高效液相色谱法拆分α氨基酸的邻苯二甲酰衍生物对映体
高效液相色谱法,手性固定相,α氨基酸的邻苯二甲酰衍生物,对映体拆分,,高效液相色谱法,手性固定相,α氨基酸的邻苯二甲酰衍生物,对映体拆分,高效液相色谱法拆分α氨基酸的邻苯二甲酰衍生物对映体
摘 要 建立用高效液相色谱拆分α氨基酸的邻苯二甲酰衍生物对映体的方法。用多糖类手性固定相Chiralcel OD, Chiralpak AD, Chiralpak AS柱;5%异丙醇/正己烷(V/V)含0.1% 三氟醋酸溶液为流动相;流速为1 mL/min;检测波长:UV=254 nm。考察了α氨基酸的邻苯二甲酰衍生物在不同手性固定相(Chiralcel OD,Chiralpak AD,Chiralpak AS柱)上的对映体的手性分离。结果表明,α氨基酸的邻苯二甲酰衍生物对映体在Chiralcel OD柱上的分离效果最佳(α=1.34~2.11),并且全部得到了基线分离。关键词 高效液相色谱法,手性固定相,α氨基酸的邻苯二甲酰衍生物,对映体拆分
Enantiomer Resolution of NPhthaloyl αAmino Acids
by High Performance Liquid Chromatography
Lee Wonjae, Baek Chaesun, Jin Jingyu
(College of Pharmacy, Chosun University, Gwangju, 501759, Republic of Korea)
Abstract The Nphthaloyl(PHT) group for amino acids was attractive in certain instances, because it was often used for protecting moiety of primary amino group. And it can be readily removed under mild conditions of hydrazine reagents. In this study, the liquid chromatographic enantiomer separation of Nphthaloy protected αamino acids on three polysaccharidederived chiral stationary phases(CSPs), e.i. Chiralcel OD, Chiralpak AD and Chiralpak AS was performed. The chromatographic condition used on all CSPs was 5% 2propanol/hexane(V/V) containing 0.1% trifluoroacetic acid as the mobile phase at 1mL/min of flow rate and ultraviolet 254 nm detection. Chiralcel OD showed performance superior to other CSPs for resolution of Nphthaloyl αamino acids(α=1.34~2.11). The enantiomers of all examined Nphthaloyl αamino acids were baseline resolved on Chiralcel OD. The Lenantiomers of all analytes examined are preferentially retained on Chiralcel OD. It is expected that Chiralcel OD will be useful for enantiomer resolution of other Nphthaloyl protected αamino acids and related compounds. ......
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