CN104069187A - Technological method extracting duckwheat flavone from duckwheat - Google Patents
Technological method extracting duckwheat flavone from duckwheat Download PDFInfo
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- CN104069187A CN104069187A CN201410354754.7A CN201410354754A CN104069187A CN 104069187 A CN104069187 A CN 104069187A CN 201410354754 A CN201410354754 A CN 201410354754A CN 104069187 A CN104069187 A CN 104069187A
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- fagopyri tatarici
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Abstract
The invention discloses a technological method extracting duckwheat flavone from duckwheat. The technological method comprises the following steps: (1) extraction of ethyl alcohol: taking a duckwheat raw material; adding ethyl alcohol of which the mass is 3-6 times of mass of the duckwheat raw material and the mass fraction is 50%-80% of mass fraction of the duckwheat; conducting heating, reflowing and extracting at a temperature of 60 DEG C-80 DEG C for two times, wherein each time lasts for two hours; combing the extracted solution of the two times; conducting separation; collecting the separated liquid; (2) recovery of the ethyl alcohol: concentrating the separated liquid under reduced pressure; recovering the ethyl alcohol; conducting concentration until 1 ml of the concentrated solution contains 1 g of the duckwheat raw material to obtain a concentrated solution; (3) water adding and sedimentation: adding purified water of which the mass is 3-6 times of the concentrated solution into the concentrated solution; heating the solution to 60 DEG C-70 DEG C; stirring for 30-60 min; cooling to 5 DEG C-20 DEG C; still standing for 2-10 hours; enabling the duckwheat flavone to be sedimentary and layered; (4) sedimentation separation: conducting centrifugal separation sedimentation; conducting drying, and obtaining the duck wheat flavone. The technological method is environment-friendly, simple in technology, low in preparation cost, and easy to popularize.
Description
Technical field
The present invention relates to a kind of method of extracting separating active substances from plant, specifically from Radix Et Rhizoma Fagopyri Tatarici, extract the process of purification Radix Et Rhizoma Fagopyri Tatarici flavone.
Background technology
Radix Et Rhizoma Fagopyri Tatarici (Fagopyrum tatarium Gaertn.) also claim hull buckwheat, English Buckwheat by name, belong to Polygonaceae (Polygonaceae) Fagopyrum (Fagopyrum), it is the medicine-food two-purpose crop that occurring in nature is very few, in Southwestern China mountain area and Shaanxi plantation more, mainly be distributed in high and cold 2000 meters of above areas, belong to free of contamination pollution-free food resource.In Radix Et Rhizoma Fagopyri Tatarici, contain abundant bioflavonoids, and almost do not have in other corn, Radix Et Rhizoma Fagopyri Tatarici flavone is a kind of Polyphenols natural product in flower, stem, leaf and the seed that is present in Radix Et Rhizoma Fagopyri Tatarici, mainly comprises four kinds of main components such as rutin, Quercetin, kaempferol and morin.Radix Et Rhizoma Fagopyri Tatarici flavone has blood sugar lowering, blood fat reducing, antioxidation, enhancing immunity, smelting to treat the effects such as cardiovascular and cerebrovascular disease.Therefore, from Radix Et Rhizoma Fagopyri Tatarici, extract flavonoid substance, as the raw materials for production of health food and medicine, become one of direction of Radix Et Rhizoma Fagopyri Tatarici exploitation.
The preparation method of Radix Et Rhizoma Fagopyri Tatarici flavone mainly contains following three kinds at present: the one, and soak with ethanol reflux, extract,, by Radix Et Rhizoma Fagopyri Tatarici merge extractive liquid, after the immersion reflux, extract, of ethanol repeatedly, through concentrating under reduced pressure, reclaim ethanol, then through drying and crushing, obtain the thick product of Radix Et Rhizoma Fagopyri Tatarici flavone; Due in crude product with the black impurity that is rich in chlorophyll composition, flavones content not high (50% left and right).The 2nd, by alcohol reflux concentrated solution, by macroporous resin adsorption, then use ethanol elution, finally reclaim ethanol dry content higher than 70% Radix Et Rhizoma Fagopyri Tatarici flavone.Because macroporous resin is expensive, the cost of large-scale industrial production is higher, and elution process also needs with a large amount of ethanol, and after having reclaimed ethanol, water-fast Flavonoid substances is separated out and is formed precipitation from solution, thereby cause resin to stop up, to large-scale production, cause difficulty, further increased its production cost.The 3rd, utilize organic solvent repeatedly to extract alcohol reflux concentrated solution, separated lower sediment is also dried to obtain tartary buckwheat extract.And most organic solvents have certain toxicity to human body, and environment is had to certain harm, be unfavorable for large-scale commercial production.
Summary of the invention
The object of this invention is to provide a kind of environmental friendliness, technique is simple, production cost is low, the Radix Et Rhizoma Fagopyri Tatarici flavone method for extraction and purification of easy popularization; Resulting Radix Et Rhizoma Fagopyri Tatarici flavone content >=85% of this method.
The present invention extracts the process of purification Radix Et Rhizoma Fagopyri Tatarici flavone from Radix Et Rhizoma Fagopyri Tatarici, comprises the steps:
(1) ethanol extraction: get Radix Et Rhizoma Fagopyri Tatarici raw material, add the ethanol that its weight 3-6 doubly measures, mass fraction is 50%-80%, heating and refluxing extraction is 2 times under 60 ℃ of-80 ℃ of conditions, each 2 hours, extracted twice liquid is merged, separation, collects separating medium;
(2) reclaim ethanol: by separating medium concentrating under reduced pressure, reclaim ethanol, thickening temperature is controlled at below 75 ℃, be concentrated into every 1ml concentrated solution containing 1g Radix Et Rhizoma Fagopyri Tatarici raw material, obtain concentrated solution;
(3) aqueous precipitation: add 3-6 doubly to measure pure water in concentrated solution, be heated to 60 ℃-70 ℃, and stir after 30-60 minute and be cooled to 5 ℃-20 ℃, standing 2-10 hour, makes Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated;
(4) precipitate and separate: centrifugalize precipitation, will be deposited at 60-80 ℃ and be drying to obtain; Radix Et Rhizoma Fagopyri Tatarici flavone content >=85%.
The preferred technical solution of the present invention is:
(1) ethanol extraction: take Radix Et Rhizoma Fagopyri Tatarici raw material, add the food stage ethanol that 3 times of its weight, mass fraction are 80% to carry out hot reflux extraction, extracting temperature is 60 ℃, and extraction time is 2 hours, extraction time is 2 times, extracting solution merges, and adopts Alfa Laval disc centrifuge to carry out high speed centrifugation, and the time is 40min, rotating speed is 6000r/min, centrifugal liquid, require centrifugal liquid clear, the precipitation after centrifugal is directly drained;
(2) reclaim ethanol: the extracting solution after centrifugal adopts dual-effect concentrator to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 ℃, be concentrated into 1ml concentrated solution containing Radix Et Rhizoma Fagopyri Tatarici raw material 1g, obtain concentrated solution;
(3) aqueous precipitation: in concentrated solution, add 3 times of amount pure water, be heated to 65 ℃, and stir 30 minutes, then cooling down to 5 ℃;
(4) precipitate and separate: standing 5 hours, Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated, adopted Horizontal helical type centrifuge precipitation separation, and rotating speed is 5400 r/min, is deposited at 70 ℃ and is drying to obtain Radix Et Rhizoma Fagopyri Tatarici flavone, and after testing, Radix Et Rhizoma Fagopyri Tatarici flavone content is 86.5%.
The present invention utilizes the water-fast feature of Radix Et Rhizoma Fagopyri Tatarici flavone, and the concentrated solution aqueous precipitation by Radix Et Rhizoma Fagopyri Tatarici extracting solution after reclaiming ethanol is removed the water-solubility impurity in concentrated solution, and isolated by filtration precipitates, thereby reaches the object of separated Radix Et Rhizoma Fagopyri Tatarici flavone.
The present invention compared with prior art, has following characteristics:
1. environmental friendliness, technique is simple, with short production cycle, and cost is low, easily promotes; Only in extraction step, use ethanol as extracting solvent, than existing process, reduced production cost; Production time reduced to 48 hours by 72 hours.The present invention will extract concentrated solution aqueous precipitation, and a step can reach the object that improves Radix Et Rhizoma Fagopyri Tatarici flavone content;
2. extraction ratio is high: because production process is simple, reduced the loss in technical process, extraction rate reached to 1.5%, improves 0.2-0.3 percentage point than existing technique;
3. DNA purity is high: Radix Et Rhizoma Fagopyri Tatarici concentrated solution heats after adding water, then cooling precipitate, can remove most water-solubility impurity, Radix Et Rhizoma Fagopyri Tatarici flavone content >=85% of gained; Than the high 3-4 percentage point of prior art.
The specific embodiment
Embodiment 1
(1) ethanol extraction: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, add 300L food stage 80% ethanol to carry out hot reflux extraction, extracting temperature is 60 ℃, and extraction time is 2 hours, extraction time is 2 times, extracting solution merges, and adopts Alfa Laval disc centrifuge to carry out high speed centrifugation, and the time is 40min, rotating speed is 6000r/min, centrifugal liquid, require centrifugal liquid clear, the precipitation after centrifugal is directly drained;
(2) reclaim ethanol: the extracting solution after centrifugal adopts dual-effect concentrator to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 ℃, is concentrated into 100L, obtains concentrated solution;
(3) aqueous precipitation: in concentrated solution, add 3 times of amount pure water, be heated to 65 ℃, and stir 30 minutes, then cooling down to 5 ℃;
(4) precipitate and separate: standing 5 hours, Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated, adopted Horizontal helical type centrifuge precipitation separation, and rotating speed is 5400 r/min, is deposited at 70 ℃ and is drying to obtain Radix Et Rhizoma Fagopyri Tatarici flavone, and after testing, Radix Et Rhizoma Fagopyri Tatarici flavone content is 86.5%.
Embodiment 2
(1) ethanol extraction: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, add 400 L food stage 60% ethanol to carry out hot reflux extraction, extracting temperature is 70 ℃, and extraction time is 2 hours, extraction time is 2 times, extracting solution merges, and adopts disc centrifuge to carry out high speed centrifugation, and the time is 50min, rotating speed is more than 6000r/min, centrifugal liquid, require centrifugal liquid clear, the precipitation after centrifugal is directly drained;
(2) reclaim ethanol: the extracting solution after centrifugal adopts dual-effect concentrator to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 65 ℃, is concentrated into 100L, obtains concentrated solution;
(3) aqueous precipitation: in concentrated solution, add 4 times of amount pure water, be heated to 60 ℃, and stir 45 minutes, then cooling down to 10 ℃;
(4) precipitate and separate: standing 2 hours, Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated, adopted Horizontal helical type centrifuge precipitation separation, and rotating speed is 5400 r/min, is deposited at 60 ℃ and is drying to obtain, and after testing, Radix Et Rhizoma Fagopyri Tatarici flavone content is 85.2%.
Embodiment 3
(1) ethanol extraction: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, add 600 L food stage 50% ethanol to carry out hot reflux extraction, extracting temperature is 80 ℃, and extraction time is 2 hours, extraction time is 2 times, extracting solution merges, and adopts Alfa Laval disc centrifuge to carry out high speed centrifugation, and the time is 60min, rotating speed is 6000r/min, centrifugal liquid, require centrifugal liquid clear, the precipitation after centrifugal is directly drained;
(2) reclaim ethanol: the extracting solution after centrifugal adopts dual-effect concentrator to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 65 ℃, is concentrated into 100L, obtains concentrated solution;
(3) aqueous precipitation: in concentrated solution, add 6 times of amount pure water, be heated to 70 ℃, and stir 60 minutes, then cooling down to 15 ℃;
(4) precipitate and separate: standing 10 hours, Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated, adopted Horizontal helical type centrifuge precipitation separation, and rotating speed is 5400 r/min, is deposited at 80 ℃ and is drying to obtain Radix Et Rhizoma Fagopyri Tatarici flavone, and after testing, Radix Et Rhizoma Fagopyri Tatarici flavone content is 85.3%.
Below the inventive method and existing methodical contrast situation:
From above contrast, can find out, comprehensive Radix Et Rhizoma Fagopyri Tatarici flavone content and yield, the inventive method has that cost is low really, and yield is high, the advantage that content is high, and also easy and simple to handle, environmental protection.
Claims (2)
1. from Radix Et Rhizoma Fagopyri Tatarici, extract the process of purification Radix Et Rhizoma Fagopyri Tatarici flavone, it is characterized in that comprising the steps:
(1) ethanol extraction: get Radix Et Rhizoma Fagopyri Tatarici raw material, add its weight 3-6 doubly, the mass fraction ethanol that is 50%-80%, under 60 ℃ of-80 ℃ of conditions, heating and refluxing extraction is 2 times, each 2 hours, extracted twice liquid is merged, separation, collects separating medium;
(2) reclaim ethanol: by separating medium concentrating under reduced pressure, reclaim ethanol, thickening temperature is controlled at below 75 ℃, be concentrated into every 1ml concentrated solution containing 1g Radix Et Rhizoma Fagopyri Tatarici raw material, obtain concentrated solution;
(3) aqueous precipitation: add 3-6 times of pure water in concentrated solution, be heated to 60 ℃-70 ℃, and stir after 30-60 minute and be cooled to 5 ℃-20 ℃, standing 2-10 hour, makes Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated;
(4) precipitate and separate: precipitation separation, will be deposited at 60-80 ℃ and be drying to obtain Radix Et Rhizoma Fagopyri Tatarici flavone, wherein Radix Et Rhizoma Fagopyri Tatarici flavone content >=85%.
2. the process of extracting purification Radix Et Rhizoma Fagopyri Tatarici flavone from Radix Et Rhizoma Fagopyri Tatarici according to claim 1, is characterized in that comprising the steps:
(1) ethanol extraction: take Radix Et Rhizoma Fagopyri Tatarici raw material, add the food stage ethanol that 3 times of its weight, mass fraction are 80% to carry out hot reflux extraction, extracting temperature is 60 ℃, and extraction time is 2 hours, extraction time is 2 times, extracting solution merges, and adopts Alfa Laval disc centrifuge to carry out high speed centrifugation, and the time is 40min, rotating speed is 6000r/min, centrifugal liquid, require centrifugal liquid clear, the precipitation after centrifugal is directly drained;
(2) reclaim ethanol: the extracting solution after centrifugal adopts dual-effect concentrator to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 ℃, be concentrated into 1ml concentrated solution containing Radix Et Rhizoma Fagopyri Tatarici raw material 1g, obtain concentrated solution;
(3) aqueous precipitation: in concentrated solution, add 3 times of amount pure water, be heated to 65 ℃, and stir 30 minutes, then cooling down to 5 ℃;
(4) precipitate and separate: standing 5 hours, Radix Et Rhizoma Fagopyri Tatarici flavone precipitated and separated, adopted Horizontal helical type centrifuge precipitation separation, and rotating speed is 5400 r/min, is deposited at 70 ℃ and is drying to obtain Radix Et Rhizoma Fagopyri Tatarici flavone; After testing, Radix Et Rhizoma Fagopyri Tatarici flavone content is 86.5%.
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Cited By (5)
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| CN105795480A (en) * | 2016-04-08 | 2016-07-27 | 吉林鑫水科技开发有限公司 | Extraction and analysis method and application of flavone in buckwheat |
| CN107913309A (en) * | 2017-11-28 | 2018-04-17 | 张夏洋 | The method of the total brass of high efficiency extraction bitter buckwheat seed |
| CN111518660A (en) * | 2020-04-29 | 2020-08-11 | 劲牌有限公司 | Health-care white spirit with effect of relieving alcoholic brain injury and preparation method thereof |
| CN112592413A (en) * | 2021-01-06 | 2021-04-02 | 黑龙江省药品检验研究中心 | Preparation method of wild buckwheat rhizome polysaccharide |
| CN115974826A (en) * | 2022-12-28 | 2023-04-18 | 西昌航飞苦荞科技发展有限公司 | Method for preparing tartary buckwheat quercetin from tartary buckwheat flavone extract |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105795480A (en) * | 2016-04-08 | 2016-07-27 | 吉林鑫水科技开发有限公司 | Extraction and analysis method and application of flavone in buckwheat |
| CN107913309A (en) * | 2017-11-28 | 2018-04-17 | 张夏洋 | The method of the total brass of high efficiency extraction bitter buckwheat seed |
| CN111518660A (en) * | 2020-04-29 | 2020-08-11 | 劲牌有限公司 | Health-care white spirit with effect of relieving alcoholic brain injury and preparation method thereof |
| CN112592413A (en) * | 2021-01-06 | 2021-04-02 | 黑龙江省药品检验研究中心 | Preparation method of wild buckwheat rhizome polysaccharide |
| CN115974826A (en) * | 2022-12-28 | 2023-04-18 | 西昌航飞苦荞科技发展有限公司 | Method for preparing tartary buckwheat quercetin from tartary buckwheat flavone extract |
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Address after: 435000 9 Shengming Road, Jinshan street, Huangshi economic and Technological Development Zone, Hubei Province Patentee after: Jingpai Zhengtang Pharmaceutical Co.,Ltd. Address before: 435100 south of Jinshan Avenue, Jinshan Industrial Park, Huangshi City, Hubei Province Patentee before: JING BRAND BIO-MEDICINE Co.,Ltd. |