CN103980384A - Preparation method of water-soluble pectin of shaddock albedo - Google Patents
Preparation method of water-soluble pectin of shaddock albedo Download PDFInfo
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- 239000001814 pectin Substances 0.000 title claims abstract description 27
- 229920001277 pectin Polymers 0.000 title claims abstract description 27
- 235000010987 pectin Nutrition 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 5
- 235000001759 Citrus maxima Nutrition 0.000 title 1
- 244000276331 Citrus maxima Species 0.000 title 1
- 240000000560 Citrus x paradisi Species 0.000 claims abstract description 62
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000605 extraction Methods 0.000 claims abstract description 33
- 239000002244 precipitate Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000005119 centrifugation Methods 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 7
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000010178 pectin extract Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 12
- 239000002775 capsule Substances 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 5
- 238000003809 water extraction Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 231100000331 toxic Toxicity 0.000 abstract description 2
- 230000002588 toxic effect Effects 0.000 abstract description 2
- 238000002386 leaching Methods 0.000 abstract 1
- 235000013399 edible fruits Nutrition 0.000 description 6
- 238000000926 separation method Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 239000001606 7-[(2S,3R,4S,5S,6R)-4,5-dihydroxy-6-(hydroxymethyl)-3-[(2S,3R,4R,5R,6S)-3,4,5-trihydroxy-6-methyloxan-2-yl]oxyoxan-2-yl]oxy-5-hydroxy-2-(4-hydroxyphenyl)chroman-4-one Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 238000002481 ethanol extraction Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- DFPMSGMNTNDNHN-ZPHOTFPESA-N naringin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1[C@H](OC=2C=C3O[C@@H](CC(=O)C3=C(O)C=2)C=2C=CC(O)=CC=2)O[C@H](CO)[C@@H](O)[C@@H]1O DFPMSGMNTNDNHN-ZPHOTFPESA-N 0.000 description 1
- 229940052490 naringin Drugs 0.000 description 1
- 229930019673 naringin Natural products 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
一种柚子白囊水溶性果胶的制备方法，取柚子白囊烘干或自然晾干、切块，95%乙醇浸泡12h以上，烘干；采用热水浸提制备水溶性果胶，柚子白囊/水比1:10-1:50，温度60-100℃，浸提1-3次，每次时间1-5h，不断搅拌；浸提液过滤，得上清液；上清液浓缩至原体积的1/8-1/10，醇沉12h，3000r/min-4800r/min，5-10min离心收集沉淀，沉淀物40-55℃干燥，得到水溶性柚子白囊果胶。本发明实现柚子皮废弃物的重复利用，提高资源利用率；提取效率高，无需有毒、有害有机试剂，产品安全；工艺简单、应用前景广。A method for preparing grapefruit white sac water-soluble pectin. The white sac of grapefruit is dried or naturally dried, cut into pieces, soaked in 95% ethanol for more than 12 hours, and dried; hot water extraction is used to prepare water-soluble pectin, grapefruit white Capsule/water ratio 1:10-1:50, temperature 60-100°C, leaching 1-3 times, each time 1-5h, stirring constantly; extracting solution filtered to obtain supernatant; supernatant concentrated to 1/8-1/10 of the original volume, alcohol precipitation for 12 hours, 3000r/min-4800r/min, 5-10min centrifugation to collect the precipitate, and dry the precipitate at 40-55°C to obtain water-soluble pomelo alba pectin. The invention realizes the reuse of pomelo peel waste, improves the utilization rate of resources, has high extraction efficiency, does not need toxic and harmful organic reagents, and has safe products, simple process and wide application prospect.
Description
技术领域 technical field
本发明属食品加工领域。 The invention belongs to the field of food processing.
背景技术 Background technique
柚类果实以其果形硕大、果肉晶莹脆嫩、营养丰富、风味清香独特、耐贮运而深受广大消费者喜爱，仅我国就有200多个柚类品种，年产量超过100万吨。柚子皮约占整个柚子重量的40%，在日常生活中柚子皮却往往被人们直接丢弃。即使在工厂加工过程中，柚子皮仅仅是被简单的加工成果脯和蜜饯等产品，但是综合利用仍不够高。柚果果皮中，中果皮层（海绵层、白囊层）较厚，富含果胶。果胶作为一种高档的天然食品添加剂和保健品，可广泛应用于食品、医药保健品和一些化妆品中。柚皮果胶具有良好的生理活性作用，而且产品口感良好，还带有柚子特有的香味，很容易获得广大消费者的青睐。因此，若是对柚子皮中的果胶加以利用，可以极大提升柚子附加值，提高可再生资源的利用率。 Pomelo fruits are popular among consumers because of their large fruit shape, crystal clear and crisp flesh, rich nutrition, unique flavor and good storage and transportation resistance. There are more than 200 pomelo varieties in my country alone, with an annual output of more than 1 million tons. Grapefruit peel accounts for about 40% of the weight of the whole grapefruit, but grapefruit peel is often discarded directly by people in daily life. Even in the process of factory processing, pomelo peels are simply processed into products such as candied fruit and candied fruit, but the comprehensive utilization is still not high enough. In the pomelo fruit peel, the mesocarp layer (sponge layer, white sac layer) is thicker and rich in pectin. As a high-grade natural food additive and health product, pectin can be widely used in food, medicine and health products and some cosmetics. Pomelo peel pectin has good physiological activity, and the product has a good taste and a unique fragrance of grapefruit, which is easy to win the favor of consumers. Therefore, if the pectin in pomelo peel is utilized, it can greatly increase the added value of pomelo and improve the utilization rate of renewable resources.
中国专利CN1530376A于2004年9月22日公开了“从柚子中同时提取果胶、柚皮甙等八种产物的方法”，主要针对柚子全果中相关成分进行制备，分别采用冷磨法、压榨法、纳滤、微波或回流浸提、超滤浓缩、色谱分离、乙醇浸提等得到不同产物。中国专利CN102212145A于2011年10月12日公开了“柚子多糖的加工方法”，主要针对柚子皮和果渣混合物进行果胶提取，将上述混合物烘干、粉碎、水浸、酶解获得酶解液，然后采用压滤法获得酶解滤液，最后通过超滤、真空干燥获得柚子多糖。但尚未见专门针对柚子白囊果胶的提取工艺，同时上述专利中叙述的工艺流程较为复杂，降低经济效益。 Chinese patent CN1530376A disclosed on September 22, 2004 "a method for simultaneously extracting eight kinds of products such as pectin and naringin from pomelo", mainly for the preparation of related components in the whole fruit of pomelo, using cold grinding method, pressing Different products can be obtained by different methods such as nanofiltration, microwave or reflux extraction, ultrafiltration concentration, chromatographic separation, and ethanol extraction. Chinese patent CN102212145A disclosed "the processing method of pomelo polysaccharide" on October 12, 2011, mainly for the pectin extraction of the pomelo peel and pomace mixture, drying the above mixture, pulverizing, soaking in water, and enzymatic hydrolysis to obtain the enzymatic solution , and then the enzymolysis filtrate was obtained by pressure filtration, and finally the pomelo polysaccharide was obtained by ultrafiltration and vacuum drying. However, there is no specific extraction process for grapefruit white capsule pectin, and the technical process described in the above-mentioned patent is relatively complicated, which reduces economic benefits.
发明内容 Contents of the invention
本发明的目的在于提供一种柚子白囊水溶性果胶的制备方法，实现对柚子加工过程中产生的废弃物高效利用。 The purpose of the present invention is to provide a preparation method of pomelo white sac water-soluble pectin, so as to realize efficient utilization of the waste produced in the pomelo processing process.
本发明工艺步骤为： Process step of the present invention is:
（1）取柚子白囊烘干或自然晾干。 (1) Dry the pomelo white sac or dry it naturally.
（2）原料前处理：取干燥后的柚子白囊，将其切成块状，经95%乙醇浸泡12 h以上，过滤后置于烘箱中干燥，调节温度40-55℃，干燥10 h以上。 (2) Pre-treatment of raw materials: take the dried pomelo white sac, cut it into pieces, soak it in 95% ethanol for more than 12 hours, filter it and put it in an oven to dry, adjust the temperature to 40-55°C, and dry it for more than 10 hours .
（3）果胶浸提：将步骤（2）处理后的柚子白囊采用热水浸提制备水溶性果胶，柚子白囊/水的重量/体积（kg/L）比为1:10-1:50，浸提温度为60-100℃，浸提次数为1-3次，每次浸提时间为1-5 h，浸提过程中不断搅拌。 (3) Pectin extraction: extract the pomelo white sac treated in step (2) with hot water to prepare water-soluble pectin, the weight/volume (kg/L) ratio of pomelo white sac/water is 1:10- 1:50, the extraction temperature is 60-100°C, the number of extractions is 1-3 times, each extraction time is 1-5 h, and the extraction process is constantly stirred.
（4）将步骤（3）中提取得到的果胶浸提液进行过滤，采用纱布过滤，分离得到上层清液。 (4) Filter the pectin extract extracted in step (3), filter it with gauze, and separate to obtain the supernatant.
（5）将步骤（4）中分离得到的上层清液浓缩至原体积的1/8-1/10，再用乙醇沉淀，体系中的乙醇质量浓度控制在80%，醇沉12 h后，3000 r/min-4800 r/min离心收集沉淀，离心时间5-10 min；收集沉淀物置于烘箱中干燥，干燥温度控制在40-55℃，得到水溶性柚子白囊果胶。 (5) Concentrate the supernatant obtained in step (4) to 1/8-1/10 of the original volume, and then precipitate with ethanol. The mass concentration of ethanol in the system is controlled at 80%. After 12 hours of alcohol precipitation, The precipitate was collected by centrifugation at 3000 r/min-4800 r/min, and the centrifugation time was 5-10 min; the collected precipitate was dried in an oven, and the drying temperature was controlled at 40-55°C to obtain water-soluble pomelo alba pectin.
本发明步骤（3）所述的柚子白囊/水的重量/体积（kg/L）比优选为1:20-1:40，浸提温度优选为80-100℃，浸提次数为1-3次，每次浸提时间优选为2-4 h。 The weight/volume (kg/L) ratio of pomelo white sac/water described in step (3) of the present invention is preferably 1:20-1:40, the extraction temperature is preferably 80-100°C, and the extraction times are 1- 3 times, each extraction time is preferably 2-4 h.
本发明的优点是：1、实现柚子皮废弃物的重复利用，提高资源利用率；2、采用热水法提取水溶性果胶，提取效率高，无需有毒、有害有机试剂，产品安全；3、本方法的生成工艺简单、应用前景广。 The advantages of the present invention are: 1. Realize the reuse of pomelo peel waste and improve the utilization rate of resources; 2. Use the hot water method to extract water-soluble pectin, with high extraction efficiency, no need for toxic and harmful organic reagents, and product safety; 3. The production process of the method is simple and the application prospect is wide.
具体实施方式 Detailed ways
本发明将通过以下实施例作进一步说明。 The invention will be further illustrated by the following examples.
实施例1。 Example 1.
将柚子最外层皮剥离，露出白囊部分，然后再将白囊层从柚子上剥离下来，实现和果肉分离，将获得的白囊烘干。取干燥后的柚子白囊，将其切成块状，经95%乙醇浸泡12 h，过滤后置于烘箱中干燥，调节温度55℃，干燥10 h以上，然后采用热水浸提制备柚子白囊水溶性果胶，柚子白囊/水的重量/体积（kg/L）比为1:20，浸提温度为90oC，浸提1次，浸提时间为2 h，浸提过程中不断搅拌。提取得到的果胶浸提液进行过滤，采用纱布过滤，分离得到上层清液并浓缩至原体积的1/8，再用乙醇沉淀，体系中的乙醇质量浓度控制在80%，醇沉12 h后，离心收集沉淀（转速4000 r/min），离心10 min；收集沉淀置于烘箱中干燥，得柚子白囊水溶性果胶（得率为9.12%）。 The outermost skin of the grapefruit is peeled off to expose the white sac part, and then the white sac layer is peeled off from the pomelo to realize separation from the pulp, and the obtained white sac is dried. Take the dried pomelo white sac, cut it into pieces, soak it in 95% ethanol for 12 h, filter it and put it in an oven to dry at a temperature of 55°C, dry it for more than 10 h, and then use hot water extraction to prepare pomelo white Capsule water-soluble pectin, grapefruit white capsule/water weight/volume (kg/L) ratio is 1:20, extraction temperature is 90 o C, extraction time is 2 h, during the extraction process Stir constantly. The extracted pectin extract was filtered, filtered with gauze, and the supernatant was separated and concentrated to 1/8 of the original volume, and then precipitated with ethanol. The concentration of ethanol in the system was controlled at 80%, and alcohol precipitation was carried out for 12 h. Finally, the precipitate was collected by centrifugation (rotating speed 4000 r/min), and centrifuged for 10 min; the collected precipitate was dried in an oven to obtain water-soluble pectin of pomelo white sac (yield 9.12%).
实施例2。 Example 2.
将柚子最外层皮剥离，露出白囊部分，然后再将白囊层从柚子上剥离下来，实现和果肉分离，将获得的白囊烘干或自然晾干。取干燥后的柚子白囊，将其切成块状，经95%乙醇浸泡12 h，过滤后置于烘箱中干燥，调节温度55℃，干燥10 h以上，然后采用热水浸提制备柚子白囊水溶性果胶，柚子白囊/水的重量/体积（kg/L）比为1:30，浸提温度为90oC，浸提1次，浸提时间为4h，浸提过程中不断搅拌。提取得到的果胶浸提液进行过滤，采用纱布过滤，分离得到上层清液并浓缩至原体积的1/8，再用乙醇沉淀，体系中的乙醇质量浓度控制在80%，醇沉12 h后，离心收集沉淀（转速4800 r/min），离心10 min；收集沉淀置于烘箱中干燥，得柚子白囊水溶性果胶（得率为11.78%）。 The outermost skin of the pomelo is peeled off to expose the white sac part, and then the white sac layer is peeled off from the pomelo to realize separation from the pulp, and the obtained white sac is dried or dried naturally. Take the dried pomelo white sac, cut it into pieces, soak it in 95% ethanol for 12 h, filter it and put it in an oven to dry at a temperature of 55°C, dry it for more than 10 h, and then use hot water extraction to prepare pomelo white Capsule water-soluble pectin, grapefruit white capsule/water weight/volume (kg/L) ratio is 1:30, extraction temperature is 90 o C, extraction time is 4 hours, and the extraction process is continuous Stir. The extracted pectin extract was filtered, filtered with gauze, and the supernatant was separated and concentrated to 1/8 of the original volume, and then precipitated with ethanol. The concentration of ethanol in the system was controlled at 80%, and alcohol precipitation was carried out for 12 h. Finally, the precipitate was collected by centrifugation (4800 r/min), and centrifuged for 10 min; the collected precipitate was dried in an oven to obtain water-soluble pectin of pomelo white sac (yield 11.78%).
实施例3。 Example 3.
将柚子最外层皮剥离，露出白囊部分，然后再将白囊层从柚子上剥离下来，实现和果肉分离，将获得的白囊烘干或自然晾干。取干燥后的柚子白囊，将其切成块状，经95%乙醇浸泡12 h，过滤后置于烘箱中干燥，调节温度55℃，干燥10 h以上，然后采用热水浸提制备柚子白囊水溶性果胶，柚子白囊/水的重量/体积（kg/L）比为1:30，浸提温度为70oC，浸提1次，浸提时间为3 h，浸提过程中不断搅拌。提取得到的果胶浸提液进行过滤，采用纱布过滤，分离得到上层清液并浓缩至原体积的1/8，再用乙醇沉淀，体系中的乙醇质量浓度控制在80%，醇沉12 h后，离心收集沉淀（转速4800 r/min），离心10 min；收集沉淀置于烘箱中干燥，得柚子白囊水溶性果胶（得率为4.38%）。 The outermost skin of the pomelo is peeled off to expose the white sac part, and then the white sac layer is peeled off from the pomelo to realize separation from the pulp, and the obtained white sac is dried or dried naturally. Take the dried pomelo white sac, cut it into pieces, soak it in 95% ethanol for 12 h, filter it and put it in an oven to dry at a temperature of 55°C, dry it for more than 10 h, and then use hot water extraction to prepare pomelo white Capsule water-soluble pectin, grapefruit white capsule/water weight/volume (kg/L) ratio is 1:30, extraction temperature is 70 o C, extraction time is 3 h, extraction process Stir constantly. The extracted pectin extract was filtered, filtered with gauze, and the supernatant was separated and concentrated to 1/8 of the original volume, and then precipitated with ethanol. The concentration of ethanol in the system was controlled at 80%, and alcohol precipitation was carried out for 12 h. Finally, the precipitate was collected by centrifugation (4800 r/min), and centrifuged for 10 min; the collected precipitate was dried in an oven to obtain water-soluble pectin of pomelo white sac (yield 4.38%).
实施例4。 Example 4.
将柚子最外层皮剥离，露出白囊部分，然后再将白囊层从柚子上剥离下来，实现和果肉分离，将获得的白囊烘干或自然晾干。取干燥后的柚子白囊，将其切成块状，经95%乙醇浸泡12 h，过滤后置于烘箱中干燥，调节温度55℃，干燥10 h以上，然后采用热水浸提制备柚子白囊水溶性果胶，柚子白囊/水的重量/体积（kg/L）比为1:30，浸提温度为100oC，浸提2次，浸提时间为3h，浸提过程中不断搅拌。提取得到的果胶浸提液进行过滤，采用纱布过滤，分离得到上层清液并浓缩至原体积的1/8，再用乙醇沉淀，体系中的乙醇质量浓度控制在80%，醇沉12 h后，离心收集沉淀（转速4800 r/min），离心10 min；收集沉淀置于烘箱中干燥，得柚子白囊水溶性果胶（得率为22.04%）。 The outermost skin of the pomelo is peeled off to expose the white sac part, and then the white sac layer is peeled off from the pomelo to realize separation from the pulp, and the obtained white sac is dried or dried naturally. Take the dried pomelo white sac, cut it into pieces, soak it in 95% ethanol for 12 h, filter it and put it in an oven to dry at a temperature of 55°C, dry it for more than 10 h, and then use hot water extraction to prepare pomelo white Capsule water-soluble pectin, grapefruit white capsule/water weight/volume (kg/L) ratio is 1:30, extraction temperature is 100 o C, extraction is 2 times, extraction time is 3h, continuous extraction process Stir. The extracted pectin extract was filtered, filtered with gauze, and the supernatant was separated and concentrated to 1/8 of the original volume, and then precipitated with ethanol. The concentration of ethanol in the system was controlled at 80%, and alcohol precipitation was carried out for 12 h. Finally, the precipitate was collected by centrifugation (4800 r/min), and centrifuged for 10 min; the collected precipitate was dried in an oven to obtain water-soluble pectin of pomelo white sac (yield 22.04%).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN107033256A (en) * | 2017-05-25 | 2017-08-11 | 广东药科大学 | A kind of extracting method of citrus pectin polysaccharide |
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| CN106632725A (en) * | 2017-01-10 | 2017-05-10 | 涟源康麓生物科技有限公司 | Method for separating water-soluble pectin from pectin material rinsing solution |
| CN106632725B (en) * | 2017-01-10 | 2019-06-11 | 涟源康麓生物科技有限公司 | A method of separating water soluble pectin from pectin starting material rinsing liquid |
| CN107033256A (en) * | 2017-05-25 | 2017-08-11 | 广东药科大学 | A kind of extracting method of citrus pectin polysaccharide |
| CN107794169A (en) * | 2017-11-29 | 2018-03-13 | 韦俊超 | A kind of preparation method of clearing damp glutinous rice wine |
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