基于数学模型研究差示扫描量热法测量甘氨酸纯度  

Optimization of measurement of glycine purity using differential scanning calorimetry based on mathematical models

作　　者：贺雨欣 任鹏飞 刘祎晗 文武龙 刘铭 于洲波 杨婧[2] 王锐[1] HE Yuxin;REN Pengfei;LIU Yihan;WEN Wulong;LIU Ming;YU Zhoubo;YANG Jing;WANG Rui(College of Pharmacy,Heilongjiang University of Traditional Chinese Medicine,Harbin 150040;Basic Medical College,Heilongjiang University of Traditional Chinese Medicine,Harbin 150040)

机构地区：[1]黑龙江中医药大学药学院,哈尔滨150040 [2]黑龙江中医药大学基础医学院,哈尔滨150040

出　　处：《中国食品添加剂》2025年第4期101-107,共7页China Food Additives

基　　金：国家自然科学基金资助项目(82074271);国家自然科学基金资助项目(81603418);黑龙江优秀青年人才项目(2020YQ05)。

摘　　要：为确定差示扫描量热法(DSC)测定甘氨酸纯度的最佳工艺,进而寻找适合氨基酸类物质纯度测定的新方法,本文对差示扫描量热仪进行校正后,通过单因素试验考察气氛流速、升温速率和样品质量等因素对DSC测定甘氨酸纯度的影响,通过星点设计-效应面法得到最佳条件后对甘氨酸纯度进行验证试验,并与《中国药典》[9]电位滴定法的结果进行比较。结果显示DSC测定甘氨酸纯度的最佳工艺条件为:气氛流速为50mL/min,升温速率为20℃/min,称样质量为2.0 mg(精确至0.01 mg),在此条件下进行验证得出:DSC测得甘氨酸平均纯度为99.85%,RSD值为0.02%;电位滴定法测得甘氨酸平均纯度为99.84%,两种方法测试结果无显著性差异。因此DSC法可以应用于甘氨酸纯度的测定,且操作简单、耗时较短、重现性好,可作为氨基酸类物质纯度测定的新方法。In order to determine the optimal technology of determining the purity of glycine by differential scanning calorimetry(DSC),and tofind a new method suitable for amino acid substance purity testing,the DSC was calibrated,and the effects of factors such as atmosphere flow rate,heating rate and sample quality on the determination of glycine purity by DSC were investigated using single factor experiments.After obtaining the best conditions through a central composite design-response surface methodology,validation experiments of glycine purity were conducted and compared with the results from the potentiometric titration method as outlined in the“Chinese Pharmacopoeia”.The results indicated that the optimal conditions for measuring glycine purity using DSC were:atmosphericflow rate of 50 mL/min,heating rate of 20℃/min,and sample weight of 2.0 mg(accurate to 0.01 mg).Under these conditions,it was verified that the average purity of glycine measured by DSC was 99.85%with an RSD was 0.02%.The average purity of glycine measured by potentiometric titration was 99.84%,and there was no significant difference between the two methods.Therefore,the DSC method can be used to determine the purity of glycine,providing a simple,time-efficient and reproducible method,it can be used as a new method for purity assessment of amino acids.

关 键 词：差示扫描量热法 纯度 甘氨酸 星点设计-效应面 

分 类 号：TS207.3[轻工技术与工程—食品科学]