高效毛细管电泳法测定食品和药物中的活性成分

发布时间：2018-05-15 21:45

本文选题：高效毛细管电泳 + 沙棘　；参考：《山西师范大学》2017年硕士论文

【摘要】：进入21世纪,随着人类生活水平的提高,人们对于健康和养生的关注度也逐渐提高,在确保食品安全的前提下,人们更多的希望通过食疗来调节自身的机能,在满足基本营养的同时也能祛除疾病。因此对于食品和药物中有效成分的分析研究成为当下的热点。在众多的分析检测技术中,毛细管电泳以其较高的分离效率,较短的分析时间,较低的成本消耗等优势广受分析检测实验的欢迎,是发现并解决各自研究领域中一些新问题的得力工具。本论文主要应用高效毛细管电泳-紫外吸收检测器对食品和药物中有效成分进行检测研究,具体内容如下:第一章:主要对高效毛细管电泳及其应用作出简单的综述。在技术方面包括高效毛细管电泳的发展情况,基础分离理论,分离模式,进样技术,信号检测方式及其特点等。在了解技术的基础上,本章对高效毛细管电泳技术在不同领域的应用进行简要概括,并对本论文研究的意义做出总结。第二章:应用高效毛细管区带电泳法,对3个产地沙棘果粉中的芦丁、山柰酚、异鼠李素和槲皮素4种活性物质进行同时分离测定。考察了影响电泳分离效率的各种条件:缓冲溶液20 mmol/L Na2B4O7-H3BO3,1.5 mg/m L的β-环糊精,pH 9.55,检测波长370 nm,分离电压25 kV,进样时间5 s。芦丁、山柰酚、异鼠李素和槲皮素4种活性物质在11 min内实现较好分离,线性范围分别为0.01~0.51、0.05~0.93、0.02~0.65、0.03~0.81mg/mL,相关系数r在0.9971~0.9991之间,检出限分别为5.05×10-5、2.10×10-5、3.75×10-5、1.31×10-5mg/mL(RSN=3),各物质线性关系良好。日内及日间精密度的范围是0.08%~4.72%,平均回收率在95.51%~104.66%之间,RSD%不大于3.92%(n=3)。在优化条件下,对4种活性物质标准品的混合物进行测定,并用相同的方法对3个产地沙棘果粉中活性物质的提取液进行检测。结果表明:生产地不同的沙棘中,4种被检测化合物的含量各不相同。沙棘中被测4种化合物总量最高的产自新疆乌鲁木齐,最低的产自甘肃武威,而槲皮素含量以产自山西吕梁的最高,山柰酚和异鼠李素以产自新疆乌鲁木齐最高。通过应用该方法进行检测,可以实现沙棘果粉中多种黄酮类物质的快速分离。第三章:利用高效毛细管电泳法,对苹果中根皮苷,表儿茶素,芦丁,绿原酸4种酚类化合物进行分离与测定。优化了实验条件,最佳实验条件:缓冲溶液10 mmol/L Na2B4O7-H3BO3,pH 9.2,检测波长280 nm,分离电压25 kV,进样时间5 s。其线性范围分别为0.005~0.120、0.005~0.550、0.004~0.450、0.020~0.600 mg/m L,相关系数r在0.9977~0.9992之间,最低检出限分别为3.41×10-5、5.67×10-5、3.78×10-5、3.89×10-5mg/m L(S/N=3)。之后,又进行了日内及日间精密度和平均回收率的试验,其范围分别为0.13%~4.59%和96.72%~104.55%,RSD%≤3.74%(n=3)。在优化条件下,对所检测酚类化合物标准品的混合物进行测定,并用相同的方法测定苹果皮和苹果肉样品提取液。实验结果表明,本方法操作简便、准确可靠,可作为苹果中多种酚类物质质量检测的一种手段。第四章:以高效毛细管电泳-紫外检测技术为基础,研究了决明子中5种蒽醌类化合物的毛细管电泳迁移情况,通过优化实验条件,分析各种影响因素,并对所测对照品和供试品进行定性和定量分析,最终确定最佳分离条件为:检测波长284 nm,分离电压25 kV,进样时间5 s,运行缓冲溶液Na2B4O7-H3BO3浓度20 mmol/L,pH 8.50,β-环糊精浓度为5 mmol/L,在该条件下,橙黄决明素,大黄素,大黄素甲醚,大黄酸,大黄酚在10 min内实现分离,线性范围依次为0.005~0.400、0.004~0.350、0.004~0.400、0.002~0.350、0.003~0.300 mg/mL,线性相关系数r大于0.9952,检出限分别为5.03×10-5、5.66×10-5、1.67×10-5、5.19×10-5、3.36×10-5mg/mL(S/N=3),平均回收率在96.00%~103.64%(n=3)之间,RSD%在1.39%~4.56%之间。实验结果表明,该方法线性关系良好,操作简便,分析时间短,检测成本低,可以为决明子中蒽醌类成分的分析提供一定的参考。
[Abstract]:In twenty-first Century, with the improvement of human living standard, people's attention to health and health is also increasing. On the premise of ensuring food safety, people are more hoping to regulate their own functions through diet therapy, and can also eliminate diseases while satisfying basic nutrition. Therefore, the analysis of the effective components in food and medicine is studied. In many analysis and detection techniques, capillary electrophoresis is popular with the advantages of high separation efficiency, short analysis time and low cost consumption. It is a useful tool for discovering and solving some new problems in their respective fields. This paper mainly applies high performance capillary electricity. The specific content of the active components in food and drugs is detected by swimming and ultraviolet absorption detector. The specific contents are as follows: Chapter 1: a brief overview of high performance capillary electrophoresis and its applications, including the development of high performance capillary electrophoresis, basic separation theory, separation mode, sampling technique, signal detection method and its application. On the basis of understanding the technology, this chapter briefly summarizes the application of high performance capillary electrophoresis in different fields and summarizes the significance of this study. The second chapter: using high performance capillary zone electrophoresis, 4 active substances of rutin, kaempferol, isamamenin and quercetin in 3 areas of sea buckthorn fruit powder are entered. The conditions affecting the electrophoresis separation efficiency were investigated. The conditions of affecting the electrophoresis separation efficiency were: 20 mmol/L Na2B4O7-H3BO3,1.5 mg/m L of buffer solution, beta cyclodextrin, pH 9.55, detection wavelength 370 nm, separation voltage 25 kV, 5 s. rutin, kaempferol, ISO rhamnin and quercetin in 11 min to achieve a better separation and linear range in 11 min. The detection limit is 5.05 x 10-5,2.10 x 10-5,3.75 x 10-5,1.31 x 10-5mg/mL (RSN=3), and the correlation coefficient r is between 0.9971~0.9991 and 0.9971~0.9991. The linear relationship between each substance is good. The range of intra day and day precision is 0.08%~4.72%, the average recovery is between 95.51%~104.66% and RSD% is not more than 3.92% (n=3). Under the optimum conditions, the mixture of 4 kinds of active substances was measured and the extracts of the active substances in the 3 species of seabuckthorn fruit powder were detected by the same method. The results showed that the content of the 4 kinds of compounds detected in the different Seabuckthorn production was different. The highest total of the 4 compounds in the sand spines was produced from Xinjiang. Urumqi, the lowest production from Wuwei in Gansu, and the highest content of quercetin from Lvliang in Shanxi, kaempferol and ISO rhamnin is the highest in Urumqi of Xinjiang. The rapid separation of Flavonoids from sea buckthorn fruit powder can be realized by this method. The third chapter: by high performance capillary electrophoresis, it can be used in apple. The separation and determination of 4 kinds of phenolics, such as glucoside, epicatechin, rutin and chlorogenic acid, optimized the experimental conditions. The optimum experimental conditions were as follows: the buffer solution was 10 mmol/L Na2B4O7-H3BO3, pH 9.2, the detection wavelength was 280 nm, the separation voltage was 25 kV, and the linear range of the sampling time was 0.005~0.120,0.005~0.550,0.004~0.450,0.020~0.600 mg/m L in the linear range of the sampling time. The minimum detection limit is 3.41 x 10-5,5.67 x 10-5,3.78 x 10-5,3.89 x 10-5mg/m L (S/N=3) between 0.9977~0.9992 and R. After that, the intraday and daytime precision and average recovery are tested, the range is 0.13%~4.59% and 96.72%~104.55%, RSD% < 3.74% (n=3). The mixture of the quasi product was determined and the same method was used to determine the extract of apple skin and apple meat. The experimental results showed that the method was simple, accurate and reliable, and could be used as a means to detect the quality of various phenols in apple. The fourth chapter was based on high performance capillary electrostroke UV detection technology, and studied 5 in cassia seed. The capillary electrophoresis migration of anthraquinone compounds is made by optimizing the experimental conditions and analyzing various influencing factors. The qualitative and quantitative analysis of the tested control products and the tested products is carried out. The optimum separation conditions are determined as follows: the detection wavelength is 284 nm, the separation voltage is 25 kV, the injection time is 5 s, the Na2B4O7-H3BO3 concentration of the buffer solution is 20 mmol/L, pH 8.50, the concentration of beta cyclodextrin is 5 mmol/L. Under this condition, orange cassia, emodin, emodin, chrysophanol and chrysophanol are separated in 10 min, the linear range is 0.005~0.400,0.004~0.350,0.004~0.400,0.002~0.350,0.003~0.300 mg/mL in turn, the linear correlation coefficient is more than 0.9952, and the detection limit is 5.03 * 10-5,5.66 x 10-5,1., respectively. 67 * 10-5,5.19 x 10-5,3.36 x 10-5mg/mL (S/N=3), the average recovery rate is between 96.00%~103.64% (n=3) and RSD% in 1.39%~4.56%. The experimental results show that the method has a good linear relationship, simple operation, short analysis time and low detection cost, which can provide some reference for the analysis of anthraquinones in cassia seed.

【学位授予单位】：山西师范大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O658.9;TS207.3;TQ460.72

【参考文献】