柱前衍生-气相色谱法测定2-氯丙酸的光学纯度  

GC Determination of Optical Purity of 2-Chloropropionic Acid with Precolumn Derivatization

作　　者：赵接红[1,2,3] 李东[4] 王未鲜[1,2,3] 陈玉波[1,2,3] 熊金龙 

机构地区：[1]淮安市产品质量监督检验所,淮安223001 [2]江苏省盐化工产品质量监督检验中心,淮安223001 [3]国家盐化工产品质量监督检验中心(筹),淮安223001 [4]淮阴工学院生命科学与化学工程学院,淮安223003

出　　处：《理化检验（化学分册）》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)

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.

关 键 词：气相色谱法 柱前衍生 2-氯丙酸 光学纯度 

分 类 号：O657.7[理学—分析化学]