CN102241725A - Water extraction preparation method of daily chemical sapindoside - Google Patents
Water extraction preparation method of daily chemical sapindoside Download PDFInfo
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- CN102241725A CN102241725A CN2010101723103A CN201010172310A CN102241725A CN 102241725 A CN102241725 A CN 102241725A CN 2010101723103 A CN2010101723103 A CN 2010101723103A CN 201010172310 A CN201010172310 A CN 201010172310A CN 102241725 A CN102241725 A CN 102241725A
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Abstract
The invention relates to the extraction of plant fruit active ingredients, and especially relates to a water extraction preparation method of daily chemical sapindoside. The water extraction preparation method of daily chemical sapindoside provided by the invention employs Sapindus peel as a raw material and has the main points: crushing dry Sapindus peel to 5-20 meshes so as to obtain Sapindus peel powder; adding 2-5 times by weight of water, stirring under the constant state of 30-60 DEG C to extract for 2-3 times (each time lasts for 1-8 hours), carrying out solid-liquid separation, and combining extract liquids; adding 1-5wt% of precipitation agent to the extract liquids, standing for purification, and carrying out solid-liquid separation with a centrifuge; and performing vacuum-distilling on a sapindoside supernatant with a double-effect climbing film evaporator, and performing spray-drying and dewatering on the concentrated liquid. The water extraction preparation method provided by the invention is simple in process, does not use organic solvents and lowers investment cost and production cost; and the sapindoside obtained by the water extraction preparation method has the recovery rate more than 75% and the purity of 20-40%.
Description
Technical field:
The present invention relates to the extraction of fruit effective constituent, relate in particular to the water extracting method of daily use chemicals with sapindoside, promptly water is as activeconstituents---the method for sapindoside in the extraction agent extraction Seed of Chinese Soapberry pericarp.
Background technology:
Saponin content very abundant (account for dry-matter 20%) in the Seed of Chinese Soapberry pericarp, it is a kind of natural degradable nonionic surface active agent, it reduces capillary ability even is better than some synthetic surfactant, also has antibiotic in addition, anti-inflammatory, the isoreactivity of whitening simultaneously.Therefore, sapindoside can be used as tensio-active agent and activeconstituents, is used for high-end articles for washing and makeup, as cleansing milk, shampoo, body wash and other skin care product.
For a long time, the roadside that China's Seed of Chinese Soapberry is abandoned as waste mostly, the value of itself does not obtain development and utilization.Make a general survey of documents and materials, less to the report of sapindoside extracting method, the extracting method of the present sapindoside of reporting mainly contains two kinds of alcohol extracting method and water extractions.Alcohol extracting method comprises with ethanol or methanol extraction.The extraction yield of alcohol extracting sapindoside is higher, and purity is also higher, and extracting solution concentrates and more easily carries out.But alcohol extracting expends a large amount of ethanol or methyl alcohol, and production cost improves greatly; And alcohol extracting has requirement of explosion proof to production plant and equipment, has increased cost of investment greatly.The water extraction production cost is low, production process safety.Yet because the solubleness of saponin(e in water is limited, and many other non-saponin constituents are also water-soluble in the Seed of Chinese Soapberry, and as glucide and protein etc., it is all lower to make water put forward the extraction yield and the saponin(e purity of saponin(e.In addition, because the strong whipability of saponin(e, water is carried the back extracting solution and is difficult to distill concentrated, and this has just increased the energy consumption of drying and dehydrating step.In addition, also there is the report sapindoside after water is carried, to use alcohol precipitation, ultrafiltration or purification with macroreticular resin again, obtain sapindoside purity and improve greatly, but productive rate descends greatly.
Summary of the invention
The objective of the invention is to overcome the defective that exists in the above-mentioned Seed of Chinese Soapberry pericarp extracting method, provide a kind of water to have than the daily use chemicals of high product yield and purity and obtain through refining Preparation Method with the water of sapindoside as extraction agent.
Technical scheme
The technical solution adopted in the present invention is that a kind of daily use chemicals are obtained through refining Preparation Method with the water of sapindoside, is raw material with the Seed of Chinese Soapberry pericarp, and its main points are, exsiccant Seed of Chinese Soapberry pericarp is crushed to the 5--20 order, obtain the Seed of Chinese Soapberry fruit peel powder; Add weight 2--5 water doubly, at 30 ℃--stir under 60 ℃ the temperature constant state, extract 2--3 time, extracted solid-liquid separation, united extraction liquid at every turn 1--8 hour; In extracting solution, add the precipitation agent that accounts for gross weight 1%--5%, leave standstill purification, carry out solid-liquid separation with whizzer; With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, concentrated solution carries out the spraying drying dehydration.
Water of the present invention is as the saponin(e in the extraction agent extraction Seed of Chinese Soapberry pericarp, by optimization to conditions such as solid-liquid ratio, extraction time, temperature, time in extracting, make saponin(e be extracted out to greatest extent, and protein, sugar etc. extract as far as possible less, improve the productive rate and the product purity of saponin(e, and purify the purity that further improves saponin(e by leaving standstill.Other activeconstituentss in the Seed of Chinese Soapberry pericarp as chlorogenic acid, forulic acid, polyphenol, VITAMIN, amino acid etc., also can play cosmetic result.The sapindoside purity of this extracting method gained satisfies daily use chemicals saponin(e purity requirement, and this method cost is low, simple to operate, pollution-free, and gained sapindoside liquid product and solid product can be used for the daily use chemicals industry.
After described exsiccant Seed of Chinese Soapberry pericarp is meant that the Seed of Chinese Soapberry picking fruit gets off, 60 ℃ of oven dry in baking oven, decortication, and get.
Described extraction time is that minimizing was one by one extracted 3--8 hour for the first time, extracted 1--5 hour for the second time, extracted for the third time 1--3 hour.
Described precipitation agent is meant chitosan, Tai-Ace S 150, potassium aluminium sulfate, alum etc.
The present invention is simple for process, need not to use organic solvent, has reduced cost of investment and production cost.The rate of recovery that obtains sapindoside according to above-mentioned technology is more than 75%, and product purity is 20%-40%.
Compared with prior art, advantage of the present invention has:
(1) the present invention adopts the extraction agent of water as sapindoside, by optimizing productive rate and the purity that extraction conditions (extraction time, time, temperature, sample particle size) improves saponin(e, purifies the purity that further improves saponin(e by leaving standstill.This technology not only production cost is low, safety simple to operate, and extraction efficiency height, and product purity reaches certain level.
(2) existing technology mainly is with common vaporizer sapindoside to be carried out vacuum distilling, because the strong whipability of saponin(e, is difficult to the vacuum tightness that reaches high, thereby influences concentrated effect.The economic benefits and social benefits climbing-film evaporator is a kind of vaporizer of shell and tube, with the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, thereby overcome the strong whipability of saponin(e, reach the purpose that concentrates the sapindoside clear liquor, reduce the energy consumption that dehydrates operation.
Embodiment:
The following examples can make the professional and technical personnel more understand the present invention, but do not limit the present invention in any form.
A kind of daily use chemicals are obtained through refining Preparation Method with the water of sapindoside, are raw material with the Seed of Chinese Soapberry pericarp, and exsiccant Seed of Chinese Soapberry pericarp is crushed to the 5--20 order, obtain the Seed of Chinese Soapberry fruit peel powder; Add Seed of Chinese Soapberry fruit peel powder weight 2--5 water doubly, at 30 ℃--extract 2--3 time under 60 ℃ the temperature constant state, extracted united extraction liquid at every turn 1--8 hour; In extracting solution, add the precipitation agent that accounts for gross weight 1%--5%, leave standstill purification, carry out solid-liquid separation with whizzer; With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, concentrated solution carries out the spraying drying dehydration.
Embodiment 1, after the Seed of Chinese Soapberry picking fruit gets off, and 60 ℃ of oven dry in baking oven, decortication is crushed to 20 orders with pulverizer with pericarp, obtains the Seed of Chinese Soapberry fruit peel powder; In extractor, add Seed of Chinese Soapberry fruit peel powder 10Kg, add water 50L, heat 60 ℃, stir, refluxing extraction 8 hours, solid-liquid separation gets extracting solution, adds entry 40L again, heats 60 ℃ of refluxing extraction 5 hours, and solid-liquid separation gets extracting solution, merges with primary extracting solution; Add the 3Kg chitosan in extracting solution, room temperature leaves standstill purification, and centrifugation obtains clear liquor.With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, volatilization moisture makes solid concentration reach 20%, gets sapindoside concentrated solution product 18L, and its saponin content is 4%--8%.With spray-dryer the sapindoside concentrated solution is dewatered, obtain sapindoside powder-product 3.6Kg, saponin content is 20%--40%.
Embodiment 2, after the Seed of Chinese Soapberry picking fruit gets off, and 60 ℃ of oven dry in baking oven, decortication is crushed to 5 orders with pulverizer with pericarp, obtains the Seed of Chinese Soapberry fruit peel powder; In extractor, add Seed of Chinese Soapberry fruit peel powder 10Kg, add water 50L, heat 30 ℃ of refluxing extraction 7h, stir, solid-liquid separation gets extracting solution, add entry 40L again, heat 30 ℃ of refluxing extraction 5h, solid-liquid separation gets extracting solution, add water 30L, heat 30 ℃ of refluxing extraction 3h, solid-liquid separation gets extracting solution, with the extracting solution merging of first and second time; Add 3.5Kg Tai-Ace S 150 in extracting solution, room temperature leaves standstill purification, and centrifugation obtains clear liquor.With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, volatilization moisture makes solid concentration reach 20%, gets sapindoside concentrated solution product 18L, and its saponin content is 4%--8%.With spray-dryer the sapindoside concentrated solution is dewatered, obtain sapindoside powder-product 3.6Kg, saponin content is 20%--40%.
Embodiment 3, after the Seed of Chinese Soapberry picking fruit gets off, and 60 ℃ of oven dry in baking oven, decortication is crushed to 5 orders with pulverizer with pericarp, obtains the Seed of Chinese Soapberry fruit peel powder; In extractor, add Seed of Chinese Soapberry fruit peel powder 10Kg, add water 50L, heat 40 ℃ of refluxing extraction 4h, stir, solid-liquid separation gets extracting solution, add entry 30L again, heat 40 ℃ of refluxing extraction 3h, solid-liquid separation gets extracting solution, add water 20L, heat 40 ℃ of refluxing extraction 1h, solid-liquid separation gets extracting solution, with the extracting solution merging of first and second time; Add the 2Kg potassium aluminium sulfate in extracting solution, room temperature leaves standstill purification, and centrifugation obtains clear liquor.With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, volatilization moisture makes solid concentration reach 20%, gets sapindoside concentrated solution product 18L, and its saponin content is 4%--8%.With spray-dryer the sapindoside concentrated solution is dewatered, obtain sapindoside powder-product 3.6Kg, saponin content is 20%--40%.
Embodiment 4, after the Seed of Chinese Soapberry picking fruit gets off, and 60 ℃ of oven dry in baking oven, decortication is crushed to 20 orders with pulverizer with pericarp, obtains the Seed of Chinese Soapberry fruit peel powder; Add Seed of Chinese Soapberry fruit peel powder 10Kg in extractor, add water 50L, heated 50 ℃ of refluxing extraction 4 hours, stir, solid-liquid separation gets extracting solution, adds entry 40L again, heats 50 ℃ of refluxing extraction 2 hours, and solid-liquid separation gets extracting solution, merges with primary extracting solution; Add 2Kg alum in extracting solution, room temperature leaves standstill purification, and centrifugation obtains clear liquor.With the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, volatilization moisture makes solid concentration reach 20%, gets sapindoside concentrated solution product 18L, and its saponin content is 4%--8%.With spray-dryer the sapindoside concentrated solution is dewatered, obtain sapindoside powder-product 3.6Kg, saponin content is 20%--40%.
Effect relatively
| Extraction agent | The rate of recovery | Purity | Extraction agent cost (ten thousand/ton liquid product) |
| Ethanol | ?58％-74％ | 30％-42％ | 2.5 |
| Water (old law) | ?48％-71％ | 20-33％ | 1.8-2.0 |
| Water (the present invention) | ?75％ | 20％-40％ | 1.7 |
Claims (4)
1. daily use chemicals are obtained through refining Preparation Method with the water of sapindoside, are raw material with the Seed of Chinese Soapberry pericarp, it is characterized in that, exsiccant Seed of Chinese Soapberry pericarp is crushed to 5---and 20 orders obtain the Seed of Chinese Soapberry fruit peel powder; Add weight 2---5 times water, at 30 ℃---stir under 60 ℃ the temperature constant state, extraction 2---3 times, extracted 1---8 hours at every turn, solid-liquid separation, united extraction liquid; Adding accounts for gross weight 1%---5% precipitation agent in extracting solution, leaves standstill purification, carries out solid-liquid separation with whizzer, with the economic benefits and social benefits climbing-film evaporator sapindoside clear liquor is carried out vacuum distilling, and concentrated solution carries out the spraying drying dehydration.
2. a kind of daily use chemicals according to claim 1 are obtained through refining Preparation Method with the water of sapindoside, it is characterized in that, after described exsiccant Seed of Chinese Soapberry pericarp is meant that the Seed of Chinese Soapberry picking fruit gets off, and 60 ℃ of oven dry in baking oven, decortication, and get.
3. a kind of daily use chemicals according to claim 1 are obtained through refining Preparation Method with the water of sapindoside, it is characterized in that, described extraction time is, reduce one by one, extract 3 for the first time---8 hours, extract 1 for the second time---5 hours, extracting 1 for the third time---3 hours.
4. a kind of daily use chemicals according to claim 1 are obtained through refining Preparation Method with the water of sapindoside, it is characterized in that, described precipitation agent is meant chitosan, Tai-Ace S 150, potassium aluminium sulfate, alum.
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| CN2010101723103A CN102241725A (en) | 2010-05-13 | 2010-05-13 | Water extraction preparation method of daily chemical sapindoside |
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| CN2010101723103A CN102241725A (en) | 2010-05-13 | 2010-05-13 | Water extraction preparation method of daily chemical sapindoside |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603855A (en) * | 2011-11-25 | 2012-07-25 | 北京林业大学 | Extraction method of sapindus saponin |
| CN102617695A (en) * | 2012-03-08 | 2012-08-01 | 华南理工大学 | Desugared and decolored soapberry saponin and preparation method thereof |
| CN103059093A (en) * | 2013-01-18 | 2013-04-24 | 北京林业大学 | Method for preparing saponin by vacuum digestion |
| CN103073599A (en) * | 2013-01-18 | 2013-05-01 | 北京林业大学 | Concentrating and extracting method for saponins |
| CN103142430A (en) * | 2011-12-07 | 2013-06-12 | 横浜油脂工业株式会社 | Cleaning agent |
| CN108794562A (en) * | 2018-08-30 | 2018-11-13 | 佛山市欧若拉生物科技有限公司 | A kind of processing technology of sapindoside extract |
| CN108997443A (en) * | 2018-08-01 | 2018-12-14 | 李晌 | A kind of method that microbial fermentation extracts saponin(e in plant |
| CN109369744A (en) * | 2018-10-11 | 2019-02-22 | 浙江大学自贡创新中心 | A kind of method of sapindoside in aqueous two-phase extraction soapberry |
| CN109674701A (en) * | 2019-01-14 | 2019-04-26 | 澳宝化妆品（惠州）有限公司 | One kind scalp cleaning compositions of extract containing soapberry fruit and preparation method thereof |
| CN110075013A (en) * | 2019-05-28 | 2019-08-02 | 上海思珥生物科技有限公司 | A kind of makeup removing, face cleaning and the facial cleanser of antibacterial three-in-one and preparation method thereof |
| CN110407890A (en) * | 2019-07-18 | 2019-11-05 | 佛山市欧若拉生物科技有限公司 | The preparation method of sapindoside |
| CN113502196A (en) * | 2021-06-19 | 2021-10-15 | 广东菁萃生物科技有限公司 | Preparation method and application of mild non-irritant saponin composition |
| CN113549118A (en) * | 2021-06-23 | 2021-10-26 | 广东菁萃生物科技有限公司 | Extraction method and application of high-purity triterpenoid saponin |
| CN113801172A (en) * | 2021-09-14 | 2021-12-17 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
| WO2022268235A1 (en) * | 2021-06-23 | 2022-12-29 | 广东菁萃生物科技有限公司 | Saponin composition having high stability and use thereof |
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| CN1935820A (en) * | 2006-10-14 | 2007-03-28 | 合肥新新石化助剂有限公司 | Method for preparing total saponin of sapindusmukerossi |
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Cited By (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603855B (en) * | 2011-11-25 | 2014-03-05 | 北京林业大学 | Extraction method of sapindus saponin |
| CN102603855A (en) * | 2011-11-25 | 2012-07-25 | 北京林业大学 | Extraction method of sapindus saponin |
| CN103142430A (en) * | 2011-12-07 | 2013-06-12 | 横浜油脂工业株式会社 | Cleaning agent |
| CN103142430B (en) * | 2011-12-07 | 2015-07-15 | 横浜油脂工业株式会社 | Cleaning agent |
| CN102617695A (en) * | 2012-03-08 | 2012-08-01 | 华南理工大学 | Desugared and decolored soapberry saponin and preparation method thereof |
| CN102617695B (en) * | 2012-03-08 | 2013-12-11 | 华南理工大学 | Desugared and decolored soapberry saponin and preparation method thereof |
| CN103059093A (en) * | 2013-01-18 | 2013-04-24 | 北京林业大学 | Method for preparing saponin by vacuum digestion |
| CN103073599A (en) * | 2013-01-18 | 2013-05-01 | 北京林业大学 | Concentrating and extracting method for saponins |
| CN103073599B (en) * | 2013-01-18 | 2015-01-28 | 北京林业大学 | Concentrating and extracting method for saponins |
| CN103059093B (en) * | 2013-01-18 | 2015-05-20 | 北京林业大学 | Method for preparing saponin by vacuum digestion |
| CN108997443A (en) * | 2018-08-01 | 2018-12-14 | 李晌 | A kind of method that microbial fermentation extracts saponin(e in plant |
| CN108794562A (en) * | 2018-08-30 | 2018-11-13 | 佛山市欧若拉生物科技有限公司 | A kind of processing technology of sapindoside extract |
| CN109369744A (en) * | 2018-10-11 | 2019-02-22 | 浙江大学自贡创新中心 | A kind of method of sapindoside in aqueous two-phase extraction soapberry |
| CN109674701A (en) * | 2019-01-14 | 2019-04-26 | 澳宝化妆品（惠州）有限公司 | One kind scalp cleaning compositions of extract containing soapberry fruit and preparation method thereof |
| CN110075013A (en) * | 2019-05-28 | 2019-08-02 | 上海思珥生物科技有限公司 | A kind of makeup removing, face cleaning and the facial cleanser of antibacterial three-in-one and preparation method thereof |
| CN110407890A (en) * | 2019-07-18 | 2019-11-05 | 佛山市欧若拉生物科技有限公司 | The preparation method of sapindoside |
| CN113502196A (en) * | 2021-06-19 | 2021-10-15 | 广东菁萃生物科技有限公司 | Preparation method and application of mild non-irritant saponin composition |
| CN113502196B (en) * | 2021-06-19 | 2023-05-09 | 广东菁萃生物科技有限公司 | Preparation method and application of mild and non-irritating saponin composition |
| CN113549118A (en) * | 2021-06-23 | 2021-10-26 | 广东菁萃生物科技有限公司 | Extraction method and application of high-purity triterpenoid saponin |
| CN113549118B (en) * | 2021-06-23 | 2022-04-22 | 广东菁萃生物科技有限公司 | Extraction method and application of high-purity triterpenoid saponin |
| WO2022268235A1 (en) * | 2021-06-23 | 2022-12-29 | 广东菁萃生物科技有限公司 | Saponin composition having high stability and use thereof |
| CN113801172A (en) * | 2021-09-14 | 2021-12-17 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
| CN113801172B (en) * | 2021-09-14 | 2022-09-06 | 广州市润研基因科技有限公司 | Method for separating protein in soapberry saponin water extract |
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Application publication date: 20111116 |