节点文献
反相高效液相色谱法拆分谷氨酸和天门冬氨酸对映体
RP-HPLC chiral separations of glutamic acid and aspartic acid
【摘要】 目的:建立 HPLC 法拆分了谷氨酸(Glu)和天门冬氨酸(Asp)对映体的方法。方法:本文利用邻苯二甲醛(OPA)柱前衍生,以β-环糊精(β-CD)为手性添加剂,乙腈-缓冲溶液(0.02mol·L-1醋酸钠:三乙胺=100:0.018,)为流动相,检测波长为330nm。考察了不同色谱柱、缓冲溶液 pH、β-环糊精浓度、流动相比例和柱温对分离的影响。优化的色谱条件为:色谱柱为 Hypersil AA-ODS,分离温度40℃,流动相为乙腈-缓冲溶液(0.02mol·L-1醋酸钠:三乙胺=100:0.018,用2%醋酸调pH 7.2,其中含6mmol·L-1β-CD)=1:99。结果:在优化的色谱条件下,上述两种氨基酸对映体均得到基线分离。结论:所建立的方法简便、快速、分离度高。
【Abstract】 Objective:To establish a method for the chiral separations of glutamic acid(Glu)and aspartic acid (Asp)by high performance liquid chromatography(HPLC).Method:The amino acids were derivatized with o- phthaladehyde(OPA)before separations.β-CD was used as a chiral mobile phase additive.The mobile phase was acetonitrile-buffer solution [0.02 mol·L-1NaAc-(CH3CH2)3 N=100:0.018].The detective wavelength was 330 nm.The influences of colums,the composition of mobile phase,pH,the concentration of β-CD and colum temperature on the enantiomerie separations of Glu and Asp were investigated.The optimized chromatographic con- ditions for the separations were at 40℃ on a Hypersil AA-ODS colum and the mobile phase was acetonitrile- buffer solution [0.02 mol·L-1NaAc-(CH3 CH2)3 N=100:0.018,adjusting to pH=7.2 with 2% HAc and con- taining 6 mmol·L-1β-CD](1:99)at a flow rate of 0.45 mL·min-1.Results:Under the chromatographic con- ditions,baseline separations of these enantiomers could be obtained.Conclusion:The method was simple,rapid with high resolutions.
- 【文献出处】 药物分析杂志 ,Chinese Journal of Pharmaceutical Analysis , 编辑部邮箱 ,2006年06期
- 【分类号】R917
- 【被引频次】1
- 【下载频次】177