CN105541940A - Method for extracting rutin - Google Patents
Method for extracting rutin Download PDFInfo
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- CN105541940A CN105541940A CN201510926215.0A CN201510926215A CN105541940A CN 105541940 A CN105541940 A CN 105541940A CN 201510926215 A CN201510926215 A CN 201510926215A CN 105541940 A CN105541940 A CN 105541940A
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- rutin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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Abstract
The invention belongs to the technical field of extraction and separation of natural products, and particularly relates to a method for extracting rutin. The method comprises the steps: combining ultrasonic waves and microwaves, firstly, dissolving with alkali liquor, then bearing with an acid, finally precipitating from a liquid phase, and thus directly obtaining high-purity rutin. In addition, the content of alcohols and carboxylic acids in impurities is preciously little, so as to be favorable for further high-purity refining.
Description
Technical field
The invention belongs to natural product extraction separation technology field, be specifically related to the extracting method of a kind of rutin.
Background technology
The sophora bud is the bud of leguminous plants Chinese scholartree (SophorajaponicaL.), begin to be loaded in " Japan hanako materia medica ", be classified as top grade in Shennong's Herbal, be now listed in first integration of drinking and medicinal herbs list of health ministry, there is cooling blood for hemostasis, the effects such as clearing liver-fire.The flavones ingredient such as rutin and Quercetin is rich in the sophora bud, wherein main active ingredient rutin, there is the normal elasticity of maintenance and recovery kapillary, strengthen its resistibility, prevent many-sided physiologically actives such as hemocyte cohesion, normal in medicine industry is that main raw material extracts rutin with the sophora bud, mainly sells to the countries and regions such as Japan, South East Asia and America and Europe.China is the country of origin of the sophora bud, and all there is plantation all parts of the country, mostly is wild.Due to the factor such as kind and environmental difference, it is uneven that sophora bud quality is produced in various places.At present, relatively less to the research report of Different sources Quantitative Determination of Rudin in Flos Sophorae, for determining best crude drug source, this experiment have collected the sophora bud in the places of production such as Guangxi, Hunan, Shaanxi and Vietnam, adopt high performance liquid chromatography, the Different sources sophora bud is carried out to the mensuration of rutin content, for the quality evaluating the sophora bud provides scientific basis.
By the hydroxyl on quercetin (Quercetin) 3 and rutinose (Rutinose) (for the disaccharide that glucose (Glucose) and rhamnosyl (Rhamnose) form), dewater rutin (Rutin) glycosides synthesized.Rutin (Rutin) is extensively present in vegitabilia, has now found that plant containing rutin is at least more than 70 kinds, as tobacco leaf, sophora flower, buckwheat and taraxacum etc.Especially the highest with content in Flos Sophorae Immaturus (the unopened bud for plant Sophorajaponica) and buckwheat, can be used as a large amount of raw material extracting rutin.Rutin is buff powder or superfine needle crystal, the crystal water containing three molecules, and fusing point is 174 ~ 178 DEG C, anhydride 188 ~ 190 DEG C.Solubleness: be 1:10000 in cold water; 1:200 in hot water; Cold ethanol 1:650; Hot ethanol 1:60; Cold pyridine 1:12.Be slightly soluble in acetone, ethyl acetate, be insoluble to benzene, ether, chloroform, sherwood oil, be dissolved in alkali and in yellow.Rutin has the effect of vitamin P sample, contributes to the normal elasticity keeping and recover capillary vessel, mainly as the auxiliary therapeutical agent preventing and treating essential hypertension, also can be used for other hemorrhages of preventing and treating for want of caused by rutin.
The extracting method of tradition rutin is: first sophora bud high temperature is stifling, pulverizing, and boiling water is scalded in rear loading diacolation jar, and after saturated limewater diacolation, collect percolate, then regulate pH value with dilute hydrochloric acid, leave standstill, rutin crystallization, obtains rutin runic thing; Because sophora bud high temperature is stifling and boiling water is scalded and all can be destroyed rutin, cause yield to reduce, alkali extraction and acid precipitation process afterwards also can destroy structure and the precipitation of rutin, and a large amount of sour waters of discharge bring pollution to environment, deal with very difficult.Whole leaching process requires the processing condition such as high temperature, strong acid and strong base, and the cycle is long, and the three wastes of generation are many, and rutin yield can only reach 18 ~ 20%.
The method that the sophora bud ferments is extracted rutin by present domestic useful rutin metabolizing enzymes, and roughly method is: the sophora bud is cleaned oven dry and is placed in fermentor tank, add metabolizing enzymes, proceed to extractor after sealed fermenting; In extractor, add methyl alcohol, alcohol mixed solvent, stirring, filtration obtain filtrate; Recycling design after filtrate distillation, obtains Extraction of rutin thing; In Extraction of rutin thing, add the mixed solvent of acetone, sherwood oil and n-Octanol, ordinary method stirs, extract, filter, filtrate is distilled, and obtains high-purity rutoside finished product after recycling design.Because the method employs mixed solvent in a large number, although yield increases than traditional method, mixed solvent is not easily separated, causes production cost significantly to raise; The recovery and reuse of mixed solvent are again very complicated technical barriers.And whole method complicated operation, can bring loss and the environmental pollution of a large amount of organic solvent, and investment goods is too much, the production cycle is long, is not suitable for promoting.
Summary of the invention
For solving the deficiencies in the prior art, the invention provides the extracting method of a kind of rutin.
An extracting method for rutin, comprises the following steps:
1) by sophora bud crushing grinding powdered, with the weight of sophora bud powder for benchmark, the sophora bud powder of 6 ~ 8g is joined in the hot water of 70 ~ 90 DEG C of 150 ~ 200ml, add in the sodium hydroxide solution of the 0.5mol/L of 70 ~ 90 DEG C of 100 ~ 150ml again, ultrasonic disperse 20 ~ 40 minutes, filter, obtain sample solution.
Concrete, step 1) in, the ultrasonic frequency of ultrasonic disperse is 25 ~ 40KHz, ultrasonic power 40 ~ 100w.
2) regulating step 1) pH value of sample solution that obtains is 4 ~ 6, cooling, suction filtration, obtains sample.
3) by step 2) sample dissolution that obtains is in the dehydrated alcohol of 100 ~ 200mL; homogenous disperse; add the polyacrylic acid of 1.5 ~ 2.0g again; esterification is carried out under acylating agent, normal temperature and mechanical agitation; in reaction process, interval drips catalyzer, reacts 4 ~ 6 hours, 60 ~ 90 DEG C of condensing refluxes; be concentrated into 60 ~ 120mL, obtain middle crude product.
Preferably, step 3) in, polyacrylic number-average molecular weight is 1000 ~ 5000.
Concrete, step 3) in, the process that interval drips catalyzer is: dripped 2 ~ 3 every 1 ~ 2 hour, repeat 2 ~ 3 times.
4) by step 3) the middle crude product that obtains mixes with the sodium hydroxide solution of the 1mol/L of 150 ~ 250ml, and be hydrolyzed under microwave condition, under water bath with thermostatic control condition, be acidified to pH value is afterwards 4 ~ 6, and cooling is separated out, filter, and obtains the thin product of rutin.
Preferably, step 4) in, the temperature of water bath with thermostatic control is 16 ~ 25 DEG C, and the power of microwave hydrolysis is 100 ~ 1000w.
By the extracting method of rutin provided by the present invention, can directly obtain highly purified rutin.In its impurity, the content of alcohols and carboxylic-acid is few, is conducive to further high-purity refining.
Embodiment
Be described principle of the present invention and feature below, illustrated embodiment, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
1) by sophora bud crushing grinding powdered, with the weight of sophora bud powder for benchmark, the sophora bud powder of 6.5g is joined in the hot water of 85 DEG C of 170ml, add in the sodium hydroxide solution of the 0.5mol/L of 85 DEG C of 120ml again, ultrasonic disperse 30 minutes, ultrasonic frequency is 30KHz, and ultrasonic power 80w filters, and obtains sample solution.
2) regulating step 1) pH value of sample solution that obtains is 5, cooling, suction filtration, obtains sample.
3) by step 2) sample dissolution that obtains is in the dehydrated alcohol of 150mL, homogenous disperse, add the polyacrylic acid of 1.7g again, esterification is carried out under thionyl chloride, normal temperature and mechanical agitation, in reaction process, interval drips DMF, reacts 4.5 hours, 80 DEG C of condensing refluxes, be concentrated into 80mL, obtain middle crude product.
4) by step 3) the middle crude product that obtains mixes with the sodium hydroxide solution of the 1mol/L of 150ml, be hydrolyzed under microwave condition, the power of microwave hydrolysis is 400w, under water bath with thermostatic control condition, be acidified to pH value is afterwards 4, the temperature of water bath with thermostatic control is 25 DEG C, cooling is separated out, filtration, obtains the thin product of rutin, purity 97.7%.
Embodiment 2
1) by sophora bud crushing grinding powdered, with the weight of sophora bud powder for benchmark, the sophora bud powder of 7.5g is joined in the hot water of 88 DEG C of 190ml, add in the sodium hydroxide solution of the 0.5mol/L of 85 DEG C of 150ml again, ultrasonic disperse 20 minutes, ultrasonic frequency is 25KHz, and ultrasonic power 75w filters, and obtains sample solution.
2) regulating step 1) pH value of sample solution that obtains is 6, cooling, suction filtration, obtains sample.
3) by step 2) sample dissolution that obtains is in the dehydrated alcohol of 180mL, homogenous disperse, add the polyacrylic acid of 2.0g again, esterification is carried out under thionyl chloride, normal temperature and mechanical agitation, in reaction process, interval drips DMF, reacts 4 hours, 90 DEG C of condensing refluxes, be concentrated into 110mL, obtain middle crude product.
4) by step 3) the middle crude product that obtains mixes with the sodium hydroxide solution of the 1mol/L of 200ml, be hydrolyzed under microwave condition, the power of microwave hydrolysis is 800w, under water bath with thermostatic control condition, be acidified to pH value is afterwards 6, the temperature of water bath with thermostatic control is 18 DEG C, cooling is separated out, filtration, obtains the thin product of rutin, purity 98.0%.
Embodiment 3
1) by sophora bud crushing grinding powdered, with the weight of sophora bud powder for benchmark, the sophora bud powder of 7g is joined in the hot water of 80 DEG C of 175ml, add in the sodium hydroxide solution of the 0.5mol/L of 85 DEG C of 135ml again, ultrasonic disperse 40 minutes, ultrasonic frequency is 40KHz, and ultrasonic power 100w filters, and obtains sample solution.
2) regulating step 1) pH value of sample solution that obtains is 4, cooling, suction filtration, obtains sample.
3) by step 2) sample dissolution that obtains is in the dehydrated alcohol of 200mL, homogenous disperse, add the polyacrylic acid of 1.8g again, esterification is carried out under thionyl chloride, normal temperature and mechanical agitation, in reaction process, interval drips DMF, reacts 5.5 hours, 90 DEG C of condensing refluxes, be concentrated into 100mL, obtain middle crude product.
4) by step 3) the middle crude product that obtains mixes with the sodium hydroxide solution of the 1mol/L of 250ml, be hydrolyzed under microwave condition, the power of microwave hydrolysis is 600w, under water bath with thermostatic control condition, be acidified to pH value is afterwards 6, the temperature of water bath with thermostatic control is 25 DEG C, cooling is separated out, filtration, obtains the thin product of rutin, purity 98.2%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an extracting method for rutin, is characterized in that, comprises the following steps:
1) by sophora bud crushing grinding powdered, with the weight of sophora bud powder for benchmark, the sophora bud powder of 6 ~ 8g is joined in the hot water of 70 ~ 90 DEG C of 150 ~ 200ml, add in the sodium hydroxide solution of the 0.5mol/L of 70 ~ 90 DEG C of 100 ~ 150ml again, ultrasonic disperse 20 ~ 40 minutes, filter, obtain sample solution;
2) regulating step 1) pH value of sample solution that obtains is 4 ~ 6, cooling, suction filtration, obtains sample;
3) by step 2) sample dissolution that obtains is in the dehydrated alcohol of 100 ~ 200mL, homogenous disperse, add the polyacrylic acid of 1.5 ~ 2.0g again, esterification is carried out under acylating agent, normal temperature and mechanical agitation, in reaction process, interval drips catalyzer, reacts 4 ~ 6 hours, 60 ~ 90 DEG C of condensing refluxes, be concentrated into 60 ~ 120mL, obtain middle crude product;
4) by step 3) the middle crude product that obtains mixes with the sodium hydroxide solution of the 1mol/L of 150 ~ 250ml, and be hydrolyzed under microwave condition, under water bath with thermostatic control condition, be acidified to pH value is afterwards 4 ~ 6, and cooling is separated out, filter, and obtains the thin product of rutin.
2. the extracting method of rutin according to claim 1, is characterized in that: step 1) in, the ultrasonic frequency of ultrasonic disperse is 25 ~ 40KHz, ultrasonic power 40 ~ 100w.
3. the extracting method of rutin according to claim 2, is characterized in that: step 3) in, polyacrylic number-average molecular weight is 1000 ~ 5000.
4. the extracting method of rutin according to claim 3, is characterized in that, step 3) in, the process that interval drips catalyzer is: dripped 2 ~ 3 every 1 ~ 2 hour, repeat 2 ~ 3 times.
5. the extracting method of rutin according to claim 4, is characterized in that, step 4) in, the temperature of water bath with thermostatic control is 16 ~ 25 DEG C.
6. the extracting method of rutin according to claim 5, is characterized in that, step 4) in, the power of microwave hydrolysis is 100 ~ 1000w.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510926215.0A CN105541940A (en) | 2015-12-11 | 2015-12-11 | Method for extracting rutin |
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| CN201510926215.0A CN105541940A (en) | 2015-12-11 | 2015-12-11 | Method for extracting rutin |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501356A (en) * | 2017-08-16 | 2017-12-22 | 湖南科技学院 | A kind of method that rutin is extracted from the sophora bud |
| CN107509848A (en) * | 2016-06-16 | 2017-12-26 | 巩发永 | A kind of preparation method of saqima made of buckwheat flour |
| CN107722072A (en) * | 2017-11-07 | 2018-02-23 | 何本科 | A kind of extracting method of rutin |
| CN108329369A (en) * | 2018-04-08 | 2018-07-27 | 河南师范大学 | A kind of preparation method of high-content rutin |
| CN115109108A (en) * | 2022-06-21 | 2022-09-27 | 云南八凯农业开发有限公司 | Method for extracting buckwheat rutin |
Citations (3)
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| 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 |
| CN103435667A (en) * | 2013-09-17 | 2013-12-11 | 南京通泽农业科技有限公司 | Novel method for extracting rutin from pagodatree flower bud |
| CN104130300A (en) * | 2014-08-11 | 2014-11-05 | 白心亮 | Method for extracting rutin from pagodatree flower bud |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN103435667A (en) * | 2013-09-17 | 2013-12-11 | 南京通泽农业科技有限公司 | Novel method for extracting rutin from pagodatree flower bud |
| CN104130300A (en) * | 2014-08-11 | 2014-11-05 | 白心亮 | Method for extracting rutin from pagodatree flower bud |
Non-Patent Citations (2)
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107509848A (en) * | 2016-06-16 | 2017-12-26 | 巩发永 | A kind of preparation method of saqima made of buckwheat flour |
| CN107501356A (en) * | 2017-08-16 | 2017-12-22 | 湖南科技学院 | A kind of method that rutin is extracted from the sophora bud |
| CN107722072A (en) * | 2017-11-07 | 2018-02-23 | 何本科 | A kind of extracting method of rutin |
| CN108329369A (en) * | 2018-04-08 | 2018-07-27 | 河南师范大学 | A kind of preparation method of high-content rutin |
| CN108329369B (en) * | 2018-04-08 | 2021-02-12 | 河南师范大学 | Preparation method of high-content rutin |
| CN115109108A (en) * | 2022-06-21 | 2022-09-27 | 云南八凯农业开发有限公司 | Method for extracting buckwheat rutin |
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