摘要
建立折光率-HPLC联合应用测定连续丁酮肟化反应中关键组分含量的分析方法。结果表明,折光率法检测速度快,检测通量高,适用于过程检测;HPLC法检测结果准确度高,有助于物料衡算与产品质量控制;由于杂质影响,折光率法的测定结果略低于HPLC法,但不影响工艺过程的判断。折光率法与HPLC法进行方法学验证。折光率法用标准曲线法进行定量,丁酮肟精密度的RSD小于2.0%,回收率在98.03%~99.08%之间,均符合要求;HPLC法采用双波长同时测定丁酮肟与丁酮,方法验证结果表明,HPLC法的专属性、线性关系均良好,丁酮与丁酮肟的精密度结果小于2.0%,丁酮肟与丁酮回收率均在99.5%~101.0%之间,均符合要求。将折光率法与HPLC法相结合,既适用于连续肟化反应的快速检测,又适用于各物料的具体组成,为工艺的调整与丁酮肟产品的质量控制提供有利的数据支撑。
The analytical method for the detection of key components during butanone oxime reaction by combining refractive index and HPLC was established.The results showed that the refractive index method had fast detection speed and high detection flux which;HPLC method had high accuracy,which was helpful for material accounting and product quality control;Due to the influence of impurities,the measurement results of the refractive index method was slightly lower than those of the HPLC method,which didn’t affect the inspection and judgment of the continuous process.Methodological validation of refractive index method and HPLC method.The refractive index method adopted the standard curve method for quantification,and the precision RSD of butanone oxime was less than 2.0%and the recovery rate was within the range of 98.03%to 99.08%,both of which met the requirements.The results showed that the specificity and linear relationship of the HPLC method were excellence.The precision of butanone and butanone oxime was less than 2.0%,and the recovery rates of butanone oxime and butanone were both in the range of 99.5%to 101.0%,which met the requirements.The combination of refractive index method and HPLC method was suitable for both rapid detection of continuous reaction solution and specific composition of various materials,providing favorable data support for process adjustment and product quality control.
作者
王艳
赵相柱
杨旭
高爱红
岳涛
WANG Yan;ZHAO Xiang-zhu;YANG Xu;GAO Ai-hong;YUE Tao(Qingdao University of Science&Technology,Jinan 250014,China)
出处
《化学工程师》
2025年第2期82-87,共6页
Chemical Engineer
基金
山东省政府“泰山学者”建设工程资金项目(08190201)。
关键词
折光率
HPLC
连续丁酮肟化反应
丁酮肟
丁酮
refractive index
HPLC
continuous butanone oximation reaction
butanone oximation
butanone
