糖类衍生物在毛细管区带电泳下的分离研究

Separation of Derivatized Carbohydrates by Capillary Zone Electrophoresis

以新合成的1-萘基-3-甲基-5-吡唑啉酮(NMP)为柱前衍生试剂,采用毛细管区带电泳模式考察并优化了糖类衍生物的分离条件。实验采用58.5cm×50μmi.d.毛细管(有效柱长50cm),55mmol/L硼酸盐缓冲溶液(pH9.46),柱温20℃,分离电压22kV,进样10s,在不加任何添加剂的情况下,高效、快速地实现了9种糖的基线分离,并在最优化条件下进行了唐古特白刺实际样品的分离分析,结果令人满意。

A simple and rapid method was developed for the separation of derivatized carbohydrates using 1-naphthyl-3-methyl-5-pyrazolone （NMP） as derivatization reagent by capillary zone electrophoresis. The detection was performed with diode array at 254 nm. A 58.5cm×50μm i.d. （50 cm effective length） untreated fused-silica capillary was used. To optimize the conditions, the background electrolyte concentration, buffer pH, column temperature, voltage and other factors were studied. It was found that the buffer concentration and pH value have a greater impact on the separation, but the influences of temperature, voltage and additives on resolution were not obvious follows ： 55 mmol/L borate buffer （ pH 9.46） On the basis of the optimization, the optimum conditions are as , voltage 22 kV, column temperature at 20℃ and detection at 254 nm. The samples were atmospherically introduced with an injection time of 10 s. The results indicate that 9 NMP-derivatized carbohydrates achieve baseline resolution within 18 min under the proposed conditions. The Tangufican Nitratia sample was also analyzed under the optimum conditions.