CN107556359B - Method for improving dissolution rate of water-extracted tea saponin - Google Patents
Method for improving dissolution rate of water-extracted tea saponin Download PDFInfo
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- CN107556359B CN107556359B CN201710839054.0A CN201710839054A CN107556359B CN 107556359 B CN107556359 B CN 107556359B CN 201710839054 A CN201710839054 A CN 201710839054A CN 107556359 B CN107556359 B CN 107556359B
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Abstract
The invention discloses a method for improving the dissolution rate of water-extracted tea saponin, and belongs to the technical field of deep processing of agricultural byproduct leftovers. The extraction method adopts the staged extraction of the tea saponin in the tea seed cake residue phase, reduces the cost of using ethanol compared with an ethanol water extraction method, and has the advantages of simple process, no pollution, high resource utilization rate, high product yield and the like. The tea saponin obtained by the method has high dissolution rate, which is higher than the water extraction effect without sodium carbonate. The method is adopted to treat the tea saponin in the residue phase of the camellia seed meal for full extraction. The added value of the product is improved, the cost is reduced, and the economic benefit is improved.
Description
Technical Field
The invention relates to a method for improving the dissolution rate of water-extracted tea saponin, belonging to the technical field of deep processing of agricultural byproduct leftovers.
Background
Tea saponin (tea saponin, TS), also known as tea saponin and tea saponin, is a general name of saponin compounds in Camellia (Camellia) plants of Theaceae (Theaceae), and is a mixture of oleanane type pentacyclic triterpene saponin with similar structure composed of 7 aglucones, 4 aglucones and 2 organic acids. The tea saponin contains hydrophilic saccharide and hydrophobic ligand group, so that it is one excellent natural non-ionic surfactant with excellent foaming, dispersing, emulsifying, detergency and other surface activity. In addition, researches show that the tea saponin has remarkable biological activities of eliminating phlegm, diminishing inflammation, relieving cough, easing pain, resisting osmosis, sterilizing, killing insect and hemolysis, killing fish poison, inhibiting alcohol and the like. Therefore, in recent years, tea saponin has been widely used in the industries of daily use chemicals, building materials, aquaculture, textile and the like, and has gradually gained more attention in the industries of medicines, health products, cosmetics, foods and the like.
The tea saponin is used as a surfactant with excellent performance, can be applied to fruit and vegetable cleaning agents, household liquid detergents and the like to improve the cleaning effect, and can be applied to personal washing products such as shampoos, hair dyes and the like. At present, the application of the surface activity of the tea saponin can be that the tea saponin-rich camellia plant or the byproduct is extracted and purified by methods of water extraction, alcohol extraction and the like and then added into a detergent, or the tea saponin-rich byproduct such as tea seed meal (the content of the tea saponin is about 10-15%) after oil extraction and the like is directly wrapped in filter cloth to prepare a tea saponin washing bag. In any method, the key factor influencing the washing effect is the improvement of the leaching rate of the tea saponin in the aqueous solution. At present, the dissolution rate of tea saponin in the water extraction process is low by a water leaching method and a water extraction and alcohol extraction method, so that the extraction is limited; and the organic solvent such as methanol is used as an extracting agent, so that the method is toxic and high in production cost. The plum sensitivity and the like are used for extracting the camellia seed meal under the conditions that the material-liquid ratio is 1:20 and the ethanol concentration is 63%, the ethanol and water consumption is high, a large amount of wastewater is easily generated, and the environment is easily damaged. Therefore, the invention aims to improve the leaching effect of the tea saponin in the water-extracted camellia seed meal, so that the ethanol usage amount of the water-extracted and alcohol-extracted tea saponin is reduced, and the tea saponin leaching effect of a tea saponin washing bag can be improved.
Disclosure of Invention
Aiming at the conditions that a water extraction and alcohol extraction method consumes a large amount of ethanol and the dissolution rate of tea saponin in a tea saponin washing bag is low, the invention aims to provide a method for improving the leaching effect of the tea saponin in water-extracted camellia seed meal. The method has simple operation and safe process, can realize the recycling of the tea saponin, and is suitable for industrial production.
The first purpose of the invention is to provide a method for improving the dissolution rate of tea saponin extracted by water, which comprises the following steps:
1) pretreatment: drying and crushing the camellia seed meal, and sieving to obtain camellia seed meal powder;
2) alkalization: adding an alkaline solution into the camellia seed meal powder, uniformly stirring, and drying to obtain alkaline camellia seed meal;
3) reaction: adding water into the alkaline camellia seed meal obtained in the step 2), fully mixing and stirring uniformly, and centrifuging to obtain a supernatant after the reaction is finished.
In one embodiment of the present invention, the crushed material in step 1) is sieved by a 200-mesh sieve with 100 meshes.
In one embodiment of the present invention, the alkaline solution is Na2CO3An aqueous solution; na (Na)2CO3The concentration of the aqueous solution is 1-2% w/w.
In one embodiment of the present invention, the Na2CO3The addition amount of the water solution is 0.5-2 times of the camellia seed meal powder.
In one embodiment of the present invention, the drying temperature is 50 to 70 ℃.
In one embodiment of the invention, the water added in the step 3) is 8-10 times of the mass of the camellia seed meal powder.
In one embodiment of the present invention, the stirring temperature in step 3) is 60-70 ℃, and the stirring speed is 300-500 rpm.
The second purpose of the invention is to provide the application of the method in the aspect of recovering the tea saponin in the oil tea seed meal.
In an embodiment of the present invention, the application specific steps are as follows:
1) pretreatment: drying and crushing the camellia seed meal, and sieving the camellia seed meal with a sieve of 100-200 meshes to obtain camellia seed meal powder;
2) alkalization: adding 0.5-2 times of Na of oil Camellia seed meal powder2CO3Adding the aqueous solution into camellia seed meal powder, uniformly stirring, and drying at 50-70 ℃ to obtain alkaline camellia seed meal; the Na is2CO3The concentration of the aqueous solution is 1-2% w/w;
3) reaction: adding water 8-10 times the weight of the camellia seed meal powder into the alkaline camellia seed meal obtained in the step 2), fully stirring at the rotation speed of 500rpm of 300-70 ℃ for 20-40min, and centrifuging to take supernatant after the reaction is finished.
The third purpose of the invention is to provide the application of the method in preparing the tea saponin washing bag.
The fourth purpose of the invention is to provide a tea saponin washing bag, which is prepared by the following method:
1) pretreatment: drying and crushing the camellia seed meal, and sieving to obtain camellia seed meal powder;
2) alkalization: adding alkaline solution into the camellia seed meal powder, stirring uniformly, drying at 50-70 ℃ to obtain alkaline camellia seed meal, and wrapping the alkaline camellia seed meal in filter cloth to prepare a tea saponin washing bag.
In one embodiment of the invention, the wash pack is specifically prepared as follows:
1) pretreatment: drying and crushing the camellia seed meal, and sieving the camellia seed meal with a sieve of 100-200 meshes to obtain camellia seed meal powder;
2) alkalization: adding 0.5-2 times of Na of oil Camellia seed meal powder2CO3Adding the aqueous solution into camellia seed meal powder, uniformly stirring, and drying at 50-70 ℃ to obtain alkaline camellia seed meal; wrapping alkaline camellia seed meal in 200-mesh filter cloth to prepare a tea saponin washing bag; the Na is2CO3The concentration of the aqueous solution is 1-2% w/w.
The invention has the beneficial effects
The recovery method adopts the staged extraction of the tea saponin in the tea seed cake residue phase, reduces the cost of using ethanol compared with an ethanol water extraction method, and has the advantages of simple process, no pollution, high resource utilization rate, high product yield and the like. The tea saponin obtained by the method has high dissolution rate, which is higher than water extraction effect without sodium carbonate. Meanwhile, the method can also improve the tea saponin leaching effect of the tea saponin washing bag, so that the tea saponin is fully leached. The added value of the product is improved, the cost is reduced, and the economic benefit is improved.
Detailed Description
Example 1: extracting oil-tea camellia seed oil by ethanol water extraction method
Using 15% alcohol-water mixed solvent (pH 10 adjusted by 10% NaOH solution) and reacting at 70 deg.C500g of camellia seedsExtracting oil tea seed oil from Jiangxi Lu Yexuan biotechnology limited, centrifuging at 5000rpm for 10-15 min to obtain three phases, namely an oil phase, a water phase (about 2025mL) and a slag phase (about 400g), wherein the oil phase enters an oil refining process, and the slag phase is used for a subsequent recovery process.
Example 2: recovering tea saponin from residue phase after extracting oil tea seed oil
Drying the slag phase obtained in example 1 at 60 ℃, crushing and sieving by a 100-mesh sieve to obtain slag phase powder, and mixing 1% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Adding water with the mass 10 times of that of the slag phase, fully and uniformly mixing, stirring for 30min at the temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of about 400rpm, centrifuging after the reaction is finished at the rotating speed of about 5000rpm for 15min, and taking the supernatant. The highest concentration of the tea saponin is up to 9.47mg/ml by adopting a vanillin-concentrated sulfuric acid method, so that the leaching effect of the water-extracted tea saponin is improved.
Example 3: recovering tea saponin from residue phase after extracting oil tea seed oil
Drying the slag phase of example 1 at 50 ℃, crushing and sieving with a 100-mesh sieve to obtain slag phase powder, mixing 2% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Adding water with the mass 10 times of that of the slag phase, fully and uniformly mixing, stirring for 30min at the temperature of 70 ℃ by using a magnetic stirrer at the rotating speed of about 300rpm, centrifuging after the reaction is finished at the rotating speed of about 5000rpm for 15min, and taking the supernatant. The highest concentration of the tea saponin is up to 9.50mg/ml by adopting a vanillin-concentrated sulfuric acid method, so that the leaching effect of the water-extracted tea saponin is improved.
Example 4: recovering tea saponin from residue phase after extracting oil tea seed oil
Drying the slag phase obtained in example 1 at 70 ℃, crushing and sieving by a 100-mesh sieve to obtain slag phase powder, and mixing 1% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Adding 10 times of water, mixing, stirring at 70 deg.C for 30min at 500rpm with a magnetic stirrer, centrifuging at 5000rpm for 15min, and collecting supernatant. The tea saponin concentration is measured by vanillin-concentrated sulfuric acid method to reach 9.42mg/ml at most, and the extract is extractedImproves the extraction effect of the water-extracted tea saponin.
Example 5: recovering tea saponin from residue phase after extracting oil tea seed oil
Drying the slag phase obtained in example 1 at 60 ℃, crushing and sieving with a 100-mesh sieve to obtain slag phase powder, and mixing 2% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Adding water with the mass 10 times of that of the slag phase, fully and uniformly mixing, stirring for 30min at the temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of about 400rpm, centrifuging after the reaction is finished at the rotating speed of about 5000rpm for 15min, and taking the supernatant. The yield of the tea saponin is determined to reach 9.58mg/ml by adopting a vanillin-concentrated sulfuric acid method, and the extraction effect of the water-extracted tea saponin is improved.
Example 6: recovering tea saponin from residue phase after extracting oil tea seed oil
Drying the slag phase obtained in example 1 at 60 ℃, crushing and sieving with a 100-mesh sieve to obtain slag phase powder, and mixing 0.2% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Adding water with the mass 10 times of that of the slag phase, fully and uniformly mixing, stirring for 30min at the temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of about 400rpm, centrifuging after the reaction is finished at the rotating speed of about 5000rpm for 15min, and taking the supernatant. The concentration of tea saponin is measured to reach 8.30mg/ml by adopting a vanillin-concentrated sulfuric acid method.
Example 7: tea saponin dissolving-out effect of alkalized tea saponin washing bag
Drying the slag phase obtained in example 1 at 60 ℃, crushing and sieving with a 100-mesh sieve to obtain slag phase powder, and mixing 0.2% (w/w) of Na2CO3Dissolving the solid in water with the same mass as the slag phase, adding the solid into the slag phase powder, uniformly stirring by using a stirrer, and drying at 60 ℃ until the solid is nearly dry. Wrapping the dried residue phase in 200 mesh filter cloth to obtain tea saponin washing bag, placing the washing bag in 100 times of water of residue phase mass, stirring at 40 deg.C for 30min at rotation speed of 200rpm, simulating domestic use of tea saponin washing bag, reactingTaking the supernatant after finishing, and determining the tea saponin concentration to be 0.8mg/ml by adopting a vanillin-concentrated sulfuric acid method.
Comparative example 1: directly adding water to recover tea saponin without drying after alkalization
Drying the slag phase obtained in example 1 at 60 ℃, crushing and sieving by a 100-mesh sieve to obtain slag phase powder, and mixing 1% (w/w) of Na2CO3And dissolving the solid in water with the mass of 10 times that of the slag phase, adding the solid into the slag phase obtained in example 1, fully and uniformly mixing, stirring for 30min at the temperature of 60 ℃ by using a magnetic stirrer, wherein the rotating speed is about 400rpm, centrifuging after the reaction is finished, wherein the centrifuging rotating speed is about 5000rpm, and the time is 15min, and taking the supernatant. The concentration of tea saponin is determined to reach 7.62 mg/ml.
Comparative example 2: method for recovering tea saponin from residue phase by ethanol water extraction
The slag phase obtained in example 1 was dried at 60 ℃ and crushed and sieved through a 100-mesh sieve to obtain slag phase powder. Adding ethanol aqueous solution with volume fraction of 60% and 10 times of slag phase mass, stirring for 30min at 60 deg.C with a magnetic stirrer at 400rpm, centrifuging at 5000rpm for 15min after reaction, and collecting supernatant. The determination shows that the yield of the tea saponin reaches 9.79mg/ml, and the extraction effect of the tea saponin is improved.
Comparative example 3: direct water extraction method for recovering tea saponin from residue phase
The slag phase obtained in example 1 was dried at 60 ℃ and crushed and sieved through a 100-mesh sieve to obtain slag phase powder. Adding water with the mass 10 times of that of the slag phase, fully and uniformly mixing, stirring for 30min at the temperature of 60 ℃ by using a magnetic stirrer at the rotating speed of about 400rpm, centrifuging after the reaction is finished at the rotating speed of about 5000rpm for 15min, and taking the supernatant. The concentration of the tea saponin in the direct water extract is measured to reach 5.49 mg/ml.
Comparative example 4: water extraction effect of non-alkalized tea saponin washing bag
The slag phase obtained in example 1 was dried at 60 ℃ and crushed and sieved through a 100-mesh sieve to obtain slag phase powder. Directly wrapping the slag phase powder in 200-mesh filter cloth to obtain a tea saponin washing bag, placing the washing bag in 100 times of water of the slag phase mass, stirring for 30min at 40 ℃ and the rotation speed of about 200rpm, simulating the use of the tea saponin washing bag in a family, taking supernatant after the reaction is finished, and determining the concentration of the tea saponin to be 0.4mg/ml by adopting a vanillin-concentrated sulfuric acid method.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. The method for improving the dissolution rate of tea saponin extracted by water is characterized by comprising the following steps:
1) pretreatment: drying and crushing the camellia seed meal, and sieving to obtain camellia seed meal powder;
2) alkalization: adding an alkaline solution into the camellia seed meal powder, uniformly stirring, and drying at 60 ℃ until the camellia seed meal is nearly dry to obtain alkaline camellia seed meal;
3) reaction: adding water into the alkaline camellia seed meal obtained in the step 2), fully mixing and stirring uniformly, and centrifuging to obtain a supernatant after the reaction is finished;
sieving the crushed powder in the step 1) through a 100-200-mesh sieve; the alkaline solution is Na2CO3An aqueous solution; na (Na)2CO3The concentration of the aqueous solution is 1-2% w/w; the Na is2CO3The aqueous solution is prepared by mixing Na2CO3Dissolving the solid in water with the same mass as the camellia seed meal powder, and adding the solid into the slag phase powder; the adding amount of water in the step 3) is 8-10 times of the mass of the camellia seed meal powder; the stirring temperature in the step 3) is 60-70 ℃, and the stirring speed is 300-500 rpm.
2. Use of the method of claim 1 for recovering tea saponin from oil tea seed meal.
3. The application of claim 2, wherein the application specific steps are:
1) pretreatment: drying and crushing the camellia seed meal, and sieving the camellia seed meal with a sieve of 100-200 meshes to obtain camellia seed meal powder;
2) alkalization: adding 0.5-2 times of Na of oil Camellia seed meal powder2CO3Adding the aqueous solution into camellia seed meal powder, uniformly stirring, and drying at 60 ℃ to obtain alkaline camellia seed meal; the Na is2CO3The concentration of the aqueous solution is 1-2% w/w;
3) reaction: adding water 8-10 times the weight of the camellia seed meal powder into the alkaline camellia seed meal obtained in the step 2), fully stirring at the rotation speed of 500rpm of 300-70 ℃ for 20-40min, and centrifuging to take supernatant after the reaction is finished.
4. Use of the method of claim 1 in the preparation of a tea saponin washing pack.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06211674A (en) * | 1993-01-14 | 1994-08-02 | Itouen:Kk | Antiulcer agent |
| JPH0761998A (en) * | 1993-08-24 | 1995-03-07 | Itouen:Kk | New saponin compound and desacyl saponin compound |
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| CN102952624A (en) * | 2012-11-06 | 2013-03-06 | 安徽新世界绿洲茶油有限公司 | Preparation process for strong-flavor tea-seed oil and prepared strong-flavor tea-seed oil |
| CN105441215A (en) * | 2015-12-16 | 2016-03-30 | 泉州市福达科技咨询有限公司 | Environmentally friendly camellia seed detergent and preparation method thereof |
| CN106544195A (en) * | 2016-10-07 | 2017-03-29 | 常州市鼎日环保科技有限公司 | A kind of preparation method of automobile glass cleaning agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH06211674A (en) * | 1993-01-14 | 1994-08-02 | Itouen:Kk | Antiulcer agent |
| JPH0761998A (en) * | 1993-08-24 | 1995-03-07 | Itouen:Kk | New saponin compound and desacyl saponin compound |
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