6种核磁共振法含量测定用标准物质纵向弛豫时间影响因素分析

Longitudinal relaxation influencing factors of six internal reference standards for quantitative nuclear magnetic resonance

目的:研究6种核磁共振法含量测定用标准物质(核磁定量内标物)纵向弛豫时间(T1)的影响因素。方法:使用Bruker AVANCE NEO 600 MHz核磁共振波谱仪,采用反转恢复法采集6种核磁内标物(对苯二酚、苯甲酸、富马酸、马来酸、对苯二甲酸二甲酯、1,3,5-三甲氧基苯)在不同溶剂(D2O、DMSO-d6、CD3OD、CDCl3)、不同浓度(1.25、2.5、5、10 mg·mL-1)以及不同温度(20、30、40、45℃)下的T1。结果:溶剂和温度对T1的影响显著,浓度对其影响不大。不同的核磁内标物在不同的化学环境(不同溶剂、不同浓度以及不同温度)中,T1不尽相同。结论:核磁定量内标物T1的影响因素研究结果,可以为定量核磁共振法中重要参数弛豫延迟时间(D1)的设置提供参考。

Objective:To study the longitudinal relaxation(T1)influencing factors of six internal reference standards for quantitative nuclear magnetic resonance spectroscopy(qNMR).Methods:The longitudinal relaxations of six internal reference standards for qNMR(hydroquinone,benzoic acid,fumaric acid,maleic acid,dimethyl terephthalate and 1,3,5-trimethoxybenzene)were determined by inversion recovery technique in different solvents(D2O,DMSO-d6,CD3OD,CDCl3),with the different concentrations(1.25,2.5,5,10 mg·mL-1)and at the different temperatures(20,30,40,45℃)using a Bruker AVANCE NEO 600 MHz nuclear magnetic resonance spectrometer.Results:The effect of solvent and temperature on T1 was significant,but that of concentration was not significant.The different internal reference standards had different T1 in different chemical environments(solvents,concentrations and temperatures).Conclusion:Research result for influencing factors of T1 and provides a reference for the setting of D1 which is an important parameter in qNMR.