CN106749454A - A kind of extracting method of rutin - Google Patents
A kind of extracting method of rutin Download PDFInfo
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- CN106749454A CN106749454A CN201510832001.7A CN201510832001A CN106749454A CN 106749454 A CN106749454 A CN 106749454A CN 201510832001 A CN201510832001 A CN 201510832001A CN 106749454 A CN106749454 A CN 106749454A
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- rutin
- sophora bud
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Abstract
The present invention provides a kind of extracting method of rutin, and its production stage includes:The sophora bud is steamed 0.9-1 hours with container, is crushed after cooling, be placed in extractor；Sodium pyrosulfite and borax are added, its weight proportion is 0.8 ~ 1.2:4.5~5.5；20% alcohol solvent is added, at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring；The sophora bud is leached with gauze, 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collect supernatant；The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring, and the sophora bud is leached with gauze, and 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collects supernatant；Filtrate obtained by filtering twice is merged；Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 65 ~ 70 DEG C；The thick hydrochloric acid regulation pH value of enriching is 3.2 ~ 5.0, and refrigeration stands overnight；Weigh packaging.The present invention solves that Extraction of rutin purity not high, complex process, extracting cycle be long and technical problem of inefficiency.
Description
Technical field
The present invention relates to the extraction field of rutin, and in particular to a kind of extracting method of novel rutin.
Background technology
Rutin, is also called rutin, and citrin, rutin, Lu Ding, road fourth powder, Lu Tong, network leads to, Rutin.Main application is anti-inflammatory, antiviral etc., is being clinically used for preventing and treating cerebral hemorrhage, hypertension, retinal hemorrhage, purple scar and acute hemorrhagic ephritis.Its pharmacological action is：Rutin belongs to vitamin drug, plays the role of to reduce capillary permeability and fragility, keeps and recover the normal elasticity of capillary.The production technology of rutin is main to be completed by operations such as alcohol extracting, extraction, chromatography, crystallizations.But, existing rutin extraction technology processing cost is very high, and complex process, and purity is relatively low, of poor quality.
The content of the invention
It is an object of the invention to overcome prior art to be extracted from the sophora bud, rutin complex process, extracting cycle are long, impurity is more, purity is low and are difficult to the problem for purifying, a kind of technique that rutin is extracted from the sophora bud is provided, the process is simple, extracting cycle is short, the rutin purity of extraction is high, impurity is few, and low cost.
In order to realize the purpose of foregoing invention, the technical solution adopted by the present invention is as follows：
A kind of extracting method of rutin is provided, is comprised the following steps：
The first step：The sophora bud is steamed 0.9-1 hours with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 0.8 ~ 1.2:4.5~5.5；Because containing adjacent two phenolic hydroxyl group, property less stable in rutin molecule；Exposure in atmosphere can slow oxidation be changed into crineous, be oxidized easily decomposition.Borax can reach the purpose of protection with adjacent diphenol hydroxy combining, therefore when extracting rutin, often add a small amount of borax, be conducive to the extraction of high-purity rutoside.
3rd step：20% alcohol solvent is added, at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring；The removal of impurity can more fully be gone in hot bath using alcohol solvent, and the generation of deposited phenomenon is prevented from the alcohol solvent of 20% concentration, it is ensured that the purity of the rutin for extracting.
4th step：The sophora bud is leached with gauze, 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring, and the sophora bud is leached with gauze, and 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collects supernatant；Again repeat extract can further by the Extraction of rutin in filter residue out, increase clear liquid in rutin content.
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 65 ~ 70 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 3.2 ~ 5.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Compared with prior art, the technical scheme that the present invention is provided greatly improves the production purity of rutin, and extraction process compared with the prior art for the simpler, cycle time that extracts, the produced pollution is smaller, and the rutin precision extracted is higher, better quality.
Further, weight proportion is 1 in second step:5.
Further, bath temperature is 65 DEG C in the 3rd step.
Further, stirred in the 3rd step and extract 55min.
Further, it is centrifuged with the rotating speed of 3000r/m in the 4th step.
Further, 7min is centrifuged in the 4th step.
Further, be concentrated under reduced pressure removal ethanol in the 5th step at 68 DEG C.
Further, pH value is 3.5 in the 9th step.
In order to technique effect of the invention is better described, the heavy method of acid and technical scheme are put forward with alkali extraction and acid precipitation, hot water carries out rutin preparation to the 40g sophora bud.
| Extracting method | The consumption sophora bud/g | Extract dry weight/g | Extract rutin content/(mg/g) | Rutin purity/% |
| Alkali extraction and acid precipitation | 40 | 1.389 | 627.0 | 45.1% |
| Hot water puies forward the heavy method of acid | 40 | 0.8732 | 469.2 | 53.7% |
| Hot water puies forward 20% alcohol precipitation impurity removal method | 40 | 0.7290 | 719.9 | 98.8% |
Specific embodiment
In order that technical problem solved by the invention, technical scheme and beneficial effect become more apparent, with reference to embodiments, the present invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not intended to limit the present invention.All any modification, equivalent and improvement made within the spirit and principles in the present invention etc., should be included within the scope of the present invention.
Embodiment 1
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 1 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 0.8:4.5；
3rd step：20% alcohol solvent is added, at being 60 DEG C in water-bath, 50min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 2800r/m centrifugation 6min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 DEG C in water-bath, 50min is extracted in stirring, and the sophora bud is leached with gauze, 2800r/m centrifugation 6min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 65 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 3.2, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 2
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 0.9 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 1.2:5.5；
3rd step：20% alcohol solvent is added, at being 70 DEG C in water-bath, 60min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 3200r/m centrifugation 8min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 70 DEG C in water-bath, 60min is extracted in stirring, and the sophora bud is leached with gauze, 3200r/m centrifugation 8min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 70 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 5.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 3
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 1 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 1:5；
3rd step：20% alcohol solvent is added, at being 65 DEG C in water-bath, 55min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 3000r/m centrifugation 7min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 65 DEG C in water-bath, 55min is extracted in stirring, and the sophora bud is leached with gauze, 3000r/m centrifugation 7min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 68 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 3.5, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 4
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 0.9 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 1.2:4.5；
3rd step：20% alcohol solvent is added, at being 60 DEG C in water-bath, 50min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 2800r/m centrifugation 6min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 DEG C in water-bath, 50min is extracted in stirring, and the sophora bud is leached with gauze, 2800r/m centrifugation 6min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 65 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 3.2, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 5
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 0.9 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 0.8：5.5；
3rd step：20% alcohol solvent is added, at being 70 DEG C in water-bath, 50min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 3200r/m centrifugation 8min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 70 DEG C in water-bath, 50min is extracted in stirring, and the sophora bud is leached with gauze, and 3200r/m collects supernatant from 8min；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 70 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 5.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 6
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 1 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 1:5；
3rd step：20% alcohol solvent is added, at being 60 DEG C in water-bath, 50min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 2800r/m centrifugation 6min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 DEG C in water-bath, 50min is extracted in stirring, and the sophora bud is leached with gauze, 2800r/m centrifugation 6min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 68 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 5.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Embodiment 7
A kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 0.9 hour with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 1.2:4.5；
3rd step：20% alcohol solvent is added, at being 70 DEG C in water-bath, 60min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 2800r/m centrifugation 6min collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 70 DEG C in water-bath, 560min is extracted in stirring, and the sophora bud is leached with gauze, 2800r/m centrifugation 6min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 70 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 4.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
Claims (8)
1. a kind of extracting method of rutin, comprises the following steps：
The first step：The sophora bud is steamed 0.9-1 hours with container, is crushed after cooling, be placed in extractor；
Second step：Sodium pyrosulfite and borax are added, its weight proportion is 0.8 ~ 1.2:4.5~5.5；
3rd step：20% alcohol solvent is added, at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring；
4th step：The sophora bud is leached with gauze, 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collect supernatant；
5th step：The sophora bud that will be leached adds 20% alcohol solvent again, and at being 60 ~ 70 DEG C in water-bath, 50 ~ 60min is extracted in stirring, and the sophora bud is leached with gauze, and 2800r/m ~ 3200r/m is centrifuged 6 ~ 8min, collects supernatant；
6th step：Filtrate obtained by filtering twice is merged；
7th step：Filtrate is concentrated at 85 DEG C, ethanol is added, refrigeration is stood overnight；
8th step：Filtered, taken filtrate, be concentrated under reduced pressure removal ethanol at 65 ~ 70 DEG C；
9th step：The thick hydrochloric acid regulation pH value of enriching is 3.2 ~ 5.0, and refrigeration stands overnight；
Tenth step：Weigh packaging.
2. rutin extraction method according to claim 1, it is characterised in that weight proportion is 1 in second step:5.
3. rutin extraction method according to claim 1, it is characterised in that bath temperature is 65 DEG C in the 3rd step.
4. rutin extraction method according to claim 1, it is characterised in that stirred in the 3rd step and extract 55min.
5. rutin extraction method according to claim 1, it is characterised in that be centrifuged with the rotating speed of 3000r/m in the 4th step.
6. rutin extraction method according to claim 1, it is characterised in that 7min is centrifuged in the 4th step.
7. rutin extraction method according to claim 1, it is characterised in that be concentrated under reduced pressure removal ethanol in the 5th step at 68 DEG C.
8. rutin extraction method according to claim 1, it is characterised in that pH value is 3.5 in the 9th step.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111635443A (en) * | 2020-06-15 | 2020-09-08 | 深圳市蜜踪生物科技有限公司 | Sophora flower extraction process |
| 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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| CN102718820A (en) * | 2012-07-10 | 2012-10-10 | 刘志强 | Method for extracting and refining rutin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111635443A (en) * | 2020-06-15 | 2020-09-08 | 深圳市蜜踪生物科技有限公司 | Sophora flower extraction process |
| 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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Application publication date: 20170531 |