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机构地区:[1]食品安全分析与检测技术教育部重点实验室福州大学运动科学研究中心,福建福州350002
出 处:《分析测试技术与仪器》2007年第1期17-21,共5页Analysis and Testing Technology and Instruments
基 金:福建省重大专项;国家自然科学基金(20675016);福建省科技厅自然科学基金(B0510006);福州大学科技发展基金(2004XQ208)资助项目
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 min内达到基线分离.在上述最佳分离条件下,当电极电位为1.050V、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 20、.999 0,检测限分别为3.0×10-7、2.0×10-7mol/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.
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
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