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目的建立手性配体高效液相色谱法对肌肽对映体进行拆分。方法在Phenomenex chirex 3126手性色谱柱上,以硫酸铜为手性配体流动相,考察了进样量、流动相有机添加剂、流速、柱温、Cu2+浓度等因素下肌肽色谱拆分行为和热力学特性,并初步探讨了溶质在配体手性柱上的识别机制。结果检测波长在254nm,流动相为2mmol.L 1CuSO4水溶液-乙腈(96∶4),流速1.0mL.min-1可实现肌肽对映体的基线分离。其在色谱柱分离的焓变差值ΔΔHo与熵变差值ΔΔSo对手性识别都有贡献,拆分过程为焓控过程。其中L-肌肽与手性配体及Cu2+形成的络合物呈现出不稳定性,与典型的构像异构色谱行为一致。结论肌肽对映体可采用手性配体色谱法实现基线分离,其中L-肌肽形成的配位体具不稳定性。
OBJECTIVE To establish a chiral ligand high performance liquid chromatographic method for the separation of carnosine enantiomers. Methods The mobile phase of chiral ligand was prepared on a Phenomenex chirex 3126 chiral column. The chromatographic behavior and thermodynamics of carnosine were investigated under the conditions of injection volume, mobile phase organic additives, flow rate, column temperature and Cu2 + concentration. The mechanism of solute recognition on ligand chiral columns was also discussed. Results Baseline separation of the carnosine enantiomers was achieved with a detection wavelength of 254 nm and a mobile phase of 2 mmol·L-1 CuSO4-acetonitrile (96: 4) at a flow rate of 1.0 mL · min-1. Its enthalpy difference ΔΔHo and entropy change ΔΔSo on the chromatographic separation contribute to the chiral recognition. The resolution process is enthalpy control. Among them, L-carnosine exhibited complex interactions with chiral ligands and Cu2 + complexes, consistent with typical conformational isomeric chromatographic behavior. Conclusion The carnosine enantiomers can be separated by chiral ligand chromatography. The L-carnosine ligands are unstable.