目的建立毛细管电泳电化学技术(capillary electrophoresis with electrochemical detection,CE-ECD)检测人全血中同型半胱氨酸(homocysteine,Hcy)、半胱氨酸(cysteine,Cys)和还原型谷胱甘肽(reducedglutathione,GSH)的方法。考察缓冲...目的建立毛细管电泳电化学技术(capillary electrophoresis with electrochemical detection,CE-ECD)检测人全血中同型半胱氨酸(homocysteine,Hcy)、半胱氨酸(cysteine,Cys)和还原型谷胱甘肽(reducedglutathione,GSH)的方法。考察缓冲液的浓度、酸碱度、分离电压、进样时间和检测电压等参数对分离和检测的影响,确定最佳的实验条件。方法以直径为500μm的铂圆盘电极作为检测电极,用长度为50cm的熔融石英毛细管对一系列待检物标准溶液和人全血样本进行毛细管电泳电化学检测。结果在最优条件下,当电极电位为+1.05V(相对饱和甘汞电极)、分离电压为18kV时,Hcy、Cys和GSH于100mmol/L的磷酸盐缓冲液(pH7.8)中在10min内获得理想分离。检测下限(S/N=3)在0.29～0.80μmol/L范围内,且在3倍数量级浓度范围内,3种组分的浓度与峰电流呈良好线性关系。对0.5mmol/L的混合标准溶液连续检测7次,Hcy、Cys和GSH峰高的相对标准偏差(relative standard deviation,RSD)分别为3.7%、3.1%和2.9%。结论 CE-ECD方法可对Hcy、Cys和GSH等3种生物活性巯基化合物进行高效分离及检测,具有分析速度快、成本低、灵敏度高、试剂及样品用量小等优点,因此在生物医药领域具有广泛的应用前景。本实验采用的铂圆盘电极具有污染少、重复性好的特点。展开更多
Electrochemical extraction of contaminants from soils is a promising soil decontamination technology. Various experiments have been conducted to study electrochemical reactions and geochemical processes in the electro...Electrochemical extraction of contaminants from soils is a promising soil decontamination technology. Various experiments have been conducted to study electrochemical reactions and geochemical processes in the electrochemical extraction using different experimental apparatuses. This paper presents the development of a new closed two-dimensional(2D) apparatus that can better simulate the field application of the technology and accurately monitor the most important electrochemical parameters to understand the process. The innovative features of the new apparatus include the outer and inner electrodes designed to apply a non-uniform electrical field across the specimen as in the field electrochemical remediation process, the probes installed to measure the 2D distribution of electrical voltage, and the gas and fluid volume measurement devices used to accurately monitor the gas generation and electroosmotic flow rates at both electrodes as a function of time. The components of this new apparatus and the features of each component are described. The operating procedure and some typical results from three experiments with the apparatus are demonstrated. The results show that the variation of the gas generation rate is in good agreement with the electric current. Their relation provides a valid evaluation for electrochemical behavior of the system and Faraday's laws of electrolysis. The 2D profiles of cadmium concentration and voltage distribution at the end of the experiment reveal the great effects of a non-uniform electrical field on the contaminant mobilization.展开更多
文摘目的建立毛细管电泳电化学技术(capillary electrophoresis with electrochemical detection,CE-ECD)检测人全血中同型半胱氨酸(homocysteine,Hcy)、半胱氨酸(cysteine,Cys)和还原型谷胱甘肽(reducedglutathione,GSH)的方法。考察缓冲液的浓度、酸碱度、分离电压、进样时间和检测电压等参数对分离和检测的影响,确定最佳的实验条件。方法以直径为500μm的铂圆盘电极作为检测电极,用长度为50cm的熔融石英毛细管对一系列待检物标准溶液和人全血样本进行毛细管电泳电化学检测。结果在最优条件下,当电极电位为+1.05V(相对饱和甘汞电极)、分离电压为18kV时,Hcy、Cys和GSH于100mmol/L的磷酸盐缓冲液(pH7.8)中在10min内获得理想分离。检测下限(S/N=3)在0.29～0.80μmol/L范围内,且在3倍数量级浓度范围内,3种组分的浓度与峰电流呈良好线性关系。对0.5mmol/L的混合标准溶液连续检测7次,Hcy、Cys和GSH峰高的相对标准偏差(relative standard deviation,RSD)分别为3.7%、3.1%和2.9%。结论 CE-ECD方法可对Hcy、Cys和GSH等3种生物活性巯基化合物进行高效分离及检测,具有分析速度快、成本低、灵敏度高、试剂及样品用量小等优点,因此在生物医药领域具有广泛的应用前景。本实验采用的铂圆盘电极具有污染少、重复性好的特点。
基金Supported by the National Natural Science Foundation of China(41201303,20807028,41372262)the Fundamental Research for the Central Universities(14CX02052A,14CX02191A)+1 种基金the Qingdao Science and Technology Program for young scientists(14-2-4-86-jch)the State Key Laboratory of Pollution Control and Resource Reuse Foundation(PCRRF13023)
文摘Electrochemical extraction of contaminants from soils is a promising soil decontamination technology. Various experiments have been conducted to study electrochemical reactions and geochemical processes in the electrochemical extraction using different experimental apparatuses. This paper presents the development of a new closed two-dimensional(2D) apparatus that can better simulate the field application of the technology and accurately monitor the most important electrochemical parameters to understand the process. The innovative features of the new apparatus include the outer and inner electrodes designed to apply a non-uniform electrical field across the specimen as in the field electrochemical remediation process, the probes installed to measure the 2D distribution of electrical voltage, and the gas and fluid volume measurement devices used to accurately monitor the gas generation and electroosmotic flow rates at both electrodes as a function of time. The components of this new apparatus and the features of each component are described. The operating procedure and some typical results from three experiments with the apparatus are demonstrated. The results show that the variation of the gas generation rate is in good agreement with the electric current. Their relation provides a valid evaluation for electrochemical behavior of the system and Faraday's laws of electrolysis. The 2D profiles of cadmium concentration and voltage distribution at the end of the experiment reveal the great effects of a non-uniform electrical field on the contaminant mobilization.
