电解质溶液界面中移动氧化还原界面的理论建立、实验验证以及区带界面的应用性研究
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摘要
电解质溶液界面作为电化学的一个重要分支,已经成为分析化学领域的研究热点,特别是其中的移动化学反应界面和区带界面更是作为近十年的重点研究方向。本论文的研究工作主要集中在对电解质溶液界面中新型移动氧化还原界面的理论模型的初步创建、实验验证以及区带界面中毛细管区带电泳的应用性研究,具体研究内容如下:
1、移动氧化还原界面模型的初步建立
在本论文的第二章中,我们以移动化学反应界面(MCRB)为理论基础,结合以往已经研究成熟的其他反应界面,从一个简单的氧化还原反应出发(氧化剂为FeCl3,还原剂为KI),创新性的提出了移动氧化还原界面(MORB)的概念,建立了理论模型,并根据此模型进一步推导出了界面迁移的速度表达式,也是为移动化学反应界面理论做了一点拓展研究。
2、移动氧化还原界面模型的实验验证
在本论文的第三章中,我们紧紧围绕第二章中提出的移动氧化还原界面模型和界面迁移速度表达式进行了具体的大管实验验证,其结果与理论预测相符。验证结果显示:①施加电场后,能够清晰的观察到氧化剂FeCl3与还原剂KI之间形成的移动氧化还原界面。②氧化剂与还原剂的浓度比在界面迁移速度和方向上发挥着重要作用,通过改变二者之间的浓度配比可以控制界面的迁移速度。③通过理论推导出的界面迁移公式,理论预测的各参数对界面速度的影响和实验结果相符。以上结果都证明了理论模型和公式的正确性,也为今后的深入研究提供了坚实的理论基础。
3、应用毛细管区带电泳分离灵芝发酵菌丝体中灵芝酸相似物
在本论文的第四章中,我们基于区带界面中最常用的毛细管区带电泳作为分析方法,完成了对灵芝发酵菌丝体中多种灵芝酸同系物的同步分离与定量检测。在最终优化的最佳的实验条件下,当以245 nm为检测波长,甘草次酸为内标时,四种灵芝酸在9分钟左右即可达到基线分离。所有物质的标准曲线均呈较好的线性关系(r2 >0.9958),检测限(LOD)和定量限(LOQ)分别低于0.6和1.8μg mL-1,精密度和回收率的相对标准偏差均低于5%,回收率在91.4%到103.6%之间。所有实验结果表明,我们建立的这种方法真实、有效,为灵芝酸同系物的分离提供了一种可供选择的分析方法。
As one of the important branches of electrochemistry, the electrolyte solution boundary has become a very hot topic in analytical chemistry, among them moving chemical reaction boundary (MCRB) and zone boundary have come to be the main development trend in recent 10 years. The main work of this paper is focus on the establishment and verification of the newly moving oxidation-reduction boundary (MORB) and the application study of the capillary electrophoresis. The main points of this thesis are summarized as follows:
1、Preliminary establishment of the moving oxidation-reduction boundary.
In Chapter 2, based on the concept of MCRB and along with the previous research of other reaction boundary, a model of moving oxidation-reduction boundary was created by the common oxidant and reductant: FeCl3 and KI. Thus the model of MORB was established. From the MORB model, the expression of the velocity of MORB was deducted.
2、Experimental verification of MORB.
In Chapter 3, to avoid getting the parameters difficult to obtain required in the calculations involved and simplify the computation, a very convenient and efficient data processing method was worked out to validate the model and expression of MORB which submitted in Chapter 2. The experimental results well accord with the prediction, they showed:①The MORB between FeCl3 and KI could be observed clearly between oxidant and reductant by an electric field applied to the large tube.②The ratio of the concentrations of the oxidant and reductant played an important role in the migration of the boundary, and the velocity of the MORB could be controlled by changing the concentration ratio of the oxidant and reductant.③By the expressions of the theory, the influence on the parameters of the velocity were well accord with the predicted ones, which could prove the correctness of the MORB model and expression. Our work was hoped to offer a solid theory foundation and pave a way for further studies.
3、Analysis of four ganoderic acids from fermentation mycelia powder of Ganoderma lucidum by capillary zone electrophoresis (CZE)
In Chapter 4, a simple and reliable method was developed for the separation and quantitative determination of four ganoderic acids(GAs) from dried triterpene-enriched extracts of Ganoderma lucidum mycelia powder by CZE which was the most commonly used analysis method in zone boundary. Under the optimum conditions, the four GAs reached the baseline separation in 9 min with Glycyrrhetinic acid (GTA) as internal standard. The four GAs and internal standard (GTA) were detected at a wavelength 245 nm. All calibration curves showed good linearity (r2 >0.9958) within test ranges. Limit of detection (LOD) and limit of quantification (LOQ) were less than 0.6 and 1.8μg mL-1, respectively. The relative standard deviation (R.S.D.) values of precision and recoveries was less than 5% and recoveries ranged from 91.4% to 103.6%. It showed that the developed method was effective and stably, it could be regarded as an alternative method for the analysis of the four GAs.
1、移动氧化还原界面模型的初步建立
在本论文的第二章中,我们以移动化学反应界面(MCRB)为理论基础,结合以往已经研究成熟的其他反应界面,从一个简单的氧化还原反应出发(氧化剂为FeCl3,还原剂为KI),创新性的提出了移动氧化还原界面(MORB)的概念,建立了理论模型,并根据此模型进一步推导出了界面迁移的速度表达式,也是为移动化学反应界面理论做了一点拓展研究。
2、移动氧化还原界面模型的实验验证
在本论文的第三章中,我们紧紧围绕第二章中提出的移动氧化还原界面模型和界面迁移速度表达式进行了具体的大管实验验证,其结果与理论预测相符。验证结果显示:①施加电场后,能够清晰的观察到氧化剂FeCl3与还原剂KI之间形成的移动氧化还原界面。②氧化剂与还原剂的浓度比在界面迁移速度和方向上发挥着重要作用,通过改变二者之间的浓度配比可以控制界面的迁移速度。③通过理论推导出的界面迁移公式,理论预测的各参数对界面速度的影响和实验结果相符。以上结果都证明了理论模型和公式的正确性,也为今后的深入研究提供了坚实的理论基础。
3、应用毛细管区带电泳分离灵芝发酵菌丝体中灵芝酸相似物
在本论文的第四章中,我们基于区带界面中最常用的毛细管区带电泳作为分析方法,完成了对灵芝发酵菌丝体中多种灵芝酸同系物的同步分离与定量检测。在最终优化的最佳的实验条件下,当以245 nm为检测波长,甘草次酸为内标时,四种灵芝酸在9分钟左右即可达到基线分离。所有物质的标准曲线均呈较好的线性关系(r2 >0.9958),检测限(LOD)和定量限(LOQ)分别低于0.6和1.8μg mL-1,精密度和回收率的相对标准偏差均低于5%,回收率在91.4%到103.6%之间。所有实验结果表明,我们建立的这种方法真实、有效,为灵芝酸同系物的分离提供了一种可供选择的分析方法。
As one of the important branches of electrochemistry, the electrolyte solution boundary has become a very hot topic in analytical chemistry, among them moving chemical reaction boundary (MCRB) and zone boundary have come to be the main development trend in recent 10 years. The main work of this paper is focus on the establishment and verification of the newly moving oxidation-reduction boundary (MORB) and the application study of the capillary electrophoresis. The main points of this thesis are summarized as follows:
1、Preliminary establishment of the moving oxidation-reduction boundary.
In Chapter 2, based on the concept of MCRB and along with the previous research of other reaction boundary, a model of moving oxidation-reduction boundary was created by the common oxidant and reductant: FeCl3 and KI. Thus the model of MORB was established. From the MORB model, the expression of the velocity of MORB was deducted.
2、Experimental verification of MORB.
In Chapter 3, to avoid getting the parameters difficult to obtain required in the calculations involved and simplify the computation, a very convenient and efficient data processing method was worked out to validate the model and expression of MORB which submitted in Chapter 2. The experimental results well accord with the prediction, they showed:①The MORB between FeCl3 and KI could be observed clearly between oxidant and reductant by an electric field applied to the large tube.②The ratio of the concentrations of the oxidant and reductant played an important role in the migration of the boundary, and the velocity of the MORB could be controlled by changing the concentration ratio of the oxidant and reductant.③By the expressions of the theory, the influence on the parameters of the velocity were well accord with the predicted ones, which could prove the correctness of the MORB model and expression. Our work was hoped to offer a solid theory foundation and pave a way for further studies.
3、Analysis of four ganoderic acids from fermentation mycelia powder of Ganoderma lucidum by capillary zone electrophoresis (CZE)
In Chapter 4, a simple and reliable method was developed for the separation and quantitative determination of four ganoderic acids(GAs) from dried triterpene-enriched extracts of Ganoderma lucidum mycelia powder by CZE which was the most commonly used analysis method in zone boundary. Under the optimum conditions, the four GAs reached the baseline separation in 9 min with Glycyrrhetinic acid (GTA) as internal standard. The four GAs and internal standard (GTA) were detected at a wavelength 245 nm. All calibration curves showed good linearity (r2 >0.9958) within test ranges. Limit of detection (LOD) and limit of quantification (LOQ) were less than 0.6 and 1.8μg mL-1, respectively. The relative standard deviation (R.S.D.) values of precision and recoveries was less than 5% and recoveries ranged from 91.4% to 103.6%. It showed that the developed method was effective and stably, it could be regarded as an alternative method for the analysis of the four GAs.
引文
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