摘要
应用反相高效液相色谱法(RP-HPLC)研究了5对L,D-多肽非对映异构体在不同条件下的分离情况。通过改换色谱柱、改变流动相的组成及梯度淋洗条件,发现其中的2对(Boc-Ala-L,D-Ala-GlyOBzl和Boc-Gly-L,D-Ala-ValOBzl)可以得到较好的分离,分离度分别为1.1和1.6,因此这2对L,D-多肽非对映异构体可以作为研究接肽反应消旋情况的模型体系。
he resolution of 5 pairs of L,D - peptide diastereoisomers( Boc-Phe-GlyOBzl and Boc - D - Phe -GlyOBzl; Boc -Ala -Ala-GlyOBzl and Boc-Ala-D-Ala-GlyOBzl Boc-Ala-Phe-GlyOBzlandBoc-Ala-D-Phe-GlyOBzl; Boc-Ala-Leu-GlyOBzl and Boc-Ala-D-Leu-GlyOBzl ;Boc-Gly-L, D-Ala-ValOBzl) were investigated with reversed-phase high performance liquid chromatography under different conditions. The columns: NovaPak C_(18) (150×3. gmm i. d.), μ Bondapak C_(18) (250 × 3.9mm i.d.)μ Bondapak CN(150×3. 9mm i. d.),μBondapak Phenyl (300 × 3. 9mm i. d.),Synchropak RP-P (250×4. 6mm i. d.).Mobile phases:(1) A:0.1 % TFA-H_2O, B: 0. 1% TFA-MeCNI (2) A: 0. 1% TPA-H_2O, B: 0.1% TFA-MeOH. Detector wave length: 214nm.The optimum conditions obtained are Synchropak RP-P column with 20%-60% (1)B as gradient eluent for Boc-Ala-L, D-Ala-GlyOBzl and Novapak C_(18)column with 30% (1 )B for Boc-Gly-L,D-Ala-ValOBzl. They were successively recognized into their chiralities respectively with 1. 1 and 1. 6 of resolution factors. It is recommended that the method can be applied to the racemzition study in peptide synthesis process.
出处
《色谱》
CAS
CSCD
北大核心
1996年第3期202-204,共3页
Chinese Journal of Chromatography
基金
国家"攀登"项目
关键词
高效液相色谱
多肽
非对映异构体
分离
high performance liquid chromatography, L,D-peptide, separation of diastereoisomers