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
L-硒-甲基硒代半胱氨酸是一种新型硒源类的食品营养强化剂,而D-硒-甲基硒代半胱氨酸的安全性尚没有相关研究,目前对于L-硒-甲基硒代半胱氨酸含量的测定方法多集中在测定硒-甲基硒代半胱氨酸含量,无法检测到其中L-硒-甲基硒代半胱氨酸的...L-硒-甲基硒代半胱氨酸是一种新型硒源类的食品营养强化剂,而D-硒-甲基硒代半胱氨酸的安全性尚没有相关研究,目前对于L-硒-甲基硒代半胱氨酸含量的测定方法多集中在测定硒-甲基硒代半胱氨酸含量,无法检测到其中L-硒-甲基硒代半胱氨酸的含量。本文建立了通过手性色谱柱分离、标准曲线法测定L-硒-甲基硒代半胱氨酸的高效液相色谱法(HPLC)。实验使用EC250/4NUCLEOSIL Chiral-1手性色谱柱(4 mm×250 mm,5μm),流动相为0.4mmol/L Cu SO4·5H2O水溶液,柱温为35℃,流速为1.0 m L/min,进样量为20μL,检测波长为240 nm;在该条件下L-硒-甲基硒代半胱氨酸的检测线性范围为0.541~1.352 mg/ml,线性相关系数R达0.9999,在线性范围内精密度和稳定性良好,平均回收率为97.73%。该方法操作简单,结果准确,可用于L-硒-甲基硒代半胱氨酸产品及其制品质量的监控。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.
文摘L-硒-甲基硒代半胱氨酸是一种新型硒源类的食品营养强化剂,而D-硒-甲基硒代半胱氨酸的安全性尚没有相关研究,目前对于L-硒-甲基硒代半胱氨酸含量的测定方法多集中在测定硒-甲基硒代半胱氨酸含量,无法检测到其中L-硒-甲基硒代半胱氨酸的含量。本文建立了通过手性色谱柱分离、标准曲线法测定L-硒-甲基硒代半胱氨酸的高效液相色谱法(HPLC)。实验使用EC250/4NUCLEOSIL Chiral-1手性色谱柱(4 mm×250 mm,5μm),流动相为0.4mmol/L Cu SO4·5H2O水溶液,柱温为35℃,流速为1.0 m L/min,进样量为20μL,检测波长为240 nm;在该条件下L-硒-甲基硒代半胱氨酸的检测线性范围为0.541~1.352 mg/ml,线性相关系数R达0.9999,在线性范围内精密度和稳定性良好,平均回收率为97.73%。该方法操作简单,结果准确,可用于L-硒-甲基硒代半胱氨酸产品及其制品质量的监控。
