离子色谱法在食品中糖类化合物的应用研究

发布时间：2018-07-27 13:47

【摘要】：离子色谱法(Ion chromatography,IC)具备高效、快捷灵敏、操作简单等优点,在现代分析领域如食品卫生、环境安全、化学工程、生物工程等方面具有非常广泛的应用。它的原理是根据被测物的可解离性与固定相表面带电荷的功能基团相互作用,使得被测物保留在固定相上,不同的离子因与固定相的作用力不同而得以分离的液相色谱方法。近年来,糖类化合物的药理作用被发现,且部分糖类化合物还可作为衡量产品质量的重要依据,因此糖类化合物的分析一直是广大研究者致力于研究的方向。采用离子色谱法准确分析糖类化合物已被认定为一种有效的方法,并在食品行业中发挥着重要的作用。本文由两部分构成:绪论部分和研究报告。第一部分绪论首先叙述了离子色谱法的概念及发展、分类及原理和检测技术,其次阐述了离子色谱在食品分析中的应用,最后对糖类化合物的概念及分类,提取方法和分析方法做了简单介绍。第二部分研究报告建立了热带水果,花卉,红枣和瓶装绿茶饮料食品中糖类化合物的提取分离方法。1.离子交换色谱法测定10种水果中的葡萄糖、蔗糖和果糖建立了阴离子交换-脉冲安培检测(High performance anion exchange-pulsed amperometric detection,HPAE-PAD)测定火龙果、莲雾、牛油果等10种热带水果中葡萄糖、蔗糖和果糖的检测方法。10种水果中的多糖经超声萃取后,用METROSEP CARB 1(150 mm×4.0 mm)色谱柱进行分离,以30.0 mmol/L NaOH为流动相,等度洗脱,用安培检测器检测,18 min可完成对样品多糖的分离和定量分析。经测定,葡萄糖和蔗糖的检出限分别为0.121 mg/L和0.283 mg/L,线性范围为1.0~70.0 mg/L;果糖的检出限为0.550 mg/L,线性范围为5.0~80.0 mg/L。样品溶液连续5次进样,3种糖的相对标准偏差为0.67%~7.04%,平均回收率为78.70%~117.75%。该方法前处理简单、选择性好、灵敏度高,可用于水果中可溶性糖的测定。2.超声萃取-离子色谱法测定5种花卉中的游离糖基于超声波辅助萃取技术,利用离子色谱法分离和测定了百合,桂花,菊花,金银花以及玫瑰花中的游离糖(半乳糖、葡萄糖、甘露糖和果糖)。室温下,超声水提花卉中的多糖,以METROSEP CARB 1(150 mm×4.0 mm)色谱柱作为分离柱,8.0mmol/L NaOH为流动相等度洗脱,脉冲安培检测器检测。经测定,半乳糖、葡萄糖和甘露糖的检出限分别为0.228 mg/L、0.345 mg/L和0.480 mg/L,线性范围为1.0~60.0 mg/L;果糖的检出限为1.910 mg/L,线性范围为2.0~70.0 mg/L。将10.0mg/L的混合标准溶液连续6次进样,得到半乳糖,葡萄糖,甘露糖和果糖峰高的相对标准偏差为2.66%、2.81%、2.12%、4.80%,峰面积测定值的相对标准偏差为3.23%、5.41%、4.19%、7.03%,保留时间的相对标准偏差为1.92%、2.64%、3.01%、4.62%。样品测定的回收率为72.31%~112.00%。本方法前处理简单、测定准确、灵敏度高,为花卉中游离糖的分离和定量提供了实验依据。3.碱液提取-离子色谱法测定红枣中的3种糖以碱液作为萃取剂,建立了高效阴离子交换-脉冲安培检测法测定红枣中葡萄糖、果糖和蔗糖3种糖的检测方法。采用METROSEP CARB 1(150 mm×4.0 mm)色谱柱,180.0 mmol/L NaOH为流动相等度洗脱,用安培检测器检测,8 min可完成对样品多糖的分离和定量分析。加入1:20(g:ml)料液比的0.5 mol/L Na2CO3溶液,并在90℃的水浴条件下浸提3 h。经测定,葡萄糖、果糖和蔗糖的检出限分别为0.068 mg/L、0.178 mg/L和0.191 mg/L,线性范围为1.0~60.0 mg/L,相对标准偏差为1.22%~5.35%(n=5),平均回收率为82.15%~120.65%。本实验方法分析速度快、重现性好、灵敏度高,可用于红枣中葡萄糖、果糖和蔗糖的测定。4.阴离子交换-脉冲安培检测法检测5种瓶装绿茶饮料中的单糖和寡糖利用阴离子交换-脉冲安培检测法分离和测定了5种瓶装绿茶饮料中的单糖和寡糖(蔗糖、葡萄糖、甘露糖和果糖)。采用METROSEP CARB 1(150 mm×4.0 mm)色谱柱完成蔗糖、葡萄糖、甘露糖和果糖的分离;流动相为7.0 mmol/L NaOH,进行等度洗脱,流速1.0 m L/min。在30 min内完成4种糖的色谱分离,并且得到了满意的线性范围(r0.9980,n=8),蔗糖、葡萄糖、甘露糖和果糖检出限分别为0.300mg/L、0.114 mg/L、0.184 mg/L和1.164 mg/L。蔗糖、葡萄糖、甘露糖线性范围为1.0~60.0 mg/L,果糖的线性范围为5.0~80.0 mg/L。样品的平均回收率为87.00%~107.60%。得到蔗糖,葡萄糖,甘露糖和果糖的日内精密度分别为1.25%、0.68%、2.57%和3.74%,日间精密度分别为3.56%、2.09%、4.63%和5.87%。该分析方法绿色环保、灵敏度高、重复性好,可作为瓶装绿茶饮料的质量控制方法。
[Abstract]:Ion chromatography (IC) has many advantages, such as high efficiency, quick and sensitive, simple operation and so on. It has a very wide application in the fields of modern analysis such as food hygiene, environmental safety, chemical engineering, biological engineering and so on. Its principle is to interact with the functional groups with the charge of the fixed phase surface with the solvability of the measured objects. In recent years, the pharmacological effects of carbohydrates have been found, and some carbohydrates can also be used as an important basis for measuring the quality of the products. The analysis of these compounds has been caused by the majority of researchers. The accurate analysis of carbohydrate compounds by ion chromatography has been identified as an effective method and plays an important role in the food industry. This article is composed of two parts: introduction and research. First part of the introduction describes the concept and development of ion chromatography, classification, principle and detection. Technology, secondly, the application of ion chromatography in food analysis is expounded. At last, the concept and classification of saccharides, extraction methods and analytical methods are briefly introduced. The second part of the study has established the extraction and separation method of sugar compounds in tropical fruit, flowers, red dates and bottled green tea drinks food.1. ion exchange chromatography Glucose, sucrose and fructose in 10 kinds of fruit were determined by the method of anion exchange pulse ampere detection (High performance anion exchange-pulsed amperometric detection, HPAE-PAD) for the determination of glucose, sucrose and fructose in 10 kinds of tropical fruits, pitaya, lotus fog and cow oil. The polysaccharides in.10 fruit were extracted by ultrasonic extraction. After extraction, the separation was made with METROSEP CARB 1 (150 mm x 4 mm) column, 30 mmol/L NaOH as mobile phase, equal degree elution, detection by ampere detector and 18 min to complete the separation and quantitative analysis of sample polysaccharide. The detection limit of glucose and sucrose was 0.121 mg/L and 0.283 mg/L respectively, and the linear range was 1.0~70.0 mg/L; fructose The detection limit is 0.550 mg/L, the linear range is 5.0~80.0 mg/L. sample solution for 5 consecutive samples, the relative standard deviation of 3 sugars is 0.67%~7.04%, the average recovery rate is 78.70%~117.75%., the pretreatment is simple, the selectivity is good, and the sensitivity is high. It can be used for the determination of soluble sugar in fruit by.2. ultrasonic extraction ion chromatography for the determination of 5 kinds of flowers. Free sugar based on ultrasonic assisted extraction technology, the free sugar (galactose, glucose, mannose and fructose) in lily, osmanthus, chrysanthemum, honeysuckle and rose were separated and measured by ion chromatography. At room temperature, the polysaccharides in flowers were extracted by ultrasonic water, and METROSEP CARB 1 (150 mm x 4 mm) column was used as separation column, 8.0mmol/L NaO The detection limits of galactose, glucose and mannose were 0.228 mg/L, 0.345 mg/L and 0.480 mg/L, and the linear range was 1.0~60.0 mg/L, the detection limit of fructose was 1.910 mg/L, and the linear range was 2.0~70.0 mg/L., and the mixed standard solution of 10.0mg/L was 6 times continuously. The relative standard deviation of lactose, glucose, mannose and fructose peak is 2.66%, 2.81%, 2.12%, 4.80%, and the relative standard deviation of the peak area determination value is 3.23%, 5.41%, 4.19%, 7.03%. The relative standard deviation of the retention time is 1.92%, 2.64%, 3.01%, and the recovery rate of the 4.62%. sample is 72.31%~112.00%.. The sensitivity of 3 kinds of sugar in red jujube was determined by.3. alkaline solution ion chromatography. The determination of 3 kinds of glucose, fructose and sucrose in red jujube was established by high performance anion exchange pulse ampere detection. The method of METROSEP CARB 1 (150 mm x 4) was used to determine the method of determination of glucose, fructose and sucrose in red date. Mm) the chromatographic column, 180 mmol/L NaOH was eluted for the flow equality, was detected by an ampere detector, and 8 min could complete the separation and quantitative analysis of the polysaccharide. 0.5 mol/L Na2CO3 solution was added to the 1:20 (g:ml) mixture, and the 3 h. was extracted at 90 C in water bath, and the detection limit of glucose, fructose and sucrose was 0.068 mg/L, 0.178 m respectively. G/L and 0.191 mg/L, the linear range is 1.0~60.0 mg/L, the relative standard deviation is 1.22%~5.35% (n=5), the average recovery rate is 82.15%~120.65%., the experimental method is fast, reproducible and sensitive. It can be used for the determination of glucose, fructose and sucrose in red jujube with.4. negative exchange pulse amperometric detection method for the detection of 5 kinds of bottled green tea drinks Monosaccharides and oligosaccharides were used to separate and determine monosaccharides and oligosaccharides (sucrose, glucose, mannose and fructose) in 5 kinds of bottled green tea beverages by anion exchange and pulse ampere detection. The separation of sucrose, glucose, mannose and fructose by METROSEP CARB 1 (150 mm x 4 mm) column was completed; the flow phase was 7 mmol/L NaOH. Elution, flow rate of 1 m L/min. in 30 min to complete the chromatographic separation of 4 kinds of sugar, and obtained a satisfactory linear range (r0.9980, n=8), sucrose, glucose, mannose and fructose detection limits are 0.300mg/L, 0.114 mg/L, 0.184 mg/L and 1.164 mg/L. sucrose, glucose, mannose linear range is 1.0~60.0 mg/L, the linear range of fructose is 5.0~80 The average recovery of.0 mg/L. samples was 87.00%~107.60%. for sucrose, glucose, mannose and fructose, the intraday precision was 1.25%, 0.68%, 2.57% and 3.74% respectively. The day precision was 3.56%, 2.09%, 4.63% and 5.87%., respectively. The analysis method was green, high sensitivity and good reproducibility, which could be used as the quality control method for the bottle of green tea beverage.
【学位授予单位】：西南大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.7;TS207.3

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