中，然后输送到BDS C18(100 mm × 4。6 mm，2。4 μm)色谱柱，以0。1％甲酸水溶液-甲醇为二维流动相，进行梯度洗脱实现快速脱盐。电喷雾负离子化-四极杆-飞行时间串联高分辨质谱检测各有关物质母离子及其子离子的准确质量和元素组成，通过质谱解析、有机反应机制分析，甚至对照品对照鉴定它们的结构。在所建立的分析条件下，间苯三酚及其有关物质分离良好，首次检测并鉴定出间苯三酚注射液及其强制降解实验样品中17个主要有关物质，鉴定结果可为间苯三酚注射液质量控制提供参考依据。
Structural identification of the related substances in phloroglucinol injection by two-dimensional liquid chromatography-quadrupole time-of-flight mass spectrometry
This study aimed to identify the related substances of phloroglucinol injection by two-dimensional liquid chromatography quadrupole time-of-flight mass spectrometry(2D-LC-Q-TOF/MS).The first-dimensional separation was carried out on an HSS T3(250 mm × 4.6 mm,5 μm)column by gradient elution using 1.36 g·L1 potassium dihydrogen phosphate buffer solution(pH adjusted to 3.0 with diluted phosphoric acid)and acetonitrile as the mobile phases.The separated components were then trapped in switch valve tube lines respectively and delivered to the second-dimensional desalting gradient elution which was performed with a BDS C18(100 mm × 4.6 mm,2.4 μm)column using 0.1％formic acid and methanol as the mobile phases.After rapid desalting,electrospray-ionization quadrupole time-of-flight high resolution mass spectrometry was used for determining the accurate masses and elemental compositions of the parents and their product ions for both phloroglucinol and its related substance.Structures of the related substances were then figured out by mass spectrometry elucidation,organic reaction mechanism analysis,and/or comparison with reference substances.Under the established analytical conditions,phloroglucinol and its related substances were adequately separated,17 main related substances were detected and identified in the injection and its stressed samples for the first time.The identification results can provide reference for the quality control of phloroglucinol injection.
万方数据
维普
