【摘要】：離子色譜法(Ion chromatography,IC)具備高效、快捷靈敏、操作簡單等優(yōu)點,在現(xiàn)代分析領(lǐng)域如食品衛(wèi)生、環(huán)境安全、化學工程、生物工程等方面具有非常廣泛的應(yīng)用。它的原理是根據(jù)被測物的可解離性與固定相表面帶電荷的功能基團相互作用,使得被測物保留在固定相上,不同的離子因與固定相的作用力不同而得以分離的液相色譜方法。近年來,糖類化合物的藥理作用被發(fā)現(xiàn),且部分糖類化合物還可作為衡量產(chǎn)品質(zhì)量的重要依據(jù),因此糖類化合物的分析一直是廣大研究者致力于研究的方向。采用離子色譜法準確分析糖類化合物已被認定為一種有效的方法,并在食品行業(yè)中發(fā)揮著重要的作用。本文由兩部分構(gòu)成:緒論部分和研究報告。第一部分緒論首先敘述了離子色譜法的概念及發(fā)展、分類及原理和檢測技術(shù),其次闡述了離子色譜在食品分析中的應(yīng)用,最后對糖類化合物的概念及分類,提取方法和分析方法做了簡單介紹。第二部分研究報告建立了熱帶水果,花卉,紅棗和瓶裝綠茶飲料食品中糖類化合物的提取分離方法。1.離子交換色譜法測定10種水果中的葡萄糖、蔗糖和果糖建立了陰離子交換-脈沖安培檢測(High performance anion exchange-pulsed amperometric detection,HPAE-PAD)測定火龍果、蓮霧、牛油果等10種熱帶水果中葡萄糖、蔗糖和果糖的檢測方法。10種水果中的多糖經(jīng)超聲萃取后,用METROSEP CARB 1(150 mm×4.0 mm)色譜柱進行分離,以30.0 mmol/L NaOH為流動相,等度洗脫,用安培檢測器檢測,18 min可完成對樣品多糖的分離和定量分析。經(jīng)測定,葡萄糖和蔗糖的檢出限分別為0.121 mg/L和0.283 mg/L,線性范圍為1.0~70.0 mg/L;果糖的檢出限為0.550 mg/L,線性范圍為5.0~80.0 mg/L。樣品溶液連續(xù)5次進樣,3種糖的相對標準偏差為0.67%~7.04%,平均回收率為78.70%~117.75%。該方法前處理簡單、選擇性好、靈敏度高,可用于水果中可溶性糖的測定。2.超聲萃取-離子色譜法測定5種花卉中的游離糖基于超聲波輔助萃取技術(shù),利用離子色譜法分離和測定了百合,桂花,菊花,金銀花以及玫瑰花中的游離糖(半乳糖、葡萄糖、甘露糖和果糖)。室溫下,超聲水提花卉中的多糖,以METROSEP CARB 1(150 mm×4.0 mm)色譜柱作為分離柱,8.0mmol/L NaOH為流動相等度洗脫,脈沖安培檢測器檢測。經(jīng)測定,半乳糖、葡萄糖和甘露糖的檢出限分別為0.228 mg/L、0.345 mg/L和0.480 mg/L,線性范圍為1.0~60.0 mg/L;果糖的檢出限為1.910 mg/L,線性范圍為2.0~70.0 mg/L。將10.0mg/L的混合標準溶液連續(xù)6次進樣,得到半乳糖,葡萄糖,甘露糖和果糖峰高的相對標準偏差為2.66%、2.81%、2.12%、4.80%,峰面積測定值的相對標準偏差為3.23%、5.41%、4.19%、7.03%,保留時間的相對標準偏差為1.92%、2.64%、3.01%、4.62%。樣品測定的回收率為72.31%~112.00%。本方法前處理簡單、測定準確、靈敏度高,為花卉中游離糖的分離和定量提供了實驗依據(jù)。3.堿液提取-離子色譜法測定紅棗中的3種糖以堿液作為萃取劑,建立了高效陰離子交換-脈沖安培檢測法測定紅棗中葡萄糖、果糖和蔗糖3種糖的檢測方法。采用METROSEP CARB 1(150 mm×4.0 mm)色譜柱,180.0 mmol/L NaOH為流動相等度洗脫,用安培檢測器檢測,8 min可完成對樣品多糖的分離和定量分析。加入1:20(g:ml)料液比的0.5 mol/L Na2CO3溶液,并在90℃的水浴條件下浸提3 h。經(jīng)測定,葡萄糖、果糖和蔗糖的檢出限分別為0.068 mg/L、0.178 mg/L和0.191 mg/L,線性范圍為1.0~60.0 mg/L,相對標準偏差為1.22%~5.35%(n=5),平均回收率為82.15%~120.65%。本實驗方法分析速度快、重現(xiàn)性好、靈敏度高,可用于紅棗中葡萄糖、果糖和蔗糖的測定。4.陰離子交換-脈沖安培檢測法檢測5種瓶裝綠茶飲料中的單糖和寡糖利用陰離子交換-脈沖安培檢測法分離和測定了5種瓶裝綠茶飲料中的單糖和寡糖(蔗糖、葡萄糖、甘露糖和果糖)。采用METROSEP CARB 1(150 mm×4.0 mm)色譜柱完成蔗糖、葡萄糖、甘露糖和果糖的分離;流動相為7.0 mmol/L NaOH,進行等度洗脫,流速1.0 m L/min。在30 min內(nèi)完成4種糖的色譜分離,并且得到了滿意的線性范圍(r0.9980,n=8),蔗糖、葡萄糖、甘露糖和果糖檢出限分別為0.300mg/L、0.114 mg/L、0.184 mg/L和1.164 mg/L。蔗糖、葡萄糖、甘露糖線性范圍為1.0~60.0 mg/L,果糖的線性范圍為5.0~80.0 mg/L。樣品的平均回收率為87.00%~107.60%。得到蔗糖,葡萄糖,甘露糖和果糖的日內(nèi)精密度分別為1.25%、0.68%、2.57%和3.74%,日間精密度分別為3.56%、2.09%、4.63%和5.87%。該分析方法綠色環(huán)保、靈敏度高、重復性好,可作為瓶裝綠茶飲料的質(zhì)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.
【學位授予單位】：西南大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.7;TS207.3

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