CN101817857A - Process for extracting rutin from sophora japonica - Google Patents
Process for extracting rutin from sophora japonica Download PDFInfo
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- CN101817857A CN101817857A CN 201010160270 CN201010160270A CN101817857A CN 101817857 A CN101817857 A CN 101817857A CN 201010160270 CN201010160270 CN 201010160270 CN 201010160270 A CN201010160270 A CN 201010160270A CN 101817857 A CN101817857 A CN 101817857A
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Abstract
The invention discloses a process for extracting rutin from sophora japonica, which comprises the following steps of: (1) preparing and crushing sophora japonica, putting the crashed sophora japonica into an extraction tank, washing and moistening the crashed sophora japonica with boiling water, and then, introducing an extraction solvent for carrying out reverse percolation extraction, wherein the extraction solvent is a mixture of saturated lime water, borax and sodium sulfite, the proportioning by weight of the saturated lime water to the borax to the sodium sulfite is 1000:4-6:0.5-1.5, and the pressure of the reverse percolation extraction is 0.2-0.3MPa; and (2) carrying out cascade filtration on the reverse percolation extraction solution, adding hydrochloric acid after cooling to regulate the pH value to 3-4, crystallizing, taking out crystals, washing the crystals with water to the neutrality, and drying the crystals to obtain finished products. Compared with the prior art, in the invention, by using reverse percolation extraction to replace percolation extraction and combining the extraction solvent with special proportioning, the rutin in the sophora japonica can be extracted more completely, thus the extraction rate is high, and residues in the percolation solution are few and can be filtered more easily; and the invention has the advantages of simple and convenient operation and short production cycle, and the product purity can reach more than 97.5%.
Description
Technical field
The present invention relates to from plant, extract the technology of activeconstituents, be specifically related to from the sophora bud, extract the technology of rutin.
Background technology
The sophora bud is the dry flower and alabastrum of leguminous plants Chinese scholartree (Sophora japonica L.r).The sophora bud contains rutin and reaches more than 20.0%, is rutin main raw material source.Rutin is a kind of flavonoid compound, and its proterties is yellow crystalline powder or amorphism powder, and bitter taste is arranged, and is slightly water-soluble, can be dissolved in hot water and alcohol; Chance light is perishable, should preserve in the cool.It is hemorrhage that rutin is mainly used in the fragility and the perviousness of treatment capillary vessel, reduces human body blood fat and cholesterol, is the good medicine of multiple diseases such as treatment hypertension, cardiovascular disorder, stomach trouble, tetter, diabetes.It also has antibiotic and radiation resistance in addition.Rutin can be used for composite and intermediate medicine directly as medicine, is mainly used in the additive and the tinting material of food, makeup abroad.
When industrial production and laboratory extraction rutin, the method that adopts is the alkaline extraction acid precipitation method usually.This method is to utilize rutin to have acidity, can be water-soluble with the alkali salify, and after adding acid and making into acidity, its free principle of separating out obtains purer rutin through recrystallization again.Answer (" experiment of extracting rutin with decocting method and percolation from the sophora bud are compared " such as sweet-scented osmanthus as Lee, herbal medicine, 1992,23 (10): 527.) research draws: with the borax saturated limewater diacolation 3h of 30 times of sophora bud meal weight, percolate filters, and transfers pH4.5 with hydrochloric acid, leave standstill suction filtration behind the 5h, precipitation is washed to neutrality with ion-exchange, 70～80 ℃ of oven dry, yield 98.14%.This method does not need main equipment, invests lessly, and purity is higher, but its production cycle is longer.And for example fight (" cold caustic soda method is extracted the experimental study of rutin from the sophora bud ", Chinese patent medicine, 1994,16 (7): 10.) with the sophora bud be raw material, adopt cold alkali (Na such as beautiful qin
2SO
3Mix with liming-diacolation extracts) acid precipitation method, and extract Acid precipitation with cold alkali gradation and compare test, the result shows that the former rutin yield (17.00%～17.80%) is greater than the latter (12.00%～12.40%).But the purity of this method products obtained therefrom has only about 94%.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of technology of extracting rutin from the sophora bud, and this technology is simple and easy to control, and production cost is low, extraction yield height, products obtained therefrom purity height.
The technical solution used in the present invention is as follows:
From the sophora bud, extract the technology of rutin, may further comprise the steps:
1) get the sophora bud and pulverize, place extractor, boiling water is washed the profit back and is fed and extract solvent and carry out the reverse osmosis extraction of filtering;
Described extraction solvent is the mixture of saturated limewater, borax and S-WAT, and their weight proportion is a saturated limewater: borax: S-WAT=1000: 4～6: 0.5～1.5, the reverse osmosis pressure that extracts of filtering is 0.2～0.3MPa;
2) reverse osmosis is filtered extracting solution through cascade filtration, adds hydrochloric acid adjust pH to 3～4 after the cooling, crystallization, and crystal water is washed till neutrality, drying, promptly.
In order further to improve the yield of this technology, also can add an amount of solvent to the liquid level that extracts earlier and exceed raw material 5～10cm washing after profit finishes, stir, leave standstill to begin again to feed behind 5～35min and extract solvent and carry out the reverse osmosis extraction of filtering.
In the aforesaid method,
Step 2) in, described cascade filtration can secondary or secondary is above filters, and filters the order number of used filter cloth or filter screen and is obedient to rule from coarse to fine; Usually select three-stage filtration for use, wherein one-level is filtered into 80～100 orders, and cascade filtration is 150～200 orders, and three-stage filtration is 250～350 orders.
In the step 1), reverse osmosis time of extracting of filtering is 2～6h, and the consumption that extracts solvent is 15～20 times of raw material weight, and the temperature of extracting solvent is 15～75 ℃, is preferably 35～55 ℃.Reverse osmosis is filtered and is extracted the borax in the solvent and S-WAT is preferred mixes with saturated limewater after dissolving fully with suitable quantity of water earlier again.
Step 2) in,, can during leaving standstill crystallization, stir once every 20～120min for improving crystallization speed.
Compared with prior art, the invention has the advantages that:
1, filter with reverse osmosis and extract to replace diacolation to extract, raw material is more thorough with mixing of solvent, does not stay the dead angle, minimizing extraction time and time; In conjunction with the extraction solvent of special proportioning, feasible more complete to the extraction of rutin in the sophora bud, thereby the extraction yield height;
2, because what adopt is reverse osmosis extractions of filtering, the more conventional alkali of residue in the percolate of extraction gained carry or diacolation alkali extracting method few, easier filtration; By adopting the mode of cascade filtration from coarse to fine, more traditional disposable filtering pressure is little, and filtration velocity is fast, better removes impurity in the percolate;
3, easy and simple to handle, with short production cycle, extraction yield and yield height, product purity can reach more than 98%.
Embodiment
Embodiment 1
1) get the 1Kg sophora bud and be crushed to 40 orders, place extractor, boiling water is washed profit back and is fed and extract solvent and carry out reverse osmosis and filter and extract 3h, and the pressure of extraction is 0.27MPa; The consumption that wherein extracts solvent is that 20 times of raw material weight, temperature are 35 ℃, and the weight proportion of saturated liming, borax and S-WAT is 1000: 5: 1 in the solvent;
2) reverse osmosis is filtered, and (one-level is filtered into 80 orders to extracting solution through three-stage filtration, cascade filtration is 200 orders, three-stage filtration is 300 orders), add hydrochloric acid adjust pH to 3.5, crystallization after being cooled to normal temperature, soup flame filter press press filtration, washing crystallizes to neutrality, and is dry under 80 ℃ of following conditions, obtains yellow crystalline powder 0.218Kg, yield is 21.8%, and measuring its purity is 99.6%.
Embodiment 2
1) get the 1Kg sophora bud and be crushed to 20 orders, place extractor, boiling water is washed profit 2 times, adds earlier an amount of solvent to the liquid level that extracts and exceeds raw material 6cm, stirs, soak 30min after, feed again and extract solvent and carry out reverse osmosis and filter and extract 4h, the pressure of extraction is 0.2MPa; The consumption that wherein extracts solvent is that 15 times of raw material weight, temperature are 45 ℃, and the weight proportion of saturated liming, borax and S-WAT is 1000: 4: 1.5 in the solvent;
2) reverse osmosis is filtered, and (one-level is filtered into 100 orders to extracting solution through three-stage filtration, cascade filtration is 150 orders, three-stage filtration is 350 orders), add hydrochloric acid adjust pH to 4, crystallization after being cooled to normal temperature, suction filtration, washing crystallizes to neutrality, and is dry under 80 ℃ of following conditions, obtains yellow crystalline powder 0.223Kg, yield is 22.3%, and measuring its purity is 98.9%.
Embodiment 3
1) get the 1Kg sophora bud and be crushed to 60 orders, place extractor, boiling water is washed and feed to be extracted solvent after the profit 2 times and carry out reverse osmosis and filter and extract 6h, and the pressure of extraction is 0.3MPa; The consumption that wherein extracts solvent is that 20 times of raw material weight, temperature are 15 ℃, and the weight proportion of saturated liming, borax and S-WAT is 1000: 6: 0.5 in the solvent;
2) reverse osmosis is filtered, and (one-level is filtered into 150 orders to extracting solution through cascade filtration, cascade filtration is 250 orders, add hydrochloric acid adjust pH to 3 after being cooled to normal temperature, crystallization takes out crystallization, and washing crystallizes to neutrality, dry under 80 ℃ of following conditions, obtain yellow crystalline powder 0.208Kg, yield is 20.8%, and measuring its purity is 97.6%.
Embodiment 4
1) get the 1Kg sophora bud and be crushed to 10 orders, place extractor, boiling water is washed and feed to be extracted solvent after the profit 2 times and carry out reverse osmosis and filter and extract 2.5h, and the pressure of extraction is 0.23MPa; The consumption that wherein extracts solvent is that 16 times of raw material weight, temperature are 50 ℃, and the weight proportion of saturated liming, borax and S-WAT is 1000: 6: 1.5 in the solvent;
2) reverse osmosis is filtered, and (one-level is filtered into 100 orders to extracting solution through cascade filtration, cascade filtration is 300), add hydrochloric acid adjust pH to 3 after being cooled to normal temperature, the flame filter press press filtration of crystallization, soup, washing crystallizes to neutrality, dry under 80 ℃ of following conditions, obtain yellow crystalline powder 0.210Kg, yield is 21%, and measuring its purity is 98.0%.
Embodiment 5
1) get the 1Kg sophora bud and be crushed to 80 orders, place extractor, boiling water is washed profit 2 times, add earlier an amount of extract solvent to liquid level (exceed raw material 10cm, stir, soak 10min after, feed again and extract solvent and carry out reverse osmosis and filter and extract 2h, the pressure of extraction is 0.25MPa; The consumption that wherein extracts solvent is that 18 times of raw material weight, temperature are 70 ℃, and the weight proportion of saturated liming, borax and S-WAT is 1000: 5: 1.5 in the solvent;
2) reverse osmosis is filtered, and (one-level is filtered into 90 orders to extracting solution through three-stage filtration, cascade filtration is 200 orders, three-stage filtration is 350 orders), add hydrochloric acid adjust pH to 4, crystallization after being cooled to normal temperature, suction filtration, washing crystallizes to neutrality, and is dry under 80 ℃ of following conditions, obtains yellow crystalline powder 0.216Kg, yield is 21.6%, and measuring its purity is 97.7%.
Claims (7)
1. from the sophora bud, extract the technology of rutin, it is characterized in that may further comprise the steps:
1) get the sophora bud and pulverize, place extractor, boiling water is washed the profit back and is fed and extract solvent and carry out the reverse osmosis extraction of filtering;
Described extraction solvent is the mixture of saturated limewater, borax and S-WAT, and their weight proportion is a saturated limewater: borax: S-WAT=1000: 4～6: 0.5～1.5, the reverse osmosis pressure that extracts of filtering is 0.2～0.3MPa;
2) reverse osmosis is filtered extracting solution through cascade filtration, adds hydrochloric acid adjust pH to 3～4 after the cooling, crystallization, and crystal water is washed till neutrality, drying, promptly.
2. the technology of from the sophora bud, extracting rutin according to claim 1, it is characterized in that: in the step 1), after washing the profit end, add an amount of solvent to the liquid level that extracts earlier and exceed raw material 5～10cm, stir, leave standstill to begin again behind 5～35min to feed and extract solvent and carry out the reverse osmosis extraction of filtering.
3. the technology of extracting rutin from the sophora bud according to claim 1 and 2 is characterized in that: step 2) in, described cascade filtration is a three-stage filtration, and wherein one-level is filtered into 80～100 orders, and cascade filtration is 150～200 orders, and three-stage filtration is 250～350 orders.
4. the technology of extracting rutin from the sophora bud according to claim 1 is characterized in that: in the step 1), reverse osmosis time of extracting of filtering is 2～6h.
5. the technology of extracting rutin from the sophora bud according to claim 1 is characterized in that: in the step 1), the consumption that extracts solvent is 15～20 times of raw material weight.
6. the technology of extracting rutin from the sophora bud according to claim 1 is characterized in that: in the step 1), the temperature of extracting solvent is 15～75 ℃.
7. the technology of extracting rutin from the sophora bud according to claim 6 is characterized in that: the temperature of extracting solvent is 35～55 ℃.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311470A (en) * | 2011-10-13 | 2012-01-11 | 四川砚山菌业有限公司 | Novel rutin extraction technology |
| CN102675388A (en) * | 2011-12-01 | 2012-09-19 | 长沙富能生物技术有限公司 | Novel production method of rutin in accordance with requirement of EP6 (European Pharmacopoeia) 6 edition of European Union |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
| CN103923139A (en) * | 2014-05-08 | 2014-07-16 | 徐大鹏 | Method for extracting rutin from sophora flower buds |
| CN104098636A (en) * | 2014-08-11 | 2014-10-15 | 白心亮 | Method for extracting rutin from Japanese pagoda tree flowers |
| CN104592328A (en) * | 2014-12-16 | 2015-05-06 | 李玉山 | New high-purity deodorizing hesperidin extraction technology |
| CN104829665A (en) * | 2015-04-20 | 2015-08-12 | 西安天一生物技术股份有限公司 | Method for extracting rutin by pre-protecting |
| CN105647230A (en) * | 2016-03-10 | 2016-06-08 | 常州大学 | Natural Flos Sophorae Immaturus dye extraction method and application of natural Flos Sophorae Immaturus dyes |
| CN106397513A (en) * | 2016-10-27 | 2017-02-15 | 广西禅方药业股份有限公司 | Method for refining rutin having content more than or equal to 98% |
| CN106749454A (en) * | 2015-11-25 | 2017-05-31 | 衡阳市骏杰化工有限公司 | A kind of extracting method of rutin |
| CN107827941A (en) * | 2017-11-25 | 2018-03-23 | 衡阳县华盛达农林科技有限公司 | Rutin extraction method |
| CN111718384A (en) * | 2019-06-13 | 2020-09-29 | 贵州益佰女子大药厂有限责任公司 | Method for extracting rutin from sophora flower buds |
| CN114437156A (en) * | 2021-06-18 | 2022-05-06 | 山东东宇生态科技有限公司 | Preparation system and method for extracting rutin from sophora flower buds |
| CN115944666A (en) * | 2022-12-27 | 2023-04-11 | 宁波杰顺生物科技有限公司 | Sophora flower bud extract and preparation method thereof |
| CN116870048A (en) * | 2023-06-27 | 2023-10-13 | 成都市柏林生物科技开发有限公司 | Sophora flower extract and preparation method thereof |
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| CN1373128A (en) * | 2002-01-07 | 2002-10-09 | 王经安 | Enzyme-removing degumming process of preparing rutin |
| CN101423538A (en) * | 2008-12-06 | 2009-05-06 | 广西禅方药业有限公司 | Production process for extracting high-purity birutan from flos sophora |
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| CN1373128A (en) * | 2002-01-07 | 2002-10-09 | 王经安 | Enzyme-removing degumming process of preparing rutin |
| CN101423538A (en) * | 2008-12-06 | 2009-05-06 | 广西禅方药业有限公司 | Production process for extracting high-purity birutan from flos sophora |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102311470A (en) * | 2011-10-13 | 2012-01-11 | 四川砚山菌业有限公司 | Novel rutin extraction technology |
| CN102675388A (en) * | 2011-12-01 | 2012-09-19 | 长沙富能生物技术有限公司 | Novel production method of rutin in accordance with requirement of EP6 (European Pharmacopoeia) 6 edition of European Union |
| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
| CN102718820B (en) * | 2012-07-10 | 2013-07-03 | 刘志强 | Method for extracting and refining rutin |
| CN103923139B (en) * | 2014-05-08 | 2016-04-27 | 罗俊 | A kind of method extracting rutin from the sophora bud |
| CN103923139A (en) * | 2014-05-08 | 2014-07-16 | 徐大鹏 | Method for extracting rutin from sophora flower buds |
| CN104098636B (en) * | 2014-08-11 | 2016-07-27 | 内蒙古昶辉生物科技有限公司 | A kind of method extracting rutin in the Flos Sophorae Immaturus |
| CN104098636A (en) * | 2014-08-11 | 2014-10-15 | 白心亮 | Method for extracting rutin from Japanese pagoda tree flowers |
| CN104592328A (en) * | 2014-12-16 | 2015-05-06 | 李玉山 | New high-purity deodorizing hesperidin extraction technology |
| CN104829665A (en) * | 2015-04-20 | 2015-08-12 | 西安天一生物技术股份有限公司 | Method for extracting rutin by pre-protecting |
| CN106749454A (en) * | 2015-11-25 | 2017-05-31 | 衡阳市骏杰化工有限公司 | A kind of extracting method of rutin |
| CN105647230A (en) * | 2016-03-10 | 2016-06-08 | 常州大学 | Natural Flos Sophorae Immaturus dye extraction method and application of natural Flos Sophorae Immaturus dyes |
| CN106397513A (en) * | 2016-10-27 | 2017-02-15 | 广西禅方药业股份有限公司 | Method for refining rutin having content more than or equal to 98% |
| CN107827941A (en) * | 2017-11-25 | 2018-03-23 | 衡阳县华盛达农林科技有限公司 | Rutin extraction method |
| CN111718384A (en) * | 2019-06-13 | 2020-09-29 | 贵州益佰女子大药厂有限责任公司 | Method for extracting rutin from sophora flower buds |
| CN114437156A (en) * | 2021-06-18 | 2022-05-06 | 山东东宇生态科技有限公司 | Preparation system and method for extracting rutin from sophora flower buds |
| CN115944666A (en) * | 2022-12-27 | 2023-04-11 | 宁波杰顺生物科技有限公司 | Sophora flower bud extract and preparation method thereof |
| CN116870048A (en) * | 2023-06-27 | 2023-10-13 | 成都市柏林生物科技开发有限公司 | Sophora flower extract and preparation method thereof |
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