A new capillary electrophoresis apparatus was designed. Piezoelectric ceramics transformer technology was first applied in capillary electrophoresis, a high voltage and stable source was made. Amperometric detector wa...A new capillary electrophoresis apparatus was designed. Piezoelectric ceramics transformer technology was first applied in capillary electrophoresis, a high voltage and stable source was made. Amperometric detector was used in which the working electrode was closely opposite to the end of capillary. The apparatus was characterized in good reproducibility, safety and very low cost.展开更多
在制备6-磷酸甘露糖过程中,将6-磷酸甘露糖与磷酸根杂质分开是纯化过程和建立质量标准的重要环节。本文建立了6-磷酸甘露糖和磷酸根的离子色谱分离-电化学检测方法。样品经溶解、过滤后进行色谱分析,以Ion-Pac AG18离子交换柱(50 m m...在制备6-磷酸甘露糖过程中,将6-磷酸甘露糖与磷酸根杂质分开是纯化过程和建立质量标准的重要环节。本文建立了6-磷酸甘露糖和磷酸根的离子色谱分离-电化学检测方法。样品经溶解、过滤后进行色谱分析,以Ion-Pac AG18离子交换柱(50 m m×4 m m)为保护柱,在Io npac AS18离子交换色谱柱(250 m m×4 m m)上分离,以25 m m o l/L氢氧化钾溶液为流动相,等度淋洗,流速1.0 m L/m in,安培检测器和电导检测器串联检测,外标法定量。先使用安培检测器检测,在碱性条件下,6-磷酸甘露糖在安培检测器上被选择性检出;后使用电导检测器检测,经ASRS型抑制器抑制背景电导后,6-磷酸甘露糖和磷酸根同时被电导检测器检出,二者分离度良好。采用安培检测器检测时,进样量为25μL,6-磷酸甘露糖的线性范围为0.06～10.00 mg/L,相关系数为0.999 8,回收率为92.1%～103.1%,相对标准偏差均小于3%,检出限(以信噪比为3计)为0.02 m g/L。该方法灵敏度高,无杂质干扰,前处理简便,可用于原料药合成中间体的检测,结果令人满意。展开更多
A carbon wire amperometric flow through detector is described which is easily constructed at low cost for application to flow injection analysis,continuous stream analysis and liquid chromatography.The theoretical lim...A carbon wire amperometric flow through detector is described which is easily constructed at low cost for application to flow injection analysis,continuous stream analysis and liquid chromatography.The theoretical limiting current of the detector is 2.14×10~6nCD^(2/3)u_f^(1/3) with 36% actual current efficiency.By use of flow injection analysis,the detecting limits for Ag(I)and Cr(VI)had achieved 1 ppb and 0.4 ppb respectively with 1.2%(n=20)relative standard deviation after preliminary experiments.展开更多
文摘A new capillary electrophoresis apparatus was designed. Piezoelectric ceramics transformer technology was first applied in capillary electrophoresis, a high voltage and stable source was made. Amperometric detector was used in which the working electrode was closely opposite to the end of capillary. The apparatus was characterized in good reproducibility, safety and very low cost.
文摘在制备6-磷酸甘露糖过程中,将6-磷酸甘露糖与磷酸根杂质分开是纯化过程和建立质量标准的重要环节。本文建立了6-磷酸甘露糖和磷酸根的离子色谱分离-电化学检测方法。样品经溶解、过滤后进行色谱分析,以Ion-Pac AG18离子交换柱(50 m m×4 m m)为保护柱,在Io npac AS18离子交换色谱柱(250 m m×4 m m)上分离,以25 m m o l/L氢氧化钾溶液为流动相,等度淋洗,流速1.0 m L/m in,安培检测器和电导检测器串联检测,外标法定量。先使用安培检测器检测,在碱性条件下,6-磷酸甘露糖在安培检测器上被选择性检出;后使用电导检测器检测,经ASRS型抑制器抑制背景电导后,6-磷酸甘露糖和磷酸根同时被电导检测器检出,二者分离度良好。采用安培检测器检测时,进样量为25μL,6-磷酸甘露糖的线性范围为0.06～10.00 mg/L,相关系数为0.999 8,回收率为92.1%～103.1%,相对标准偏差均小于3%,检出限(以信噪比为3计)为0.02 m g/L。该方法灵敏度高,无杂质干扰,前处理简便,可用于原料药合成中间体的检测,结果令人满意。
基金This Project is supported by the National Science Foundation of China
文摘A carbon wire amperometric flow through detector is described which is easily constructed at low cost for application to flow injection analysis,continuous stream analysis and liquid chromatography.The theoretical limiting current of the detector is 2.14×10~6nCD^(2/3)u_f^(1/3) with 36% actual current efficiency.By use of flow injection analysis,the detecting limits for Ag(I)and Cr(VI)had achieved 1 ppb and 0.4 ppb respectively with 1.2%(n=20)relative standard deviation after preliminary experiments.
