差示扫描量热熔点分析法的应用性分析  

Applicability Studies of Differential Scanning Thermal Melting Point Analysis

作　　者：吴锐 林兰[2] 严菁[2] 刘万卉[1] 刘毅[2] WU Rui;LIN Lan;YAN Jing;LIU Wan-hui;LIU Yi(School of Pharmacy,Yantai University,Yantai 264005,China;National Institutes for Food and Drug Control,Beijing 102629,China)

机构地区：[1]烟台大学药学院,山东烟台264005 [2]中国食品药品检定研究院,北京102629

出　　处：《化学试剂》2020年第3期285-290,共6页Chemical Reagents

基　　金：中国食品药品检定研究院学科带头人培养基金资助项目(2015X3)。

摘　　要：选择不同温度段熔融的5个代表性品种、国内外不同来源的13个法定熔点标准物质作为研究对象,进行差示扫描量热法和毛细管法两种熔点分析方法的关联性研究,并进一步开展差示扫描量热熔点分析法关键参数的应用性分析。研究表明,毛细管法的熔点分析结果一般延后1~2℃;差示扫描量热熔点分析法的准确性和精密度更好,并且推荐采用10℃/min的升温速率参数,而升温起点、气体流量等方法参数影响较小。质量分析还证实,我国药典熔点标准物质已经具备国际竞争力。The purpose of this work was to evaluate the correlation of differential scanning calorimetry(DSC) and capillary method as melting point measurements.The objects included thirteen official chemical reference substances(CRS) for melting point from different domestic and foreign sources,representing five CRS categories of different melting temperature ranges.Applicability analysis was further carried out on the key parameters of DSC melting point measurement.The results demonstrated that melting points analyzed by capillary method were generally delayed by 1~2 ℃,and that the accuracy and precision of DSC method were better.The DSC melting point analysis was recommended as the preferred method with heating rate of 10 ℃/min as basic parameter value of DSC method.Impacts of other parameters such as initial temperature and gas flow rate were not significant.Quality assessment also indicated that the Chinese official CRS for melting point were comparable to current international CRS.

关 键 词：熔点 差示扫描量热法 毛细管法 升温速率 化学标准物质 

分 类 号：R917[医药卫生—药物分析学]