摘要
纸色谱具有微量、快速、高效和灵活程度高等特点。以滤纸为原料用高碘酸钠氧化法合成了二醛基滤纸,通过希夫碱反应接枝手性氨基酸,合成了一种具有手性分离功能的新型纸色谱材料。通过单因素试验和正交试验确定滤纸氧化的最佳合成条件为:高碘酸钠的质量分数为4%,pH值为2,反应温度45℃和反应时间4 h,该条件下氧化滤纸醛基含量为57.93%(物质的量分数)。氧化滤纸与L-谷氨酸通过微波合成得到具有手性分离功能的色谱用纸。利用该种手性滤纸分离外消旋酒石酸,展开剂配方为100 mL 50%正丁醇,50 mL乙酸和0.100 0 g溴酚绿。结果显示,L-酒石酸比移值(R_f)为0.52,D-酒石酸Rf为0.40。该方法不需要使用大型设备,适合一般的教学、研究及工业应用。
Paper chromatography (PC) is a highly flexible, fast, and efficient separation method. In this study, a chromatographic paper with a chiral separation function was investigated and a paper chromatographic method for chiral separation was developed. Single-factor experiments and orthogonal tests were used to deter-mine the optimal oxidation conditions for filter paper. The optimal conditions were that sodium periodate 4%(mass percentage) , pH 2 buffer solution, reaction temperature 45 ^ , and reaction time 4 h. Under the optimal conditions, the aldehyde group content of a dialdehyde-based filter paper was 57. 93% (amount of substance percentage). A paper-based chiral separation material was synthesized by a microwave-assisted Schiff-base re-action of the oxidized filter paper with L-glutamic acid. The developing solvent for separating racemic tartaric acid using this chiral filter paper consisted of 100 mL of n-butanol, 50 mL of 50% (v/v) acetic acid, and 0. 100 0 g of bromophenol blue. The rate of flow ( Rf ) values of L-tartaric acid and D-tartaric acid were 0. 52 and 0. 40, respectively. This method does not require large-scale equipment to perform the chiral separation and it is there-fore suitable for general teaching, research, and industrial applications.
出处
《色谱》
CAS
CSCD
北大核心
2017年第9期912-917,共6页
Chinese Journal of Chromatography
基金
2013 Hubei Province Small and Medium-Sized Enterprises(SME) Technology Innovation Project(No.201319)
关键词
纸色谱
手性分离
双醛氧化滤纸
手性分离滤纸
希夫碱反应
paper chromatography (PC)
chiral separation
dialdehyde filter paper (DaFP)
chiral separation filter paper (CFP)
Schiff-base reaction