摘要
用2,4-二硝基苯肼进行柱前衍生,建立了高效液相色谱同时测定聚醚多元醇中甲醛、乙醛、丙烯醛、丙酮和丙醛的方法,考察了衍生反应时间、温度及衍生试剂体积对反应的影响。结果表明,该方法检出限为0. 015~0. 25 mg/kg,线性相关系数R≥0. 9998。样品测定精密度为1. 03%~2. 75%,加标回收率为91. 0%~106. 7%。该方法已成功地用于实际样品检测,解决了聚醚多元醇中丙烯醛和丙酮分离的技术难题,具有线性范围宽,精密度好,回收率高等优点。
A high performance liquid chromatography(HPLC)method based on the 2,4-dinitrophenylhydrazine(DNPH)as pre-derivatization agent was developed for the determination of formaldehyde,acetaldehyde,acraldehyde,acetone and propionaldehyde.The influences of derivatization time,temperature and reagent volume were tested.Results indicated that the range of detection limit was 0.015~0.25 mg/kg,the correlative coefficients of linear regression function for aldehydes and acetone were all higher than 0.9998.Furthermore,the relative standard deviation for determination of samples was 1.03%~2.75% and the recovery rate was 91.0%~106.7%.Finally,the proposed method with wide measurement range,good precision and high recovery rate,was successfully applied to the analysis of polyether polyol samples,and it solved the separation problem of acraldehyde and acetone.
作者
吴肖肖
王榕
朱洁
李宁
张聪丽
张驰
WU Xiaoxiao;WANG Rong;ZHU Jie;LI Ning;ZHANG Congli;ZHANG Chi(Jiangsu Center of Supervision & Testing on Green Degradable Material Quality,Nanjing Institute of Supervision & Testing on Product Quality, Nanjing 210019, Jiangsu, China;Key Laboratory of Child Development and Learning Science (Ministry of Education),School of Biological Sciences & Medical Engineering, Southeast University, Nanjing 210096, Jiangsu, China;Jinqi Chemical Groups, Nanjing 210047, Jiangsu, China)
出处
《聚氨酯工业》
北大核心
2018年第6期41-44,共4页
Polyurethane Industry
基金
国家重点研发计划项目(2018YFF0215200)
国家质量监督检验检疫总局科技计划项目(2015QK055)
江苏省质量技术监督局科技项目(KJ168383
KJ168373
KJ185613)
关键词
高效液相色谱
聚醚多元醇
醛
丙酮
同时测定
high performance liquid chromatography (HPLC)
polyether polyol
aldehyde
acetone
simultaneous determination