CN102399302A - Ultrasonic extraction method of pectin - Google Patents
Ultrasonic extraction method of pectin Download PDFInfo
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- CN102399302A CN102399302A CN201110338104XA CN201110338104A CN102399302A CN 102399302 A CN102399302 A CN 102399302A CN 201110338104X A CN201110338104X A CN 201110338104XA CN 201110338104 A CN201110338104 A CN 201110338104A CN 102399302 A CN102399302 A CN 102399302A
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- pectin
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- 229920001277 pectin Polymers 0.000 title claims abstract description 28
- 235000010987 pectin Nutrition 0.000 title claims abstract description 28
- 239000001814 pectin Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000002137 ultrasound extraction Methods 0.000 title abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 244000017020 Ipomoea batatas Species 0.000 claims abstract description 7
- 235000002678 Ipomoea batatas Nutrition 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 5
- 238000001471 micro-filtration Methods 0.000 claims abstract description 5
- 239000000049 pigment Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000001105 regulatory effect Effects 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 102000004190 Enzymes Human genes 0.000 claims abstract description 3
- 108090000790 Enzymes Proteins 0.000 claims abstract description 3
- 230000003625 amylolytic effect Effects 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 244000061456 Solanum tuberosum Species 0.000 claims description 15
- 235000002595 Solanum tuberosum Nutrition 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 15
- 239000002893 slag Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 235000019698 starch Nutrition 0.000 claims description 6
- 239000008107 starch Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 150000003384 small molecules Chemical class 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 3
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000000874 microwave-assisted extraction Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 2
- MYKOKMFESWKQRX-UHFFFAOYSA-N 10h-anthracen-9-one;sulfuric acid Chemical compound OS(O)(=O)=O.C1=CC=C2C(=O)C3=CC=CC=C3CC2=C1 MYKOKMFESWKQRX-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 244000276331 Citrus maxima Species 0.000 description 1
- 235000001759 Citrus maxima Nutrition 0.000 description 1
- AEMOLEFTQBMNLQ-BKBMJHBISA-N alpha-D-galacturonic acid Chemical compound O[C@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-BKBMJHBISA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses an ultrasonic extraction method of pectin. The method is characterized by comprising the following steps of: adding amylolytic enzyme in sweet potato residue serving as raw material and containing pectin for hydrolysis, centrifuging, collecting centrifugate and adding the centrifugate to ultrasonic extraction equipment, and regulating PH value to be acidic and then carrying out microwave extraction; centrifuging, carrying out microfiltration, taking supernate, carrying out ultrafiltration and concentration, removing micro-molecular and pigment impurities, adding ethanol in concentrated solution so that the concentration reaches 75%, then completely stirring, washing and centrifuging, collecting centrifugate, namely pectin; and finally drying. The method has the advantages of reducing production cost and improving product quality and is convenient to operate industrially.
Description
Technical field
The present invention relates to a kind of pectin extraction method, relate in particular to a kind of method of utilizing ultrasonic continuous countercurrent extraction technology to extract pectin in the potato slag.
Background technology
To be sweet potato extracting starch to the potato slag, the tankage that produce when processing and fabricating bean vermicelli, vermicelli and other by-products.Sweet potato is extracted the potato slag that produces behind the starch, accounts for the 10%-14% of raw material, perhaps directly abandons yet generation a large amount of potato slags in extraction back are mainly used in animal-feed, and major part does not obtain development and use, not only causes the waste resource, also causes contaminate environment.Discover and contain abundant pectin in the potato slag, and Functionality, quality and appealing design, be good pectin source.China is maximum in the world sweet potato producing country, and raw material sources are abundant.
Pectin is water miscible; Utilize this character to arrive so far; The method of the extraction pectin from sweet potato residue, potato residues, Pericarpium Mali pumilae, Pericarpium Musae, shaddock ped etc. of research both at home and abroad is more; Mainly contain simple sour formulation, ion-exchange-resin process, microbial method, microwave method etc., but all be in the research level, do not accomplish scale production.And it is lower that simple acid extraction method extracts pectin efficient, and technology is also in constantly developing; Ion-exchange-resin process extracts pectin owing to receive between polyvalent cation, fibrous pectic substance macromole and other polymeric mechanicalness is impeded the quality that influences pectin.
The present invention takes ultrasonic method to extract, and ultrasonic method is used for the extraction of natural component, and selectivity is strong, solvent consumption is little, the running time is short, solvent consumption target components yield high, and can keep the natural radioactivity of natural component greatly.Along with the development of electronic technology and automatic industrial, make ultransonic application increasingly mature, its advantage be produce step simplify, simple to operate, level of automation is high.Ultrasonic extracting method meets the requirement of following food, medicine and healthcare products industry, is modern food, medicine and healthcare products industrial expansion direction.
Summary of the invention
The technical problem that the present invention will solve provides a kind of method of utilizing the ultrasonic continuous countercurrent extractive technique to extract pectin in the potato slag.This method can reduce production costs, and improves the quality of products, and is convenient to the industriallization operation.
In order to solve the problems of the technologies described above, it is following that the present invention proposes technical scheme:
Technical scheme of the present invention is:
The material potato slag that will contain pectin adds amylolytic enzyme and is hydrolyzed, and is centrifugal, collects centrifugal thing and puts in the supersound extraction equipment, and it is acid regulating pH value, carries out supersound extraction; Centrifugal, micro-filtration is got supernatant, and ultrafiltration and concentration is removed small molecules and pigment impurity again, in liquid concentrator, adds ethanol, and making determining alcohol is 75%, fully stirs, and washing is also centrifugal, and collecting centrifugal thing is pectin, and drying promptly gets.
In a container, put the solvent of 5～30 times of potato slag raw materials quality, soaking at room temperature 0.5～5 hour.
Solvent is one or more combinations in water, methyl alcohol, ethanol, acetone, ether, the methylene dichloride equal solvent.
Ultrasonic frequency is 10～80KHZ, extracts 40～90 ℃ of temperature, extraction time 10～60min.
Filtrating PH is that acidity is meant that PH is 1-6, and used acid is hydrochloric acid, sulfuric acid, nitric acid or mixing acid.
The tankage that starch is made back generations such as bean vermicelli, vermicelli are extracted for sweet potato processing in potato slag source.
The present invention adopts ultra extractive technique, owing to adopt ultrasonic organic solution circulation method to extract, has homogeneous heating, fast, is easy to Instantaneous Control, environmental protection characteristics, and extraction time and solvent load are saved greatly, and efficient is high, output is big, has reduced production cost; Supersound extraction is a consumer, need not be equipped with boiler, pollution-free, safely, belong to green engineering.
Embodiment
Embodiment
Embodiment 1
Get potato slag 100g, add glycase, remove remaining starch at 80 ℃ of hydrolysis 30min, centrifugal, collect centrifugal thing; Adding water 1000ml, to make into solid-liquid ratio be 1: 10 suspension, and take ultrasonic extraction to extract pectin: ultrasonic power is 15KHz, and regulating pH value is 2.0, extracts 15 minutes, centrifugal; Micro-filtration (filter opening is 0.8 μ m) is got supernatant, and ultrafiltration and concentration is removed small molecules and pigment impurity again; In liquid concentrator, add ethanol, making determining alcohol is 75%, fully stirs, and washing is also centrifugal; Collecting centrifugal thing is pectin, and vacuum-drying gets pectin dry product 8g, and the sulfuric acid anthrone method is checked, and gets the pectin finished product of content >=70%.
Embodiment 2
Get potato slag 100g, add glycase, remove remaining starch at 60 ℃ of hydrolysis 30min, centrifugal, collect centrifugal thing; Adding water 500ml and ethanol 500ml, to make into solid-liquid ratio be 1: 10 suspension, and take ultrasonic extraction to extract pectin: ultrasonic power is 30KHz, and regulating pH value is 2.0, extracts 15 minutes, centrifugal; Micro-filtration (filter opening is 0.8 μ m) is got supernatant, and ultrafiltration and concentration is removed small molecules and pigment impurity again; In liquid concentrator, add ethanol, making determining alcohol is 75%, fully stirs, and washing is also centrifugal; Collecting centrifugal thing is pectin, and vacuum-drying gets pectin dry product 11g, and the sulfuric acid anthrone method is checked, and gets the pectin finished product of content >=70%.
Claims (6)
1. extracting pectin; It is characterized in that described method comprises the following steps: that the material potato slag that contains pectin is added amylolytic enzyme to be hydrolyzed, centrifugal, collect centrifugal thing and put in the supersound extraction equipment; It is acid regulating pH value, carries out supersound extraction; Centrifugal, micro-filtration is got supernatant, and ultrafiltration and concentration is removed small molecules and pigment impurity again, in liquid concentrator, adds ethanol, and making determining alcohol is 75%, fully stirs, and washing is also centrifugal, and collecting centrifugal thing is pectin, and drying promptly gets.
2. process for extracting according to claim 1 is characterized in that: in a container, put the solvent of 5～30 times of potato slag raw materials quality, soaking at room temperature 0.5～5 hour.
3. process for extracting according to claim 1 is characterized in that described solvent is one or more combinations in water, methyl alcohol, ethanol, acetone, ether, the methylene dichloride equal solvent.
4. process for extracting according to claim 1 is characterized in that said ultrasonic frequency is 10～80KHZ, extracts 40～90 ℃ of temperature, extraction time 10～60min.
5. process for extracting according to claim 1 is characterized in that said adjusting filtrating PH is that acidity is meant that PH is 1-6, and used acid is hydrochloric acid, sulfuric acid, nitric acid or mixing acid.
6. process for extracting according to claim 1 is characterized in that described potato slag source makes the tankage of back generations such as bean vermicelli, vermicelli for sweet potato processing extraction starch.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610000917.0A CN105418793A (en) | 2011-10-31 | 2011-10-31 | Method for extracting pectin |
| CN201110338104.XA CN102399302B (en) | 2011-10-31 | 2011-10-31 | A kind of ultrasonic extracting method of pectin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110338104.XA CN102399302B (en) | 2011-10-31 | 2011-10-31 | A kind of ultrasonic extracting method of pectin |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610000917.0A Division CN105418793A (en) | 2011-10-31 | 2011-10-31 | Method for extracting pectin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102399302A true CN102399302A (en) | 2012-04-04 |
| CN102399302B CN102399302B (en) | 2016-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610000917.0A Pending CN105418793A (en) | 2011-10-31 | 2011-10-31 | Method for extracting pectin |
| CN201110338104.XA Expired - Fee Related CN102399302B (en) | 2011-10-31 | 2011-10-31 | A kind of ultrasonic extracting method of pectin |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610000917.0A Pending CN105418793A (en) | 2011-10-31 | 2011-10-31 | Method for extracting pectin |
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| CN (2) | CN105418793A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304681A (en) * | 2013-06-20 | 2013-09-18 | 中国农业科学院农产品加工研究所 | Method for extracting pectin |
| CN104086667A (en) * | 2014-06-11 | 2014-10-08 | 安徽农业大学 | Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction |
| CN104513324A (en) * | 2014-12-17 | 2015-04-15 | 广西壮族自治区农业科学院农产品加工研究所 | Method for extracting pectin from pitaya stem |
| CN105566512A (en) * | 2015-12-14 | 2016-05-11 | 山东省果树研究所 | Extracting method of persimmon fruit pectin |
| CN106519067A (en) * | 2016-11-19 | 2017-03-22 | 朱莉 | Comprehensive utilization method for sweet potato residues |
| CN108641014A (en) * | 2018-05-23 | 2018-10-12 | 广东医科大学 | A kind of clausenae Lansium pectin preparation method and the clausenae Lansium pectin using this method preparation |
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| JP3511952B2 (en) * | 1999-01-19 | 2004-03-29 | 不二製油株式会社 | Pectin, its production method, acidic protein food using the same, and its production method |
| CN101041699A (en) * | 2006-03-22 | 2007-09-26 | 中国农业科学院农产品加工研究所 | Sweet potato pectin and production technique thereof |
| CN101805416A (en) * | 2010-03-16 | 2010-08-18 | 上海交通大学 | Preparation method of canna edulis ker pectin |
| CN101942036A (en) * | 2009-07-08 | 2011-01-12 | 李浩贤 | Method for extracting pectin from pineapple peel assisted by ultrasonic wave |
| CN101891840B (en) * | 2010-08-09 | 2012-03-14 | 黑龙江北大荒斯达奇生物科技有限公司 | Method for extracting pectin by utilizing potato scraps |
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| DK2014682T3 (en) * | 2006-03-17 | 2014-09-08 | Fuji Oli Company Ltd | PROCEDURE FOR THE PRODUCTION OF PECTIN AND GELING AGENT AND GELATINO'S FOOD UNDER ITS APPLICATION |
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2011
- 2011-10-31 CN CN201610000917.0A patent/CN105418793A/en active Pending
- 2011-10-31 CN CN201110338104.XA patent/CN102399302B/en not_active Expired - Fee Related
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| JP3511952B2 (en) * | 1999-01-19 | 2004-03-29 | 不二製油株式会社 | Pectin, its production method, acidic protein food using the same, and its production method |
| CN101041699A (en) * | 2006-03-22 | 2007-09-26 | 中国农业科学院农产品加工研究所 | Sweet potato pectin and production technique thereof |
| CN101942036A (en) * | 2009-07-08 | 2011-01-12 | 李浩贤 | Method for extracting pectin from pineapple peel assisted by ultrasonic wave |
| CN101805416A (en) * | 2010-03-16 | 2010-08-18 | 上海交通大学 | Preparation method of canna edulis ker pectin |
| CN101891840B (en) * | 2010-08-09 | 2012-03-14 | 黑龙江北大荒斯达奇生物科技有限公司 | Method for extracting pectin by utilizing potato scraps |
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| 李新华等: "《粮油加工工艺学》", 30 September 2011, article ""粮油加工工艺学"", pages: 294 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304681A (en) * | 2013-06-20 | 2013-09-18 | 中国农业科学院农产品加工研究所 | Method for extracting pectin |
| CN103304681B (en) * | 2013-06-20 | 2016-03-16 | 中国农业科学院农产品加工研究所 | A kind of method extracting pectin |
| CN104086667A (en) * | 2014-06-11 | 2014-10-08 | 安徽农业大学 | Method for preparing pectin from citrus fruit peel residues by employing ultrasonic-assisted extraction |
| CN104513324A (en) * | 2014-12-17 | 2015-04-15 | 广西壮族自治区农业科学院农产品加工研究所 | Method for extracting pectin from pitaya stem |
| CN105566512A (en) * | 2015-12-14 | 2016-05-11 | 山东省果树研究所 | Extracting method of persimmon fruit pectin |
| CN105566512B (en) * | 2015-12-14 | 2018-03-30 | 山东省果树研究所 | A kind of extracting method of persimmon fruit pectin |
| CN106519067A (en) * | 2016-11-19 | 2017-03-22 | 朱莉 | Comprehensive utilization method for sweet potato residues |
| CN108641014A (en) * | 2018-05-23 | 2018-10-12 | 广东医科大学 | A kind of clausenae Lansium pectin preparation method and the clausenae Lansium pectin using this method preparation |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105418793A (en) | 2016-03-23 |
| CN102399302B (en) | 2016-06-01 |
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