毛细管电泳-柱端安培检测法用于抗癌药物2-氨基-6-巯基嘌呤和8-氮杂鸟嘌呤的研究

End-column Amperometric Detection of 2-amino-6-Mercapto-purine and 8-Azaguanine by Capillary Zone Electrophoresis

中文关键词:  2-氨基-6-巯基嘌呤,8-氮杂鸟嘌呤,毛细管区带电泳,柱端安培检测

英文关键词:2-amino-6-mercaptopurine,8-azaguanine,capillary zone electrophoresis,end-column amperometric detection

中文摘要:

      采用毛细管电泳－安培检测法建立一种简单、快速、有效的同时分析抗癌药物2-氨基-6-巯基嘌呤和8-氮杂鸟嘌呤的新方法.在长50 cm、内径为25 μm的未涂层毛细管中，采用 20 mmol/L磷酸盐(pH为7.0)缓冲液作为运行液，当分离电压为21 kV时，两组分在12 min内达到基线分离.在上述最佳分离条件下，当电极电位为1.050 V、进样时间为10 s时，2-氨基-6-巯基嘌呤和8-氮杂鸟嘌呤的峰电流和浓度之间呈良好的线性关系，其相关系数分别为0.999 2、0.999 0，检测限分别为3.0×10^-7、2.0×10^-7 mol/L. 7次重复实验2-氨基-6-巯基嘌呤和8-氮杂鸟嘌呤的日间峰电流RSD分别为2.44%、3.46% .利用该法检测了牛血清蛋白中的2-氨基-6-巯基嘌呤和8-氮杂鸟嘌呤，回收率分别为100%～113％，93.0～102％.

英文摘要:

      A end-column amperometric detection method with capillary electrophoresis for determination of 2-amino-6-mercaptopurine and 8-azaguanine has been established. A 50 cm length of 25 μm i. d., 360 o.d. μm uncoated fused-silica capillary was used. The detection conditions were optimized and the electrochemical behavior was observed. Under the optimal conditions: detection potential of 1.050 V (vs. Ag/AgCl), operating voltage of 21 kV, sample injection of 10 s at 21 kV and 20 mmol/L phosphate solution at pH 7.0 as buffer, the detection limits were 3.0×10^-7 and 2.0×10^-7 mol/L, and the calibration curve showed good linearity with r=0.9992 and r=0.9990 for 2-amino-6-mercaptopurine and 8-azaguanine, respectively. The daytime RSD of reproducibility for peak current was 2.44% and 3.46%, respectively. The method was successfully applied to determine serum samples. The recovery was found in the rang of 100%～113％ for 2-amino-6-mercaptopurine and 93.0%～102％ for 8-azaguanine, respectively.