CN104098636B - A kind of method extracting rutin in the Flos Sophorae Immaturus - Google Patents
A kind of method extracting rutin in the Flos Sophorae Immaturus Download PDFInfo
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Abstract
The invention discloses a kind of new method extracting rutin from the Flos Sophorae Immaturus, comprise the following steps: dry after the dry Flos Sophorae Immaturus is processed with dry blowing method at 70 DEG C and pulverize；Add the surfactant Tween 20 and OP 15 etc. of rational proportion, ethanol with 60%～70% carries out ultrasonic assistant extraction under certain condition, extracting solution is stood crystallization, sucking filtration obtains rutin crude product, rutin crude product is refined by n-butyl alcohol, standing crystallization and dry at 130 DEG C, obtaining the rutin product of purity more than 98%, yield reaches more than 22%.Comprehensive the above, the inventive method is easy and simple to handle, and extraction efficiency is high, it is adaptable to produce reality.
Description
Technical field
The application relates to a kind of method extracting rutin from the Flos Sophorae Immaturus.
Background technology
The Flos Sophorae Immaturus is the dry flower and alabastrum of leguminous plant Sophora japonica L., and the history being used as medicine existing more than 2000 year, Shennong's Herbal is classified as top grade.The rutin contained in the Flos Sophorae Immaturus about 8%～28%(is according to the Flos Sophorae Immaturus place of production and the difference of collecting the time and difference).Rutin, also known as rutin, rutin, belongs to flavonoid glycoside compound, has cooling blood for hemostasis, effect of purging liver-fire, can reduce capillary permeability and fragility, promote hyperplasia and prevent hemocyte from condensing, also have antiinflammatory, antiallergic, diuresis, antitussive, blood fat reducing etc. act on.Rutin has been used as the auxiliary treatment of hypertension clinically, prevents because rutin lacks other hemorrhages caused, and prevents and treat diabetes and merge hyperlipidemia.It addition, rutin as natural antioxidant and uses flavochrome, it is also widely used in health food and cosmetic kind.
Rutin extraction method common in the art has boiling water to decoct, alkali carries acid heavy, ultrasonic or microwave extraction, surname extraction, supercritical CO2Extract.Common purification process has crystallization, macroporous adsorbent resin process, high performance liquid chromatography process etc.；Along with surfactant being widely used in fields such as chemical industry, food, article of everyday use production and water process, in a lot of Chinese medicines water insoluble or be not readily dissolved in the effective ingredient of water, such as Flavonoid substances, alkaloid, volatile oil etc., adsorption can be formed on its surface or interface by surfactant, or form molecular aggregate in the solution, and then change these compositions dissolubility in aqueous, improve the extraction efficiency of Chinese medicine, reduce extraction cost, the feature of safety and environmental protection.Prior art has the report using surfactant auxiliary Extraction of rutin, but uses a kind of surfactant more.Such as (" linguistic term of Rutin Extracting Technology " such as Li Jinxiu, Li Jinxiu, Gong Shengzhao, Huang Qiujin, Guangdong chemical industry, 1st phase in 2003, P15) have employed following methods and carry out the extraction of rutin: the Flos Sophorae Immaturus is pulverized, add the water of 5 times amount, pH8～9 is regulated with lime water, it is 50～60 DEG C in temperature and extracts 20～30min, filter, repeatedly extract by similarity condition 3 times, filtrate salt acid for adjusting pH is 3, add 0.5% Surfactant OP, it is incubated 10min at 60～70 DEG C, stand 30min, filter, washing, it is dried, obtain rutin product yield 18.4%, content 96%.
Summary of the invention
The application aims to provide a kind of new method extracting rutin from the Flos Sophorae Immaturus.
The method of the invention comprises the following steps:
(1) pretreatment: with dry blowing method, the dry Flos Sophorae Immaturus is processed at 70 DEG C 30min, then goes out colloid with 70 DEG C of hot water drip washing, is dried afterwards and is pulverized as 20-80 mesh；
(2) extract: Flos Sophorae Immaturus granule is added 1～the Na of the Borax of 5%, 1～5%2SO3With the 60 of 15-30 times～70% in ethanol, use sodium bicarbonate regulation pH to 9～10, add the Tween 20 and 0.05～the OP-15 of 0.3% of 0.3～0.5%, lucifuge ultrasonic extraction 10～30min under conditions of 20～30kHz, 30～50 DEG C, filtering afterwards, filtrate lucifuge at 30～50 DEG C is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before, adds 5% activated carbon in the filtrate after merging, lucifuge stirring 10min at 30～50 DEG C, by the acidification of filtrate after filtration carbon removal to pH=3～4, standing 20～30min, sucking filtration obtains rutin crude product；
(3) refined: rutin crude product is placed in baking oven, dry at 40 DEG C to without alcohol taste, it is gradually heating to 130 DEG C of drying again, the dry rutin obtained is added in n-butyl alcohol and be heated to dissolving, filter, in filtrate, add deionized water, use the ultrasonic lucifuge process 20～30min at 0～5 DEG C of 20～30kHz, standing crystallization and dry at 130 DEG C, obtaining the rutin of purity more than 98%, yield reaches more than 22%.
Further, in step of the present invention (2), it is preferably added to 3～the Borax of 4% and the Na of 1%2SO3。
Further, in step of the present invention (2), it is preferably added to the Tween 20 and 0.05～the OP-15 of 0.2% of 0.35～0.45%.
Further, in step of the present invention (2), the condition of ultrasonic extraction preferably at 30kHz, extract 15～25min at 40～50 DEG C.
Further, in step of the present invention (3), adding the volume of n-butyl alcohol with the ratio of Flos Sophorae Immaturus raw materials quality is 20～30mL/g；Adding the volume of deionized water with the ratio of Flos Sophorae Immaturus raw materials quality is 2～3mL/g；The condition of ultrasonic Treatment preferably processes 20～30min under 30 kHz.
Further, in step of the present invention (2), more preferably add 0.35～the Tween 20 and 0.05～the OP-15 of 0.15% of 0.45%.
The present invention employs the surfactant Tween 20 and OP-15 of rational proportion in extraction step, and the surfactant of this proportioning makes extraction time and crystallization time all have shortening, and extraction efficiency improves, then is aided with ultrasound wave, makes yield increase substantially.Use n-butyl alcohol that rutin is refined, can effectively remove the residual impurity such as colloid, fatty acid, improve the purity of rutin.From the point of view of each step the most of the present invention, the method for the invention is easy and simple to handle, and extraction efficiency is high, it is adaptable to produce reality.
Accompanying drawing explanation
Fig. 1 is rutin standard substance HPLC spectrogram.
Fig. 2 is the HPLC spectrogram of rutin end-product in embodiment 2.
Detailed description of the invention
Embodiment 1
50g being dried the Flos Sophorae Immaturus and processes 30min at 70 DEG C with dry blowing method, then go out colloid with 70 DEG C of hot water drip washing, being dried afterwards and pulverizing is 20 mesh.Flos Sophorae Immaturus granule is added Borax, the Na of 1% of 3%2SO3In ethanol with the 60 of 20 times～70%, using sodium bicarbonate regulation pH to 9～10, add the Tween 20 and OP-15 of 0.15% of 0.35%, in 30kHz, lucifuge ultrasonic extraction 20min under conditions of 40 DEG C, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before；Filtrate after merging adds 5% activated carbon, lucifuge stirring 10min at 40 DEG C, by the acidification of filtrate after filtration carbon removal to pH=3～4, stand 20min, sucking filtration obtains rutin crude product.Rutin crude product is placed in baking oven, dry at 40 DEG C to without alcohol taste, it is gradually heating to 130 DEG C of drying again, the dry rutin obtained is added in 1300mL n-butyl alcohol and be heated to dissolving, filter, 130mL deionized water is added in filtrate, use the ultrasonic lucifuge process 20min at 0～5 DEG C of 30kHz, stand crystallization, leach rear 130 DEG C of drying, obtain the rutin 11.38g of purity 98.66%, yield 22.76%.
Embodiment 2
80g being dried the Flos Sophorae Immaturus and processes 30min at 70 DEG C with dry blowing method, then go out colloid with 70 DEG C of hot water drip washing, being dried afterwards and pulverizing is 40 mesh.Flos Sophorae Immaturus granule is added Borax, the Na of 1% of 4%2SO3In ethanol with the 60 of 25 times～70%, using sodium bicarbonate regulation pH to 9～10, add the Tween 20 and OP-15 of 0.10% of 0.40%, in 30kHz, lucifuge ultrasonic extraction 20min under conditions of 40 DEG C, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before；Filtrate after merging adds 5% activated carbon, lucifuge stirring 10min at 40 DEG C, by the acidification of filtrate after filtration carbon removal to pH=3～4, stand 20min, sucking filtration obtains rutin crude product.Rutin crude product is placed in baking oven, dry at 40 DEG C to without alcohol taste, it is gradually heating to 130 DEG C of drying again, the dry rutin obtained is added in 2L n-butyl alcohol and be heated to dissolving, filter, 200mL deionized water is added in filtrate, use the ultrasonic lucifuge process 20min at 0～5 DEG C of 30kHz, stand crystallization, leach rear 130 DEG C of drying, obtain the rutin 18.57g of purity 98.81%, yield 23.21%.
Embodiment 3
120g being dried the Flos Sophorae Immaturus and processes 30min at 70 DEG C with dry blowing method, then go out colloid with 70 DEG C of hot water drip washing, being dried afterwards and pulverizing is 60 mesh.Flos Sophorae Immaturus granule is added Borax, the Na of 1% of 3%2SO3In ethanol with the 60 of 30 times～70%, using sodium bicarbonate regulation pH to 9～10, add the Tween 20 and OP-15 of 0.05% of 0.45%, in 30kHz, lucifuge ultrasonic extraction 20min under conditions of 40 DEG C, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before；Filtrate after merging adds 5% activated carbon, lucifuge stirring 10min at 40 DEG C, by the acidification of filtrate after filtration carbon removal to pH=3～4, stand 20min, sucking filtration obtains rutin crude product.Rutin crude product is placed in baking oven, dry at 40 DEG C to without alcohol taste, it is gradually heating to 130 DEG C of drying again, the dry rutin obtained is added in 3L n-butyl alcohol and be heated to dissolving, filter, 300mL deionized water is added in filtrate, use the ultrasonic lucifuge process 20min at 0～5 DEG C of 30kHz, stand crystallization, leach rear 130 DEG C of drying, obtain the rutin 27.16g of purity 98.86%, yield 22.63%.
Embodiment 4
The present embodiment compared for using the surfactant of proportioning of the present invention in Extraction of rutin step and being used alone Tween 20 to rutin finished product productivity and the impact of purity.First 50g is dried the Flos Sophorae Immaturus process with the preprocess method described in the embodiment of the present application 1.Extraction step operation is: the Flos Sophorae Immaturus granule that pulverizing is 20 mesh is joined the Borax of 3%, the Na of 1%2SO3In ethanol with the 60 of 20 times～70%, using sodium bicarbonate regulation pH to 9～10, add the Tween 20 of 0.5%, in 30kHz, lucifuge ultrasonic extraction 20min under conditions of 40 DEG C, filter afterwards, filtrate lucifuge at 40 DEG C is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before；Filtrate after merging adds 5% activated carbon, lucifuge stirring 10min at 40 DEG C, by the acidification of filtrate after filtration carbon removal to pH=3～4, stand 20min, sucking filtration obtains rutin crude product.With the process for purification described in the embodiment of the present application 1, rutin crude product is refined the most again.More than operation does 2 groups of parallel check experiments respectively with method described in embodiment 1, quality and the purity of the rutin end-product obtained is contrasted, and result is as shown in the table:
Claims (6)
1. the method extracting rutin from the Flos Sophorae Immaturus, it is characterised in that comprise the following steps:
(1) pretreatment: with dry blowing method, the dry Flos Sophorae Immaturus is processed at 70 DEG C 30min, then goes out colloid with 70 DEG C of hot water drip washing, afterwards will
It dries and pulverizes as 20-80 mesh；
(2) extract: Flos Sophorae Immaturus granule is added 1～the Na of the Borax of 5%, 1～5%2SO3With the 60 of 15-30 times～70% in ethanol,
Use sodium bicarbonate regulation pH to 9～10, add the Tween 20 and 0.05～the OP-15 of 0.15% of 0.35～0.45%,
Lucifuge ultrasonic extraction 10～30min under conditions of 20～30kHz, 30～50 DEG C, filters afterwards, and filtrate is at 30～50 DEG C
Lower lucifuge is standby；Filtering residue extracts once with above-mentioned same condition again, and the filtrate obtained merges with filtrate before, after merging
Filtrate in add 5% activated carbon, lucifuge stirring 10min at 30～50 DEG C, the acidification of filtrate after carbon removal will be filtered to pH=3～4,
Standing 20～30min, sucking filtration obtains rutin crude product；
(3) refined: rutin crude product is placed in baking oven, dry extremely without alcohol taste at 40 DEG C, then be gradually heating to 130 DEG C of drying, will obtain
Dry rutin add in n-butyl alcohol and be heated to dissolving, filter, in filtrate, add deionized water, use 20～30kHz super
Sound lucifuge at 0～5 DEG C processes 20～30min, stands crystallization and dries at 130 DEG C, obtaining the rutin of purity more than 98%,
Yield reaches more than 22%.
2. the as claimed in claim 1 method extracting rutin, it is characterised in that: in described step (2), add 3～the Borax of 4% and
The Na of 1%2SO3。
3. the as claimed in claim 1 or 2 method extracting rutin, it is characterised in that: in described step (2), 30kHz, 40～
Ultrasonic extraction 15～25min under the conditions of 50 DEG C.
4. the method extracting rutin as claimed in claim 1 or 2, it is characterised in that: in described step (3), add the body of n-butyl alcohol
Long-pending and Flos Sophorae Immaturus raw materials quality ratio is 20～30mL/g；Add the ratio of the volume of deionized water and Flos Sophorae Immaturus raw materials quality be 2～
3mL/g；Ultrasonic Treatment 20～30min under the conditions of 30kHz.
5. the as claimed in claim 4 method extracting rutin, it is characterised in that: in described step (2), 30kHz, 40～50 DEG C
Under the conditions of ultrasonic extraction 15～25min.
6. the as claimed in claim 4 method extracting rutin, it is characterised in that: in described step (3), add the volume of n-butyl alcohol with
The ratio of Flos Sophorae Immaturus raw materials quality is 20～30mL/g；Adding the volume of deionized water with the ratio of Flos Sophorae Immaturus raw materials quality is 2～3mL/g；
Ultrasonic Treatment 20～30min under the conditions of 30kHz.
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| CN104558073B (en) * | 2014-12-26 | 2017-10-03 | 苏州亚宝药物研发有限公司 | A kind of preparation method of rutin |
| 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% |
| 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 (2)
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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 |
| CN101817857A (en) * | 2010-04-29 | 2010-09-01 | 桂林市振达生物科技有限责任公司 | Process for extracting rutin from sophora japonica |
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2014
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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 |
| CN101817857A (en) * | 2010-04-29 | 2010-09-01 | 桂林市振达生物科技有限责任公司 | Process for extracting rutin from sophora japonica |
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