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25μm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 rnin内达到基线分离.在上述最佳分离条件下,当电极电位为1.050V、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%.
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.