A novel chiral stationary phase(CysCSP) for ligand exchange chromatography was prepared by firstly synthesizing N,S-di(2-hydroxyl-3-octoxyl)propyl-L-cysteine as chiral selector via reaction of L-cysteine with glycidyl...A novel chiral stationary phase(CysCSP) for ligand exchange chromatography was prepared by firstly synthesizing N,S-di(2-hydroxyl-3-octoxyl)propyl-L-cysteine as chiral selector via reaction of L-cysteine with glycidyl octyl ether and then coating it on YWG-C-{18} bonded stationary phase. The enantiomeric resolutions of some D,L-α-amino acids were achieved on CysCSP by using cupric acetate aqueous solution as the mobile phase, under the conditions of column temperature 20 ℃ and detection at UV 254 nm. The enantioselectivities α of D,L-α-amino acids separated were found to be in the range from 1.11 to 1.38 with the resolution R-s ranging from 1.1 to 2.8 and the column efficiency being from 5 000 to 9 000 n/m. The elution order of D-isomer before L-isomer was obersaved for all D,L-amino acids used.展开更多
利用实验室筛选得到的高立体选择性脂肪酶产生菌株溜曲霉(Aspergillus tamarii WYC3)不对称水解拆分N-BOC-DL-α-氨基丁酸甲酯得到N-BOC-L-α-氨基丁酸,对其反应条件进行研究,确定其最优反应条件为:0.1 mol/L p H 7.2的磷酸钾缓冲液,反...利用实验室筛选得到的高立体选择性脂肪酶产生菌株溜曲霉(Aspergillus tamarii WYC3)不对称水解拆分N-BOC-DL-α-氨基丁酸甲酯得到N-BOC-L-α-氨基丁酸,对其反应条件进行研究,确定其最优反应条件为:0.1 mol/L p H 7.2的磷酸钾缓冲液,反应温度30℃,底物浓度52.24 mmol/L,0.1 g菌粉,V(底物)∶V(丙酮)=1∶8,200 r/min恒温水浴反应6 h,可获得产物N-BOC-L-α-氨基丁酸,此时e.e._(s)值达到99.95%,对映体选择率E值为20.11,产率为36.21%。展开更多
文摘A novel chiral stationary phase(CysCSP) for ligand exchange chromatography was prepared by firstly synthesizing N,S-di(2-hydroxyl-3-octoxyl)propyl-L-cysteine as chiral selector via reaction of L-cysteine with glycidyl octyl ether and then coating it on YWG-C-{18} bonded stationary phase. The enantiomeric resolutions of some D,L-α-amino acids were achieved on CysCSP by using cupric acetate aqueous solution as the mobile phase, under the conditions of column temperature 20 ℃ and detection at UV 254 nm. The enantioselectivities α of D,L-α-amino acids separated were found to be in the range from 1.11 to 1.38 with the resolution R-s ranging from 1.1 to 2.8 and the column efficiency being from 5 000 to 9 000 n/m. The elution order of D-isomer before L-isomer was obersaved for all D,L-amino acids used.
