毛细管电泳测定金花茶，六堡茶中多糖组成和食品添加剂的研究

发布时间：2018-03-08 15:50

本文选题：毛细管电泳　切入点：多糖　出处：《广西大学》2016年硕士论文　论文类型：学位论文

【摘要】：本文主要综述了多糖的单糖组成分析方法和食品中添加剂的测定方法,以及非在线分离富集样品和在线分离富集样品的方法。实验利用毛细管电泳的胶束电动色谱模式,分析广西特色茶叶品种-金花茶和六堡茶中多糖的单糖构成和摩尔比例,利用非在线分离富集技术-固相萃取和分散液液微萃取与在线富集技术-场放大样品堆积预处理食品中的添加剂,具体工作内容如下：(1)用超声波提取六堡茶中的多糖,加入乙醇使六堡茶提取液和金花茶浓缩液的粗多糖析出,然后进行活性炭脱色,体积比4：1的三氯甲烷：正丁醇除蛋白质,强酸高温降解多糖,多糖水解液经1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化后,用毛细管胶束电动色谱法测定,内标法定量分析,优化分离条件测定单糖的组成和含量,结果表明金花茶多糖和六堡茶多糖的单糖组成均为阿拉伯糖、葡萄糖、鼠李糖、甘露糖、半乳糖和半乳糖醛酸,前者物质的量之比为0.13：0.19：0.09：0.05：0.16：0.03,后者物质的量之比为0.29：0.02：0.10：0.06：0.42：0.35,各单糖在线性范围内线性关系良好,线性相关系数均在0.992以上(2)实验考察了不同固相萃取柱的萃取能力,洗脱液的种类,洗脱液的流速以及内标物的选择,优化实验条件,利用HLB固相萃取柱萃取食品中的添加剂,毛细管区带电泳测定,内标法定量分析,结果各添加剂的线性相关系数均大于0.99,相对标准偏差小于5%,样品加标回收率在95%-102%之间。(3)实验选择三氯甲烷为萃取剂,丙酮为分散剂,分散液液微萃取食品中的防腐剂,毛细管电泳在最佳条件下测定防腐剂的种类,内标法定量,结果表明各防腐剂的线性关系良好,相关系数达到0.99以上,相对标准偏差不超过6%,回收率在99%-103%之间。(4)实验选择场放大在线富集食品中的几种防腐剂和色素,毛细管电泳测定,优化水柱引入时间,分离电压和缓冲溶液pH等条件,在最佳的实验条件下,五种添加剂的线性关系良好,相关系数在0.99以上,相对标准偏差不大于8%,回收率在97%-103%之间。
[Abstract]:In this paper, the analytical methods of monosaccharide composition of polysaccharides and the determination of additives in food, as well as the methods of off-line separation and enrichment of samples and on-line separation and enrichment of samples were reviewed. The micellar electrokinetic chromatography mode based on capillary electrophoresis was used in the experiment. The monosaccharide composition and molar ratio of polysaccharides in Jinhua tea and Liubao tea were analyzed. The additives in food were pretreated with off-line separation and enrichment techniques-solid phase extraction and dispersible liquid microextraction and on-line enrichment techniques-field amplification sample stacking. The specific work is as follows: (1) extraction of polysaccharides from Rupu tea by ultrasonic wave. Adding ethanol precipitates the crude polysaccharides from Hupu tea extract and Jinhua tea concentrate, and then decolorizes the activated carbon. The volume ratio of 4: 1 trichloromethane: n-butanol deproteinizes protein, strong acid degrades polysaccharides at high temperature. The polysaccharides hydrolysate was derivatized by 1-phenyl-3-methyl-5-pyrazolone (PMP), and was determined by capillary micellar electrokinetic chromatography. The composition and content of monosaccharide were determined by internal standard method, and the separation conditions were optimized to determine the composition and content of monosaccharide. The results showed that the monosaccharide compositions of the polysaccharides of Jinhua tea and Hupu tea were arabinose, glucose, rhamnose, mannose, galactose and galacturonic acid. The volume ratio of the former is 0.13: 0.19: 0.05: 0.05: 0.016: 0.03, and the volume ratio of the latter is 0.29: 0.02: 0.10: 0.06: 0.42: 0.35. The linear range of each monosaccharide is linear, and the linear correlation coefficient is above 0.992. The flow rate of eluent, the selection of internal standard, the optimization of experimental conditions, the extraction of additives in food by HLB solid-phase extraction column, the determination of capillary zone electrophoresis, and the quantitative analysis by internal standard method. Results the linear correlation coefficient of each additive was greater than 0.99, the relative standard deviation was less than 5. The recovery rate of the sample was between 95% and 102%. In the experiment, trichloromethane was used as extractant, acetone as dispersant, and the preservative in dispersible microextraction food. The content of preservatives was determined by capillary electrophoresis under the optimum conditions. The results showed that the linear relationship of the preservatives was good, and the correlation coefficient was above 0.99. Relative standard deviation (RSDs) was not more than 6 and the recovery rate was between 99- 103%.) the experiment selected several preservatives and pigments in food enriched online by field amplification, determined by capillary electrophoresis, optimized water column introduction time, separation voltage and pH value of buffer solution, etc. Under the optimum experimental conditions, the linear relationship of the five additives is good, the correlation coefficient is more than 0.99, the relative standard deviation is not more than 8, and the recovery is between 97% and 103%.
【学位授予单位】：广西大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TS272.7;O658.9

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