本文選題：毛細(xì)管電泳　切入點(diǎn)：多糖　出處：《廣西大學(xué)》2016年碩士論文　論文類型：學(xué)位論文

【摘要】：本文主要綜述了多糖的單糖組成分析方法和食品中添加劑的測(cè)定方法,以及非在線分離富集樣品和在線分離富集樣品的方法。實(shí)驗(yàn)利用毛細(xì)管電泳的膠束電動(dòng)色譜模式,分析廣西特色茶葉品種-金花茶和六堡茶中多糖的單糖構(gòu)成和摩爾比例,利用非在線分離富集技術(shù)-固相萃取和分散液液微萃取與在線富集技術(shù)-場(chǎng)放大樣品堆積預(yù)處理食品中的添加劑,具體工作內(nèi)容如下：(1)用超聲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濃縮液的粗多糖析出,然后進(jìn)行活性炭脫色,體積比4：1的三氯甲烷：正丁醇除蛋白質(zhì),強(qiáng)酸高溫降解多糖,多糖水解液經(jīng)1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生化后,用毛細(xì)管膠束電動(dòng)色譜法測(cè)定,內(nèi)標(biāo)法定量分析,優(yōu)化分離條件測(cè)定單糖的組成和含量,結(jié)果表明金花茶多糖和六堡茶多糖的單糖組成均為阿拉伯糖、葡萄糖、鼠李糖、甘露糖、半乳糖和半乳糖醛酸,前者物質(zhì)的量之比為0.13：0.19：0.09：0.05：0.16：0.03,后者物質(zhì)的量之比為0.29：0.02：0.10：0.06：0.42：0.35,各單糖在線性范圍內(nèi)線性關(guān)系良好,線性相關(guān)系數(shù)均在0.992以上(2)實(shí)驗(yàn)考察了不同固相萃取柱的萃取能力,洗脫液的種類,洗脫液的流速以及內(nèi)標(biāo)物的選擇,優(yōu)化實(shí)驗(yàn)條件,利用HLB固相萃取柱萃取食品中的添加劑,毛細(xì)管區(qū)帶電泳測(cè)定,內(nèi)標(biāo)法定量分析,結(jié)果各添加劑的線性相關(guān)系數(shù)均大于0.99,相對(duì)標(biāo)準(zhǔn)偏差小于5%,樣品加標(biāo)回收率在95%-102%之間。(3)實(shí)驗(yàn)選擇三氯甲烷為萃取劑,丙酮為分散劑,分散液液微萃取食品中的防腐劑,毛細(xì)管電泳在最佳條件下測(cè)定防腐劑的種類,內(nèi)標(biāo)法定量,結(jié)果表明各防腐劑的線性關(guān)系良好,相關(guān)系數(shù)達(dá)到0.99以上,相對(duì)標(biāo)準(zhǔn)偏差不超過6%,回收率在99%-103%之間。(4)實(shí)驗(yàn)選擇場(chǎng)放大在線富集食品中的幾種防腐劑和色素,毛細(xì)管電泳測(cè)定,優(yōu)化水柱引入時(shí)間,分離電壓和緩沖溶液pH等條件,在最佳的實(shí)驗(yàn)條件下,五種添加劑的線性關(guān)系良好,相關(guān)系數(shù)在0.99以上,相對(duì)標(biāo)準(zhǔn)偏差不大于8%,回收率在97%-103%之間。
[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%.
【學(xué)位授予單位】：廣西大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2016
【分類號(hào)】：TS272.7;O658.9

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