CN109223993B - Method for extracting saponin from fruit and vegetable processing waste - Google Patents
Method for extracting saponin from fruit and vegetable processing waste Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/899—Poaceae or Gramineae (Grass family), e.g. bamboo, corn or sugar cane
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/72—Rhamnaceae (Buckthorn family), e.g. buckthorn, chewstick or umbrella-tree
- A61K36/725—Ziziphus, e.g. jujube
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
The invention discloses a method for extracting saponin from fruit and vegetable processing waste, belonging to the technical fields of food processing, active ingredient extraction and nano materials. The method comprises the following specific steps: preparing a micropore-mesopore extraction auxiliary agent Cu-MOF-74; and carrying out subcritical extraction on saponin in the fruit and vegetable processing waste by using the extraction aid Cu-MOF-74. The product is simple in preparation process and can be produced in large scale, the MOF is used as an extractant for subcritical extraction of the saponin, the extraction efficiency is high, the treatment cost of the fruit and vegetable processing waste is greatly reduced, the pollution of the fruit and vegetable processing waste to the environment is reduced, and the method has potential application value and economic and social benefits.
Description
Technical Field
The invention relates to a method for extracting saponin from fruit and vegetable processing waste, belonging to the technical field of food processing, active ingredient extraction and nano materials.
Background
China is the largest fruit and vegetable product processing country in the world, and the fruit and vegetable industry is the second largest agricultural support industry second to the food industry. In the deep processing process of fruits and vegetables, a large amount of processing waste is often generated, such as fallen fruits, unqualified fruits and a large amount of leftovers. For example, in the asparagus processing (asparagus can), a large amount of leftovers such as old stems, bamboo shoot skins and the like account for about 40 percent and are about 100 ten thousand tons. The waste (old stem, bamboo shoot skin, and defective bamboo shoot) generated in the processing process contains a large amount of active substances, such as polysaccharide, flavone, saponin, etc. But most of the wastes are discarded, which causes resource waste and environmental pollution. Meanwhile, a large amount of industrial wastewater is generated in the procedures of cleaning and the like in the processing process, and the wastewater also contains rich bioactive components. In recent years, more and more researchers pay attention to the extraction of active ingredients in fruit and vegetable processing wastes, but the problems that the extraction technology is not environment-friendly, the solvent extraction is mainly adopted, the energy consumption is high, the extraction rate is low, the loss of the active ingredients is serious, the applicability of the existing extraction, purification and detection technology method is not strong, the analysis and detection technology of partial active ingredients is lacked and the like exist. Therefore, research on extracting active substances from the fruit and vegetable processing waste realizes changing waste into valuable, and not only can the environment be protected, but also the economic value of the fruit and vegetable can be increased.
In recent years, the subcritical extraction technology has the advantages of environmental protection, energy conservation, safety, high extraction rate, full material utilization, suitability for large-scale production and the like, and is a novel separation technology developed after the supercritical extraction technology. Presently, the definition of subcritical fluids in the extraction industry is the state of a fluid having a temperature above the boiling point below the critical point and a pressure below the critical pressure. In this state, the extraction conditions are relatively mild, and the extraction temperature is low, so that the activity of the heat-sensitive substances is well retained. The process technology is simple and easy to operate, has high extraction speed, is safe and environment-friendly, has wide application prospect, and has been widely applied to the aspects of functional grease extraction, natural product extraction, active substance extraction and the like.
Metal-organic frameworks (MOFs) have a three-dimensional porous structure, are products of combination of subjects such as structural chemistry, material chemistry, organic chemistry, crystal engineering and the like, become a new research field, and are widely applied to scientific researches such as emerging energy sources and catalytic separation. To date, countless MOFs have been synthesized and, due to their incomparable physicochemical characteristics, have become one of the most attractive new materials. The metal-organic framework has a far-reaching development prospect in the field of separation and purification, but the application of the metal-organic framework in subcritical extraction of saponin is not reported, so that a new idea is provided for further expanding the application value of the metal-organic framework.
Disclosure of Invention
The technical task of the invention is to make up the defects of the prior art, and provide a method for extracting saponin from fruit and vegetable processing waste.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for extracting saponin from fruit and vegetable processing waste comprises the following steps:
cleaning and drying the fruit and vegetable processing waste, crushing the fruit and vegetable processing waste by a crusher, and sieving the crushed fruit and vegetable processing waste by a 100-mesh sieve to obtain fruit and vegetable processing waste powder;
mixing the fruit and vegetable processing waste powder and ethanol in a mass ratio of 1:20, and uniformly stirring to prepare an ethanol solution of the fruit and vegetable processing waste;
blending 2.8-4.0g of extraction aid Cu-MOF-74 with 80-120mL of ethanol solution of fruit and vegetable processing waste, uniformly stirring, transferring to a reaction kettle, heating the reaction kettle to 70-100 ℃, performing subcritical extraction for 15-25min, standing, cooling, and performing suction filtration to obtain an ethanol extract with a solid of Cu-MOF-74 and a liquid of saponin;
adding ethanol into solid Cu-MOF-74, performing ultrasonic treatment for 10min, centrifuging, mixing the supernatant with ethanol extractive solution of saponin, distilling to recover ethanol, aging the obtained concentrated solution, washing separated saponin with water, and drying at 70-80 deg.C to obtain saponin extract;
the mass ratio of the filtered Cu-MOF-74 to the ethanol is 1: 10;
the Cu-MOF-74 is activated at 85 ℃ overnight and then is repeatedly used;
detecting the content of total saponin to 68-73% by spectrophotometry.
The method for extracting saponin from the fruit and vegetable processing waste is selected from one of the following steps: asparagus processing waste, soybean dregs and spina date seeds.
In the method for extracting saponin from fruit and vegetable processing waste, the extraction aid Cu-MOF-74 has a chemical formula: cu2(dhBDC)(H2O)10；
The dhBDC has the structural formula as follows:
the extraction aid Cu-MOF-74 is prepared by the following steps:
0.15g of 2, 5-dihydroxy-1, 4-terephthalic acid is dissolved in 1.5-2mL of a mixed solution of DMF and water with the volume ratio of 1: 1; dissolving 0.5g of copper nitrate in 0.8-1.2mL of water; and violently shaking the two solutions into gel, aging at 85 ℃ overnight, washing with DMF, water and ethanol for 3 times in sequence, and activating at 85 ℃ to constant weight to obtain the extraction aid Cu-MOF-74 with the yield of 78-83%.
The above required raw materials are all purchased in the local chemical industry market.
The beneficial technical effects of the invention are as follows:
1. the invention provides a method for subcritical extraction of saponins in fruit and vegetable processing waste by a metal-organic framework Cu-MOF-74, which has the advantages of simple equipment, easiness in operation, energy and time saving, greatly shortens the extraction time compared with the traditional solvent extraction and reflux extraction, and effectively avoids the saponins from being decomposed by heating.
2 the metal organic framework Cu-MOF-74 extractant used in the invention has a permanent microporous structure in the framework, and forms a mesoporous and macroporous structure formed by nano particles with the particle size of 35-45nm due to the preparation of a gel method, and the extractant has high specific surface area and a plurality of active sites, and is adsorbed with fruit and vegetable waste at a plurality of sites, so that the extraction time is short, and the extraction rate is increased.
3. Metal-organic framework NH used in the invention2MIL-101, the gel method is easy to prepare and operate, and compared with a commonly adopted hydrothermal method, the gel method is energy-saving and time-saving.
Detailed Description
The present invention is further described with reference to the following examples, but the scope of the present invention is not limited to the examples, and modifications made by those skilled in the art to the technical solutions of the present invention should fall within the scope of the present invention.
Example 1 preparation method of extraction aid Cu-MOF-74
0.15g of 2, 5-dihydroxy-1, 4-terephthalic acid is dissolved in 1.5mL of a mixed solution of DMF and water in a volume ratio of 1: 1; 0.5g of copper nitrate was dissolved in 0.8mL of water; and violently shaking the two solutions into gel, aging at 85 ℃ overnight, washing with DMF, water and ethanol for 3 times in sequence, and activating at 85 ℃ to constant weight to obtain the extraction aid Cu-MOF-74 with the yield of 78%.
Example 2 preparation method of extraction aid Cu-MOF-74
0.15g of 2, 5-dihydroxy-1, 4-terephthalic acid is dissolved in 2mL of a mixed solution of DMF and water in a volume ratio of 1: 1; 0.5g of copper nitrate was dissolved in 1.2mL of water; and violently shaking the two solutions into gel, aging at 85 ℃ overnight, washing with DMF, water and ethanol for 3 times in sequence, and activating at 85 ℃ to constant weight to obtain the extraction aid Cu-MOF-74 with the yield of 80%.
Example 3 preparation method of extraction aid Cu-MOF-74
0.15g of 2, 5-dihydroxy-1, 4-terephthalic acid is dissolved in 1.7mL of a mixture of DMF and water in a volume ratio of 1: 1; 0.5g of copper nitrate was dissolved in 1.0mL of water; and violently shaking the two solutions into gel, aging at 85 ℃ overnight, washing with DMF, water and ethanol for 3 times in sequence, and activating at 85 ℃ to constant weight to obtain the extraction aid Cu-MOF-74 with the yield of 83%.
Example 4. the extraction aid, Cu-MOF-74, described in examples 1-3, has the formula: cu2(dhBDC)(H2O)10；
The dhBDC has the structural formula as follows:
embodiment 5A method for extracting saponins from fruit and vegetable processing waste
Cleaning and drying the fruit and vegetable processing waste, crushing the fruit and vegetable processing waste by a crusher, and sieving the crushed fruit and vegetable processing waste by a 100-mesh sieve to obtain fruit and vegetable processing waste powder;
mixing the fruit and vegetable processing waste powder and ethanol in a mass ratio of 1:20, and uniformly stirring to prepare an ethanol solution of the fruit and vegetable processing waste;
2.8-4.0g of the extraction aid Cu-MOF-74 prepared in the example 1 and 80-120mL of an ethanol solution of fruit and vegetable processing waste are mixed, uniformly stirred, transferred to a reaction kettle, heated to 70-100 ℃, subjected to subcritical extraction for 15-25min, placed, cooled and filtered to obtain an ethanol extraction solution with a solid of Cu-MOF-74 and a liquid of saponin;
adding ethanol into solid Cu-MOF-74, performing ultrasonic treatment for 10min, centrifuging, mixing the supernatant with ethanol extractive solution of saponin, distilling to recover ethanol, aging the obtained concentrated solution, washing separated saponin with water, and drying at 70-80 deg.C to obtain saponin extract;
detecting the content of total saponin to 68% by spectrophotometry;
the mass ratio of the filtered Cu-MOF-74 to the ethanol is 1: 10;
the Cu-MOF-74 is activated at 85 ℃ overnight and then is repeatedly used;
the fruit and vegetable processing waste is selected from one of the following: asparagus processing waste, soybean dregs and spina date seeds.
Embodiment 6A method for extracting saponins from fruit and vegetable processing waste
Cleaning and drying the fruit and vegetable processing waste, crushing the fruit and vegetable processing waste by a crusher, and sieving the crushed fruit and vegetable processing waste by a 100-mesh sieve to obtain fruit and vegetable processing waste powder;
mixing the fruit and vegetable processing waste powder and ethanol in a mass ratio of 1:20, and uniformly stirring to prepare an ethanol solution of the fruit and vegetable processing waste;
2.8-4.0g of the extraction aid Cu-MOF-74 prepared in the example 2 and 80-120mL of an ethanol solution of fruit and vegetable processing waste are mixed, uniformly stirred, transferred to a reaction kettle, heated to 70-100 ℃, subjected to subcritical extraction for 15-25min, placed, cooled and filtered to obtain an ethanol extraction solution with a solid of Cu-MOF-74 and a liquid of saponin;
adding ethanol into solid Cu-MOF-74, performing ultrasonic treatment for 10min, centrifuging, mixing the supernatant with ethanol extractive solution of saponin, distilling to recover ethanol, aging the obtained concentrated solution, washing separated saponin with water, and drying at 70-80 deg.C to obtain saponin extract;
detecting the content of total saponin to 73% by spectrophotometry;
the mass ratio of the filtered Cu-MOF-74 to the ethanol is 1: 10;
the Cu-MOF-74 is activated at 85 ℃ overnight and then is repeatedly used;
the fruit and vegetable processing waste is selected from one of the following: asparagus processing waste, soybean dregs and spina date seeds.
Example 7 method for extracting saponins from fruit and vegetable processing waste
Cleaning and drying the fruit and vegetable processing waste, crushing the fruit and vegetable processing waste by a crusher, and sieving the crushed fruit and vegetable processing waste by a 100-mesh sieve to obtain fruit and vegetable processing waste powder;
mixing the fruit and vegetable processing waste powder and ethanol in a mass ratio of 1:20, and uniformly stirring to prepare an ethanol solution of the fruit and vegetable processing waste;
2.8-4.0g of the extraction aid Cu-MOF-74 prepared in the example 3 and 80-120mL of an ethanol solution of fruit and vegetable processing waste are mixed, uniformly stirred, transferred to a reaction kettle, heated to 70-100 ℃, subjected to subcritical extraction for 15-25min, placed, cooled and filtered to obtain an ethanol extraction solution with a solid of Cu-MOF-74 and a liquid of saponin;
adding ethanol into solid Cu-MOF-74, performing ultrasonic treatment for 10min, centrifuging, mixing the supernatant with ethanol extractive solution of saponin, distilling to recover ethanol, aging the obtained concentrated solution, washing separated saponin with water, and drying at 70-80 deg.C to obtain saponin extract;
detecting the total saponin content to 70% by spectrophotometry;
the mass ratio of the filtered Cu-MOF-74 to the ethanol is 1: 10;
the Cu-MOF-74 is activated at 85 ℃ overnight and then is repeatedly used;
the fruit and vegetable processing waste is selected from one of the following: asparagus processing waste, soybean dregs and spina date seeds.
Claims (1)
1. A method for extracting saponin from fruit and vegetable processing waste is characterized by comprising the following steps:
cleaning and drying the fruit and vegetable processing waste, crushing the fruit and vegetable processing waste by a crusher, and sieving the crushed fruit and vegetable processing waste by a 100-mesh sieve to obtain fruit and vegetable processing waste powder; the fruit and vegetable processing waste is selected from one of the following: asparagus processing waste, soybean dregs and spina date seeds;
mixing the fruit and vegetable processing waste powder and ethanol in a mass ratio of 1:20, and uniformly stirring to prepare an ethanol solution of the fruit and vegetable processing waste;
blending 2.8-4.0g of extraction aid Cu-MOF-74 with 80-120mL of ethanol solution of fruit and vegetable processing waste, uniformly stirring, transferring to a reaction kettle, heating the reaction kettle to 70-100 ℃, performing subcritical extraction for 15-25min, standing, cooling, and performing suction filtration to obtain an ethanol extract with a solid of Cu-MOF-74 and a liquid of saponin;
adding ethanol into solid Cu-MOF-74, performing ultrasonic treatment for 10min, centrifuging, mixing the supernatant with ethanol extractive solution of saponin, distilling to recover ethanol, aging the obtained concentrated solution, washing separated saponin with water, and drying at 70-80 deg.C to obtain saponin extract;
the extraction aid Cu-MOF-74 has a chemical formula as follows: cu2(dhBDC)(H2O)10(ii) a The structural formula of the dhBDC is as follows:
the preparation method of the extraction aid Cu-MOF-74 comprises the following steps:
dissolving 0.15g of 2, 5-dihydroxy-1, 4-terephthalic acid in 1.5-2mL of a mixed solution of DMF and water in a volume ratio of 1: 1; dissolving 0.5g of copper nitrate in 0.8-1.2mL of water; violently shaking the two solutions into gel, aging at 85 ℃ overnight, washing with DMF, water and ethanol for 3 times in sequence, and activating at 85 ℃ to constant weight to obtain an extraction aid Cu-MOF-74;
the mass ratio of the filtered Cu-MOF-74 to the ethanol is 1: 10;
the Cu-MOF-74 is activated at 85 ℃ overnight and then repeatedly used.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102190697A (en) * | 2010-03-12 | 2011-09-21 | 中国科学院过程工程研究所 | Ultrasonic-assisted extraction and graded purification method for asparagus saponin |
| CN102491978A (en) * | 2011-12-02 | 2012-06-13 | 中国科学院过程工程研究所 | Method for preparing natural pigments, polysaccharide and saponin by utilizing disused asparagus resources |
| CN105779116A (en) * | 2016-05-05 | 2016-07-20 | 广州合诚三先生物科技有限公司 | Comprehensive extraction method for effective ingredients of spina date seeds |
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| CN102266467A (en) * | 2011-08-08 | 2011-12-07 | 南京泽朗医药科技有限公司 | Method for extracting agapanthus saponin from agipanthus |
| CN105203657B (en) * | 2015-09-15 | 2017-03-29 | 广州市药品检验所 | Semen Ziziphi Spinosae reference extract and its preparation method and application |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102190697A (en) * | 2010-03-12 | 2011-09-21 | 中国科学院过程工程研究所 | Ultrasonic-assisted extraction and graded purification method for asparagus saponin |
| CN102491978A (en) * | 2011-12-02 | 2012-06-13 | 中国科学院过程工程研究所 | Method for preparing natural pigments, polysaccharide and saponin by utilizing disused asparagus resources |
| CN105779116A (en) * | 2016-05-05 | 2016-07-20 | 广州合诚三先生物科技有限公司 | Comprehensive extraction method for effective ingredients of spina date seeds |
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