糖类衍生物在毛细管区带电泳下的分离研究

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。

Separation of Derivatized Carbohydrates by Capillary Zone Electrophoresis

A simple and rapid method was developed for the separation of the labeled carbohydrates using 1-naphthyl-3-methyl-5- pyrazolone (NMP) as the derivatization reagent by capillary zone electrophoresis. A 58.5 cm × 50 μm i.d. (50 cm effective length) untreated fused-silica capillary is used. To optimize the conditions, the buffer solution concentration, pH, column temperature, voltage and other factors are evaluated. The results indicate that the buffer concentration and pH value exhibit a significant impact on the separation, but no obvious influences of the temperature, voltage and additives on resolution are observed. On the basis of the optimization, the optimal separation conditions are as follows: 55 mM borate buffer (pH 9.46), voltage of 22 kV, column temperature of 20 °C and DAD detection of 254 nm. The samples are introduced atmospherically with an injection time of 10 s. The results indicate that nine NMP-labeled carbohydrates can be separated with a good baseline resolution within 18 min under the conditions proposed. The Tangutoium Nitratia sample is also analyzed under the optimum conditions. The separation is efficient and rapid with satisfactory results.