In the process of derivation of twenty seven kinds of amines with methylbenzoyl chloride, the reaction between active hydrogen and derivative reagent was studied. A new method has been developed for the determination of twenty seven amine derivatives by the ultra high liquid chromatography-mass spectrometry. Waters ACQUITY UPLC® HSS T3(Φ1. 8μm, 3. 0 mm × 150 mm) was employed as the analytical column, the mobile phase were acetonitrile and formic acid (0. 1%), two gradient elution procedures were used. After the separation by liquid chromatography, the mass spectrometric qualitative analysis was performed based on the selective ionic measurement [ M+H]+using the electro-spray ionization in positive mode. The instrument detection limits of amines were 0. 2 mg/L. The proposed method was successfully applied to the fast qualitative analysis of amines.%研究了27种胺类物质在与间甲基苯甲酰氯的衍生化过程中,活泼氢与衍生化试剂的反应情况.建立了超高液相色谱-质谱分析27种胺类衍生物的定性分析方法.使用Waters ACQUITY UPLC® HSS T3色谱柱(Φ1.8μm,3.0 mm×150 mm)为分离柱,乙腈和甲酸(体积比为0.1%)水溶液为流动相,采用2种梯度洗脱程序,经液相色谱分离后,质谱采用电喷雾电离源正离子模式,以各种胺类衍生化合物的选择离子[ M+H]+监测模式进行定性分析.试验发现,仪器检出限可达0.2 mg/L,可以用于胺类物质的快速定性检测.
展开▼
