摘要
提出了柱前衍生-气相色谱法测定2-氯丙酸的光学纯度。在无水硫酸镁存在下,相同体积的2-氯丙酸与二氯亚砜在冰浴中进行衍生反应30 min,所得2-氯丙酸衍生物2-氯丙酸甲酯消旋体经CYCLOSIL-B手性气相色谱柱分离,柱温为65℃。R-(+)-2-氯丙酸甲酯和S-(-)-2-氯丙酸甲酯的分离度大于2.0。方法用于2-氯丙酸光学纯度的测定,所得测定值与理论值基本一致。
A method of GC for the determination of optical purity of 2-chloropropionic acid with precolumn derivatization was proposed. 2-Chloropropionic acid was mixed with same volume of the derivatizing reagent thionyl chloride, and derivatized for 30 min in an ice bath. The derivative of 2-chloropropionic acid, racemate of methyl 2 chloropropionate, obtained was separated on CYCLOSIL-B chiral column at 65℃. The resolution of more than 2.0 was attained. The present method was used in the determination of optical putity of 2-ehloropropionic acid, and the results obtained were in conformity with the theoretical values.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2011年第9期1034-1036,1039,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家质检总局科技计划项目(2009QK166)
关键词
气相色谱法
柱前衍生
2-氯丙酸
光学纯度
GC
Precolumn derivatization
2-Chloropropionic acid
Optical purity
