【作者】 李建敏；

【导师】 刘晓红；

【作者基本信息】 南昌大学 ， 化学工艺， 2007， 硕士

【摘要】 本文进行了先用微波协同浸提柑桔皮中色素，再从所得滤渣中回收浸提果胶，然后利用超声波辅助进一步浸提橙皮苷的联合工艺研究。研究表明：通过单因素分析和正交实验，对微波协同浸提柑桔皮中色素的提取工艺进行优化研究，重点考察了原料破碎度、液料比、微波功率、辐射时间、浸提级数等因素对色素吸光度和浸提率的影响。微波协同浸提色素的最佳工艺条件为：破碎度40目，乙醇浓度100％，浸提液料比为5ml／g，微波功率25％×700W，辐射时间10min，浸提级数3级。在优化条件下，3级浸提平均浸提率达17.5％；考察了AB-8大孔树脂吸附精制对色素色价的影响，精制后色价从70.57升为164.29。产品色素通过显色反应和紫外可见吸收光谱表征，分析检测理化限量指标表明产品合格。与直接水浴加热提取法比较，微波协同浸提不仅大大缩短浸取时间，而且提高了色素浸取率和品质。浸提色素后的滤渣，通过微波协同酒石酸浸提、乙醇沉析得到果胶。以精制果胶浸提率和胶凝单元数为评价指标，单因素分析结合正交实验L₉（3⁴）筛选工艺条件为：浸提剂酒石酸，液料比10ml／g，浸提pH=2.0，微波功率280W，辐射时间5min，浸提级数3级，浓缩比为4：1，乙醇浓度60％，沉析时间60min。按优选的工艺条件实验3次，果胶平均浸提率达21.77％。通过红外光谱表征及质量检测表明产品合格。酒石酸浸提果胶产品品质好，浸提率高；微波法快速、节能、浸提率更高。浸提果胶后的滤渣，在超声波作用下，利用饱和Ca（OH）₂碱液浸提盐酸酸析得到橙皮苷，通过单因素分析和正交实验确定了超声波协同浸提橙皮苷的各因素影响主次为：碱提pH值＞液料比＞酸析pH值＞超声时间。最佳工艺条件为：碱提pH=12.5，液料比10：1，超声时间60min，酸析pH=4.7，浸提级数3级。另外，考察了重结晶法精制对橙皮苷纯度的影响，平均纯度为94.96％，提高14.72％。红外光谱、高效液相色谱等方法表征实验产品，检测产品质量并对照行业标准表明合格。通过此联合工艺可获得浸提率较高的色素、果胶和橙皮苷产品，且均符合国家或行业有关标准。该工艺具有效率高、能耗低、污染小，设备及操作简单，经济效益好等优点，对于综合开发利用柑桔皮具有较高的参考及应用价值。更多还原

【Abstract】 This article mostly discusses combined technology that firstly microwave assiststo extract pigment from tangerine peels, then recoveries and extracts pectin from filterresidue after pigment’s extraction, finally further extract hesperidin under use ofultrasonic wave. Researches indicate:Through single factor analysis and orthogonal design optimizational methods,extractive technology which obtains pigment from tangerine peels with microwave’ssynergism is optimized. Some factors such as degree of raw material’s fragmentation,ratio of solvent to material, radiative time, extractive times and so on, whose influenceon absorbancy and extractive percentage of pigment are mainly considered, and thebest craft conditions are obtained and defined, which are raw material’s fragmentation40 eyes, ethanol concentration 100％, ratio of solvent to material 5 ml/g, microwavepower 25％×700W, radiation time 10min, extractive times 3. Under optimizationalconditions, average extractive percentage reaches 17.5％; In addition, effect of AB-8macroporous resin purification on colour rate of pigment is inspected, colour rate isincreased from 70.57 to 164.29 through purification. Product’s attribute ischaracterized with methods like colour reaction and UV-vis spectroscopy, and itscontrolled indexes are also detected. The analysis test result indicates that product isqualified. Compare to direct water-bath heating extraction, microwave assistedextraction not only greatly reduces extractive time, but also increace yield and qulityof pigment.Second step, microwave accessories tartaric acid to extract then ethanol separatesand deposits pectin. Basing evaluation criterion on pectin’s extractive percentage andgelling cell data, and making use of single factor analysis combining with orthogonalexperiment L₉（3⁴） to screen craft conditions: tartaric acid as extractive solvent, ratio ofsolvent to material 10ml/g, extractive pH value 2.0, microwave power 280W, radiativetime 5min, extractive times 3, enriched ratio 4:1, ethanol concentration 60％,depositional time 60min. According to optimizational conditions, 3 times experiments are operated and average extractive percentage reaches 21.77％. The obtained result ofinfra-red spectrometry and quality detection indicates product is qualified. Tartaricacid as solvent to extract pectin has good quality and high yield; Microwave assistedextraction owns advantages of fast, energy-saving and higher yield.Ultrasonic accessories Ca（OH）₂ alkali to extract then hydrochloric acid separatesand precipitates hesperidin from obtained filter residue after pectic extraction, andunder use of single factor analysis and orthogonal design optimizational methods,principle sequence of factors’ influences is defined: pH value of alkali＞ratio of solventto material＞pH value of acid＞ultrasonic time. The best technology conditions are:pH value of alkali 12.5, ratio of solvent to material 10:1, ultrasonic time 60min, pHvalue of acid 4.7, extractive times 3. Otherwise, effect of recrystallized purification oncontent of hesperidin is researched, and average percentage purity increases 14.72％.Product is detected and characterized with methods like infra-red, high performanceliquid chromatography spectrometry, etc. Comparation to industry related standardshows product is qualify.Not only higher yield pigment, pectin and hesperidin products are obtainedthrough this combined technology, but also their qualites are all conformed to thenational and industry related standard. The craft has many advantages such as highefficiency, low energy consumption, little pollution, easy equipment and operation,rich economic performance, etc. Therefore comprehensive development and utilizationof tangerine peels has higher reference and applicational value.更多还原