本文選題：蜂蜜　切入點：高效毛細管電泳　出處：《河南科技學(xué)院》2017年碩士論文

【摘要】：中國是世界養(yǎng)蜂大國,也是世界蜂蜜生產(chǎn)大國,另外還是蜂蜜出口量最大的國家。蜂蜜中含有多種營養(yǎng)物質(zhì),具有保健功能,深受人們的歡迎。蜂蜜中的很多成分都直接影響著它的顏色、香氣、口感和保健功效,而其中的有機活性組分會直接影響其營養(yǎng)價值及其抗菌,抗氧化等生物性功能。為了更好的評價蜂蜜的品質(zhì),本論文采用色譜技術(shù)(高效液相色譜及高效毛細管電泳)建立了蜂蜜中低分子量黃酮、有機酸和水溶性維生素類化合物的毛細管電泳及高效液相色譜分離分析方法,具體結(jié)論如下:1.黃酮是蜂蜜中的重要活性成分,通過直接紫外檢測毛細管區(qū)帶電泳法開發(fā)了來自不同地理來源的許多蜂蜜中的類黃酮的分析方法。在25kV的分離電壓下,使用20mM硼酸鹽作為運行緩沖液在pH=8.4下在5min內(nèi)完全分離包括蘆丁、槲皮素、山奈酚和楊梅酮的四種典型黃酮類化合物。對于四種類黃酮獲得了在2.0-500mg/L的范圍內(nèi)的良好的線性關(guān)系,并且檢測限范圍為1.17至1.76mg/L。四種類黃酮的回收率在80%-107%的范圍內(nèi)。應(yīng)用該方法分離測定了中國河南省12個養(yǎng)蜂場蜂蜜樣品中的黃酮類化合物。在許多蜂蜜樣品中僅檢測到蘆丁和槲皮素,其可以作為鑒定來自不同地理來源的蜂蜜的標記物。2.采用毛細管電泳法,通過場放大樣品注射技術(shù)(FASI)建立了7種有機酸的分析檢測方法,對影響FASI的參數(shù)進行系統(tǒng)研究,包括pH、注射時間、水柱長度、緩沖液濃度等。在最佳條件下檢測靈敏度明顯增強,各組分富集倍數(shù)可增加7-72倍。酒石酸、原兒茶酸、綠原酸、草酸、沒食子酸、檸檬酸和香草酸的檢測限分別為0.56、0.26、0.85、0.90、0.65、0.52和0.55mg/L。該方法成功應(yīng)用于來自河南省不同地市蜂場的14種蜂蜜實際樣品的檢測。3.采用響應(yīng)曲面法,設(shè)計三因素三水平的Box-Behnken的試驗,對影響毛細管電泳分離水溶性維生素B1、B3、B5、B6及維生素C的主要影響因素(緩沖溶液的濃度、分離電壓和柱溫)進行了研究,以五種維生素中的最大分離度和最長保留時間為響應(yīng)函數(shù),建立了相應(yīng)的數(shù)學(xué)模型,得到了它們的最佳分離條件為:17mmol/L的硼砂電泳緩沖液、15 kV電壓、19℃柱溫,并在最優(yōu)的分離條件下,3分鐘內(nèi)可快速分離蜂蜜樣品中的五種水溶性維生素。4.建立了同時檢測維生素C和多巴胺的高效液相色譜-電化學(xué)檢測法。其中高效液相色譜的色譜柱采用Diamonsil C18(2)5μ150×4.6mm色譜柱,并以體積比為74:24:2的0.05mol/L磷酸二氫鈉、0.02mol/L檸檬酸和甲醇的混合液為流動相,設(shè)定檢測波長為280nm,流速為1mL/min。在室溫條件下,維生素C的線性范圍在高效液相色譜和電化學(xué)檢測器中分別為2-200μmol/L和0.05-200μmol/L,檢出限分別為1.68μmol/L和0.03μmol/L;多巴胺在高效液相色譜和電化學(xué)檢測器中分別為2-200μmol/L和0.05-200μmol/L,檢出限分別為1.25μmol/L和0.01μmol/L。高效液相色譜-電化學(xué)檢測器聯(lián)用的方法更為簡便靈敏度和準確率更高,且選擇性更好。5.建立了可靠,靈敏的反相高效液相色譜-電化學(xué)檢測(HPLC-ECD)方法測定蜂蜜中三種有機酸類電化學(xué)活性化合物(沒食子酸、綠原酸、咖啡酸)。色譜分離在反相C18柱上進行,流動相由4%的醋酸水溶液(pH=4.0)和甲醇組成,通過電流檢測,使用工作電位為+0.80V的玻碳電極進行梯度洗脫。該方法的線性,精度,精度和定量和檢測限已被驗證。在優(yōu)化條件下,電化學(xué)校準曲線的線性回歸分析顯示出良好的線性關(guān)系,在0.005 mg/L-6.0 mg/L的線性范圍內(nèi),峰面積與濃度之間的回歸系數(shù)超過0.99,其檢測限為10-5-3×10-5 mg/L。該方法可以應(yīng)用于蜂蜜中存在的三種有機酸化合物的分析。
[Abstract]:Chinese is the world beekeeping country, is also the world's honey producing countries, and is the largest in the country. The export volume of honey honey contains a variety of nutrients, with health care function, welcomed by the people. Many of the components in honey will directly affect its color, aroma, taste and health effects, and organic active components including the direct impact on the nutritional value and biological function of antibacterial, antioxidant and so on. In order to evaluate the quality of honey, this paper adopts chromatography (HPLC and HPCE) established low molecular weight honey capillary electrophoresis separation and analysis methods of flavonoids, organic acid and water soluble vitamin compounds and HPLC chromatography, specific conclusions are as follows: 1. flavone is an important active ingredient in honey, through direct UV detection by capillary zone electrophoresis was developed from different geographical origins Analysis of the flavonoids in many honey. At the separation voltage of 25kV, using 20mM borate as running buffer at pH=8.4 in 5min complete separation including rutin, quercetin, four typical flavonoids kaempferol and Yang Meitong. The good linear relationship between the four kinds of flavonoids were obtained in the range of 2.0-500mg/L the limit of detection and recovery in the range of 1.17 to four 1.76mg/L. flavonoid rate in the range of 80%-107%. The flavonoids field in honey samples of 12 beekeeping in Henan province was determined by the method of separation of Chinese. In many honey samples was detected in rutin and quercetin, which can be used as identification from different geographical origins honey marker.2. by capillary electrophoresis, through field amplified sample injection technique (FASI) was established to analyze the detection method of 7 kinds of organic acids, the effects of FASI parameters. For system research, including pH, injection time, column length, buffer concentration. Significantly enhanced the detection sensitivity in the optimum conditions, the components can be increased by 7-72 times. The enrichment of tartaric acid, protocatechuic acid, gallic acid, chlorogenic acid, oxalic acid, citric acid and vanillic acid detection limit detection of.3. were 0.56,0.26,0.85,0.90,0.65,0.52 and the 0.55mg/L. method is successfully applied to different cities of Henan province from 14 kinds of honey bee samples using response surface methodology, experimental design of three factors and three levels of Box-Behnken, the effect of capillary electrophoresis separation of water soluble vitamins B1, B3, B5, B6 and the main influence factors of vitamin C (concentration, buffer the solution of separation voltage and column temperature) were studied in five kinds of vitamins in the maximum separation degree and the long retention time of response function, the corresponding mathematical model is established, by which the optimal separation A: borax buffer solution 17mmol/L, 15 kV voltage, 19 DEG C, column temperature, and separation in the optimal condition, 3 minutes fast separation of five honey samples of water soluble vitamin.4. was developed for the determination of vitamin C and dopamine by high performance liquid chromatography with electrochemical detection. The chromatography high performance liquid chromatography using Diamonsil C18 (2) 5 ~ 150 * 4.6mm column, and the volume ratio of 74:24:2 0.05mol/L phosphate, 0.02mol/L mixture of citric acid and methanol as the mobile phase, the detection wavelength was set 280nm, the flow rate of 1mL/min. at room temperature for 2-200 mol/L and 0.05-200 respectively. Mol/L linear range of vitamin C by high performance liquid chromatography and electrochemical detector, the detection limits were 1.68 mol/L and 0.03 mol/L respectively; 2-200 mol/L and 0.05-200 mol/L dopamine in high performance liquid chromatography and electrochemical detector, detection The limits were 1.25 mol/L and 0.01 mol/L. high performance liquid chromatography with electrochemical detector is simpler and more sensitivity and higher accuracy, and better selectivity of.5. to establish a reliable and sensitive reversed-phase high-performance liquid chromatography with electrochemical detection (HPLC-ECD) determination of three organic acids in honey for electrochemically active compounds (gallic acid, chlorogenic acid, caffeic acid). Chromatographic separation was performed on a reversed-phase C18 column, the mobile phase consisted of 4% aqueous solution of acetic acid (pH=4.0) and methanol, the current detection, using the working potential of glassy carbon electrode +0.80V in linear gradient elution. The method, precision, accuracy and quantitative detection and the limit has been verified. Under the optimized conditions, the analysis showed a good linear relationship between the electrochemical linear calibration curve regression, in the linear range of 0.005 mg/L-6.0 mg/L, between the peak area and concentration of regression coefficient is more than 0.99, The detection limit of 10-5-3 x 10-5 mg/L. can be applied to the analysis of three organic acids in honey.

【學(xué)位授予單位】：河南科技學(xué)院
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O657.7;S896.1

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