论文部分内容阅读
建立拆分氨甲喋呤(MTX)对映体的毛细管电泳方法, 讨论消旋药物MTX对映体立体选择的手性识别机理。运用聚丙酰胺涂渍毛细管的毛细管电泳方法,考察了缓冲液中添加α_CD、γ_CD、HP_β_CD和Me_β_CD对MTX的拆分。最佳拆分条件为pH 7.4磷酸盐缓冲液添加0.04 mmol/LHP_β_CD, 20 kV分离电压,柱温25℃, 280 nm紫外波长检测, 氨甲喋呤对映体基本上得到了基线分离。(+) MTX在18.18~636.16 mmol/L浓度范围, (-)MTX在45.44~636.16 mmol/L浓度范围内有良好的线性关系, 两对映体的定量下限(+)MTX为18.18 mmol/L, (-)MTX为45.44 mmol/L, 并用该方法测定了血清中MTX对映体含量, 计算了在不同CDs下两对映体的稳定常数, 结果表明MTX对映体和环糊精手性匹配与配合物的键合常数和选择因子(α)有关。
To establish a capillary electrophoresis method to separate the enantiomers of methotrexate (MTX), the chiral recognition mechanism of stereoselective MTX enantiomers was discussed. Capillary electrophoresis with polyacrylamide coated capillary was used to investigate the resolution of MTX by adding α_CD, γ_CD, HP_β_CD and Me_β_CD to the buffer solution. The optimum conditions for the separation of methotrexate enantiomers were baseline separation of enantiomers of methotrexate by adding 0.04 mmol / LHP_β_CD to pH 7.4 phosphate buffer at a voltage of 20 kV and a column temperature of 25 ° C at 280 nm. (+) MTX in the range of 18.18-636.16 mmol / L, the linear range of (-) MTX was in the range of 45.44-636.16 mmol / L, and the MTx of the two enantiomers was 18.18 mmol / L (-) MTX was 45.44 mmol / L, and the contents of MTX enantiomers in serum were measured by this method. The stability constants of two enantiomers under different CDs were calculated. The results showed that the enantiomers of MTX and cyclodextrin chiral The matching is related to the bonding constant of the complex and the selection factor (α).