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以2,4-二硝基氟苯为衍生化试剂,建立柱前衍生化结合手性固定相高效液相色谱法拆分2-甲基哌嗪对映体的方法。采用Chiralpak IA(250 mm×4.6 mm,5μm)手性色谱柱,流动相为V(正己烷)∶V(无水乙醇)∶V(二乙胺)=50∶50∶0.1,检测波长261 nm,流速0.5 mL/min,柱温30℃。在此优化试验条件下,衍生后的对映体分离度达3以上,在0.15～1.5μg/mL浓度范围内线性关系良好,连续重复进样6次,相对标准偏差(RSD)在0.15%以下。该方法灵敏度高,重复性好,可用于2-甲基哌嗪异构体的质量控制。
Using 2,4-dinitrofluorobenzene as derivatization reagent, a method for the separation of 2-methylpiperazine enantiomers by precolumn derivatization combined with chiral stationary phase HPLC was established. Chiralpak IA (250 mm × 4.6 mm, 5 μm) chiral column was used with the mobile phase of V (n-hexane): V (absolute ethanol) , Flow rate 0.5 mL / min, column temperature 30 ℃. Under the optimized conditions, the derivatization enantiomeric resolution was above 3, with good linearity in the concentration range of 0.15 ~ 1.5μg / mL. The RSDs were continuously repeated for 6 times and the relative standard deviations (RSDs) were below 0.15% . The method has high sensitivity and good reproducibility and can be used for the quality control of 2-methylpiperazine isomers.