CN100566728C - A kind of extracting method of bitter buckwheat flavone in high purity - Google Patents
A kind of extracting method of bitter buckwheat flavone in high purity Download PDFInfo
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Abstract
The present invention relates to the extracting method of Radix Et Rhizoma Fagopyri Tatarici flavone, be specially a kind of extracting method of bitter buckwheat flavone in high purity.The present invention solves existing Radix Et Rhizoma Fagopyri Tatarici flavone extracting method paste-forming rate height, purity is low and technological process more complicated, the more high shortcoming of production cost.This extracting method comprise the Radix Et Rhizoma Fagopyri Tatarici seed through reflux, extract,, concentrate and to make concentrated solution and concentrated solution separation and purification; Adopt the ethanol of 30%-80% or methanol or propanol or ethyl acetate solution to carry out reflux, extract,, the ratio that reflux extracting liquid is concentrated into Radix Et Rhizoma Fagopyri Tatarici seed weight and the volume of extracting solution is 1: 4-1: 6; Concentrated solution leaves standstill cooling, under 15 ℃ of-30 ℃ of temperature, and last centrifuge centrifugalize, abandoning supernatant, precipitation part drying promptly obtains the high-purity extract.This extracting method operation reduces, and equipment is simple, and production cost is low, and product stability strengthens, and is particularly suitable for suitability for industrialized production.Extract obtained not only refining degree height, paste-forming rate is below 3%, and total flavones purity is more than 50%.
Description
Technical field
The present invention relates to the extracting method of Radix Et Rhizoma Fagopyri Tatarici flavone, be specially a kind of extracting method of bitter buckwheat flavone in high purity.
Background technology
Semen Fagopyri Esculenti is dicotyledonous buckwheat annual plant, and the Semen Fagopyri Esculenti of cultivation has two types: a kind of is general buck wheat, is called sweet buckwheat (Fagopyrum esculentum) again, and seed is prismatic; Another kind is that (Fagopymmt～aricum), be commonly called as Radix Et Rhizoma Fagopyri Tatarici, littler than general buck wheat grain, corner angle are blunt, the grain color is gloomy, matt, charge level is coarse, the cortex difficult drop-off for hull buckwheat.Compendium of Material Medica record: Radix Et Rhizoma Fagopyri Tatarici nature and flavor hardship, put down, tremble with fear, have physical strength profiting, continuous spirit, sharp knowledge, the effect that has the wide intestinal of sending down the abnormal ascending QI to be good for the stomach.Current clinical medicine is observed and is shown that Semen Fagopyri Esculenti has blood sugar lowering, blood fat reducing, strengthens the effect of body immunity, and patients such as diabetes, hypertension, hyperlipidemia, coronary heart disease, apoplexy are had the auxiliary treatment effect.
Radix Et Rhizoma Fagopyri Tatarici mainly contains flavonoid, aminoacid, organic acid, polypeptide, protein and magnesium, selenium and other trace elements.Wherein known Flavonoid substances has rutin, Quercetin, kaempferol, kaempferol-unification compounds such as 3-0-rutinoside.
Tartary buckwheat extract---Radix Et Rhizoma Fagopyri Tatarici flavone has stronger physiologically active, toxicological experiment proves that it is a material nontoxic, that have no side effect, and the zoopery of pharmacodynamics and clinical observation show that it has effects such as significant blood sugar lowering, blood fat reducing, resisting fatigue, raise immunity.
Be that the kind of raw material mostly is roughly processed product as " Radix Et Rhizoma Fagopyri Tatarici health foodstuff series one Lulibao " (patent of invention in the market with the Radix Et Rhizoma Fagopyri Tatarici, publication number CN1101238A), " hypoglycemic tartarian buckwheat powder and preparation method thereof " (patent of invention, publication number CN 1363230A).And to the further refining purification of Radix Et Rhizoma Fagopyri Tatarici effective ingredient, making its requirement that can meet modern preparation " triple effect ", " three is little " (efficient, quick-acting, long-acting and dosage is little, toxicity is little, side effect is little) is its inexorable trend that realizes the modernization of Chinese medicine; At present the conventional extract preparation of Chinese crude drug mainly is methods such as utilization decocting method, alkali extraction and acid precipitation method, organic solvent method, Amberlyst process, and the extract that these extracting method make often has that hygroscopicity is big, paste-forming rate is higher, dose is big, Flavonoid substances purity is lower, effective ingredient single relatively (only comprising one or more chemical compounds), technological process more complicated, the more high shortcoming of production cost in the Flavonoid substances; Adopt existing extractive technique to extract Radix Et Rhizoma Fagopyri Tatarici flavone, its paste-forming rate is generally about 10%, Flavonoid substances content is lower in the extract, but obtain highly purified tartary buckwheat extract (Flavonoid substances content is more than 50%), paste-forming rate is controlled at below 3%, does not reduce active constituent content again and just has been difficult to.Here the quality (as 3g) of the final dry extract for preparing of the dry quality of medicinal material of paste-forming rate (as the 3%) unit of being meant (as the 100g medical material).Paste-forming rate is more little, shows that the refining degree of extract is high more; But have only paste-forming rate not all right, because if the extract of preparation does not contain active component, then paste-forming rate is more little, and possible pharmacologically active can be more little.
Do not see paste-forming rate at present below 3%, Flavonoid substances purity reaches the report of 50% above Radix Et Rhizoma Fagopyri Tatarici total flavonoids extracting method.
Summary of the invention
The present invention for solve existing Radix Et Rhizoma Fagopyri Tatarici flavone extracting method paste-forming rate height, purity is low and technological process more complicated, the more high shortcoming of production cost, and a kind of extracting method---a kind of extracting method of bitter buckwheat flavone in high purity of new Radix Et Rhizoma Fagopyri Tatarici flavone is provided.
The present invention adopts following technical scheme to realize: a kind of extracting method of bitter buckwheat flavone in high purity, comprise the Radix Et Rhizoma Fagopyri Tatarici seed through reflux, extract,, concentrate and make concentrated solution and concentrated solution separation and purification; The ethanol of employing 30%-80% or methanol or propanol or ethyl acetate solution carry out reflux, extract,, and the ratio that reflux extracting liquid is concentrated into the volume (milliliter) of Radix Et Rhizoma Fagopyri Tatarici seed weight (gram) and extracting solution is 1: 4-1: 6; Concentrated solution leaves standstill cooling, under 15 ℃ of-30 ℃ of temperature, and last centrifuge centrifugalize, abandoning supernatant, precipitation part drying promptly obtains the high-purity extract.The paste-forming rate of the selection final decision extract of reflux, extract, solution and concentration thereof and the purity of Flavonoid substances; Used reflux, extract, solution of the present invention (ethanol or methanol or propanol or ethyl acetate solution) and concentration (30%-80%) thereof have guaranteed that the most of effective ingredient in the Radix Et Rhizoma Fagopyri Tatarici seed is dissolved in the extracting solution, avoided most invalid components (as starch etc.) to be dissolved in extracting solution, thereby guaranteed that extract has low paste-forming rate (below 3%) and highly purified Flavonoid substances (more than 50%).The concentrating degree of extracting solution determines the effect of follow-up centrifugalize purification, concentrated solution rare excessively (being that the Radix Et Rhizoma Fagopyri Tatarici seed weight is too small with the ratio of the volume of extracting solution), active substance in the concentrated solution (comprising Flavonoid substances) centrifugalize fully comes out, the part active substance can stay in concentrated solution, thereby influence the purity of paste-forming rate (in the scope below 3%) and Flavonoid substances, concentrated solution overrich (being that the Radix Et Rhizoma Fagopyri Tatarici seed weight is excessive with the ratio of the volume of extracting solution), concentrated solution can form wall built-up at container inner wall, thereby the loss active substance also can influence the purity of paste-forming rate (in the scope below 3%) and Flavonoid substances.Centrifuging temperature is an important parameter of separation and purification, the improper flavone purity that will greatly influence extract of centrifuging temperature.The centrifuging temperature (15 ℃-30 ℃) that the present invention determines by a large amount of experiments can guarantee fully that flavone purity in the extract is more than 50%.
The centrifuge speed that the present invention selects for use is for being not less than 5000rmin
-1, centrifugation time is not less than 15min.Under this centrifuge parameters, can guarantee that the basic centrifugalize of active substance in the concentrated solution is come out, and the flavone purity of assurance extract is more than 50%.Centrifuge speed is low excessively, centrifugation time is too short, can't guarantee that the active substance in the extracting solution is fully separated, and can't guarantee due paste-forming rate and flavone purity; Certainly greater than 5000rmin
-1Centrifuge speed and surpass the centrifugation time of 15min, paste-forming rate can improve slightly in being no more than 3% scope that (centrifuge speed is high again, centrifugation time is long again, paste-forming rate can not surpass 3% yet, because the final quantity of paste-forming rate has been determined by the preparation of extracting solution), flavone purity also can slightly improve, extract yield thereby improve to a certain extent, but centrifuge to expend the more energy, has a problem of weighing the advantages and disadvantages here.The centrifuge speed that the present invention selects for use is for being not less than 5000rmin
-1, centrifugation time is not less than 15min and guarantees that extract has more satisfactory paste-forming rate and flavone purity and reaches lower bound more than 50%.
Extract solution concentration and in the scope of 30%-80%, can further optimize, to obtain better extraction effect.Extract solution concentration and can select 30%-70%, 30%-60%, 40%-80%, 40%-70%, 50%-70%, 60%-70%.The methanol relative toxicity is bigger.The acetone cost is higher.Preferred alcohol solution of the present invention is as reflux, extract, solution, and the alcoholic solution of preferred 50%-70% is as reflux, extract, solution, with the extraction effect that obtains further to optimize.Concentrating of extracting solution can be adopted methods such as concentrating under reduced pressure, thin film concentration; The drying of extract can adopt technology such as normal pressure oven dry, drying under reduced pressure, spray drying and lyophilization.These methods all are the public methods in this area.
The extracting method of bitter buckwheat flavone in high purity of the present invention is compared with traditional method, and operation reduces, and the production cycle shortens, and equipment is simple, and production cost is low, and product stability strengthens, and is particularly suitable for suitability for industrialized production.Not only make with extra care the degree height with the extract that the method for the invention obtains, paste-forming rate is below 3%, and kept the active component-total flavones of most of Radix Et Rhizoma Fagopyri Tatarici, total flavones purity is more than 50%, make dose much smaller than the Radix Et Rhizoma Fagopyri Tatarici crude extract, have the characteristics of modern Chinese medicine " three is little ", " triple effect ".Therefore the high-purity extract of Radix Et Rhizoma Fagopyri Tatarici provided by the invention can be used in treatment or prevent diabetes and complication thereof as Pharmaceutical composition.Extracting method of the present invention is for more effectively utilizing the Radix Et Rhizoma Fagopyri Tatarici plant resources, and the application of widening the Radix Et Rhizoma Fagopyri Tatarici plant is also significant.
The specific embodiment
Embodiment 1
1. extract
Get Radix Et Rhizoma Fagopyri Tatarici crude drug (dry seed 100g).But drying or oven dry are handled before extracting.Wherein Radix Et Rhizoma Fagopyri Tatarici is meant dicotyledonous buckwheat plant.Under 85 ℃-100 ℃ temperature, with 60% (or 30% or 40% or 45% or 50% or 55% or 60% or 65% or 70% or 80%) the ethanol water reflux, extract, 3 times (1000mLX3) of 1000mL, each 2hr, merge extractive liquid,, filter, filtrate decompression concentrate (60 ℃, 0.08-0.1MPa), to the about 500mL of cumulative volume, room temperature leaves standstill 2-4hr, adopt high speed centrifuge or generic centrifuge, with sample (15 ℃, 20 ℃, 25 ℃, 30 ℃) under 15 ℃～30 ℃, centrifugal rotational speed 5000rmin
-1, centrifugation time is under the condition of 15min that concentrated solution is centrifugal, abandoning supernatant, precipitation put water bath method after, 50 ℃～75 ℃ oven dried 2～72hr, yellowish-brown to yellow powder, be the high-purity extract of Radix Et Rhizoma Fagopyri Tatarici, total amount is 2.22g.Paste-forming rate is 2.22%.
2. content of total flavone is measured:
The reference substance solution preparation: it is an amount of that precision takes by weighing control substance of Rutin, is configured to the solution that 1ml contains 92.8 μ g with 60% ethanol, the need testing solution preparation;
Precision takes by weighing dry this product 0.05g, places the 50mL measuring bottle, adds 60% dissolve with ethanol solution, is settled to scale, weighs, and ultrasonic dissolution is supplied weight, and is standby.
Assay method: get reference substance solution and need testing solution, put in the 10mL volumetric flask, add AlCl
3And KAc, adding to 10mL with 60% ethanol, colour developing 30min presses spectrophotography (2000 editions appendix IVA of Chinese Pharmacopoeia), measures absorbance at the 418nm place, and recording present embodiment total flavones content of material is 55.44%.
Embodiment 2
1. extract
Get Radix Et Rhizoma Fagopyri Tatarici crude drug (dry seed 100g).But drying or oven dry are handled before extracting.Wherein Radix Et Rhizoma Fagopyri Tatarici is meant dicotyledonous buckwheat plant.Under 85 ℃-100 ℃ temperature, with 50% (or 30% or 40% or 45% or 55% or 60% or 65% or 70% or 80%) the methanol-water reflux, extract, 3 times (1000mLX3) of 1000mL, each 2hr, merge extractive liquid,, filter, filtrate decompression concentrate (60 ℃, 0.08-0.1MPa), to the about 600mL of cumulative volume, room temperature leaves standstill 2-4hr, adopt high speed centrifuge or generic centrifuge, with sample (15 ℃, 20 ℃, 25 ℃, 30 ℃) under 15 ℃～30 ℃, centrifugal rotational speed 8000rmin
-1, centrifugation time is under the condition of 30min that concentrated solution is centrifugal, abandoning supernatant, precipitation put water bath method after, 50 ℃～75 ℃ oven dried 2～72hr, yellowish-brown to yellow powder, be the high-purity extract of Radix Et Rhizoma Fagopyri Tatarici, total amount is 2.52g.Paste-forming rate is 2.52%.
2. content of total flavone is measured:
The reference substance solution preparation: it is an amount of that precision takes by weighing control substance of Rutin, is configured to the solution that 1ml contains 92.8 μ g with 60% ethanol, the need testing solution preparation;
Precision takes by weighing dry this product 0.05g, places the 50mL measuring bottle, adds 60% dissolve with ethanol solution, is settled to scale, weighs, and ultrasonic dissolution is supplied weight, and is standby.
Assay method: get reference substance solution and need testing solution, put in the 10mL volumetric flask, add AlCl
3And KAc, adding to 10mL with 60% ethanol, colour developing 30min presses spectrophotography (2000 editions appendix IVA of Chinese Pharmacopoeia), measures absorbance at the 418nm place, and recording present embodiment total flavones content of material is 55.74%.
Embodiment 3
1. extract
Get Radix Et Rhizoma Fagopyri Tatarici crude drug (dry seed 100g).But drying or oven dry are handled before extracting.Wherein Radix Et Rhizoma Fagopyri Tatarici is meant dicotyledonous buckwheat plant.Under 85 ℃-100 ℃ temperature, with 70% (or 30% or 40% or 45% or 50% or 55% or 60% or 65% or 80%) the acetone water reflux, extract, 3 times (1000mLX3) of 1000mL, each 2hr, merge extractive liquid,, filter, filtrate decompression concentrate (60 ℃, 0.08-0.1MPa), to the about 400mL of cumulative volume, room temperature leaves standstill 2-4hr, adopt high speed centrifuge or generic centrifuge, with sample (15 ℃, 20 ℃, 25 ℃, 30 ℃) under 15 ℃～30 ℃, centrifugal rotational speed 13000rmin
-1, centrifugation time is under the condition of 65min that concentrated solution is centrifugal, abandoning supernatant, precipitation put water bath method after, 50 ℃～75 ℃ oven dried 2～72hr, yellowish-brown to yellow powder, be the high-purity extract of Radix Et Rhizoma Fagopyri Tatarici, total amount is 2.82g.Paste-forming rate is 2.82%.
2. content of total flavone is measured:
The reference substance solution preparation: it is an amount of that precision takes by weighing control substance of Rutin, is configured to the solution that 1ml contains 92.8 μ g with 60% ethanol, the need testing solution preparation;
Precision takes by weighing dry this product 0.05g, places the 50mL measuring bottle, adds 60% dissolve with ethanol solution, is settled to scale, weighs, and ultrasonic dissolution is supplied weight, and is standby.
Assay method: get reference substance solution and need testing solution, put in the 10mL volumetric flask, add AlCl
3And KAc, adding to 10mL with 60% ethanol, colour developing 30min presses spectrophotography (2000 editions appendix IVA of Chinese Pharmacopoeia), measures absorbance at the 418nm place, and recording present embodiment total flavones content of material is 55.98%.
Claims (3)
1, a kind of extracting method of bitter buckwheat flavone in high purity, comprise the Radix Et Rhizoma Fagopyri Tatarici seed through reflux, extract,, concentrate and to make concentrated solution and concentrated solution separation and purification, it is characterized by: adopt the ethanol of 30%-80% or methanol or propanol solution to carry out reflux, extract,, the ratio that reflux extracting liquid is concentrated into Radix Et Rhizoma Fagopyri Tatarici seed weight and the volume of extracting solution is 1: 4-1: 6; Concentrated solution leaves standstill cooling, under 15 ℃ of-30 ℃ of temperature, and last centrifuge centrifugalize, centrifuge speed is for being not less than 5000rmin
-1, centrifugation time is not less than 15min, abandoning supernatant, and precipitation part drying promptly obtains total flavones purity at the high-purity extract more than 50%.
2, the extracting method of a kind of bitter buckwheat flavone in high purity as claimed in claim 1 is characterized by: the alcoholic solution that adopts 50%-70% is as reflux, extract, solution.
3, the extracting method of a kind of bitter buckwheat flavone in high purity as claimed in claim 2 is characterized by: the alcoholic solution of employing 60% is as reflux, extract, solution.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101519457B (en) * | 2009-03-17 | 2011-04-13 | 徐德平 | Method for preparing beta-ethoxy rutinose and application thereof for reducing blood glucose |
| CN103040951A (en) * | 2012-09-07 | 2013-04-17 | 赵立地 | Method for extracting buckwheat flavonoids |
| CN102861135B (en) * | 2012-10-01 | 2014-05-28 | 师宗彤野食品有限公司 | Extraction method of buckwheat flavonoids |
| CN102895323A (en) * | 2012-10-11 | 2013-01-30 | 宁波杭州湾新区第九区科技服务有限公司 | Method for extracting buckwheat flavonoid |
| CN103829122A (en) * | 2014-01-09 | 2014-06-04 | 山西春阳生物科技有限公司 | Production method of capsule rich in beta-ethoxy rutinose |
| CN103829123A (en) * | 2014-01-09 | 2014-06-04 | 山西春阳生物科技有限公司 | Method for producing hypoglycemic hypolipemic product by using tartary buckwheat |
| CN104069187B (en) * | 2014-07-24 | 2016-06-01 | 劲牌生物医药有限公司 | The processing method of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici |
| CN107913309A (en) * | 2017-11-28 | 2018-04-17 | 张夏洋 | The method of the total brass of high efficiency extraction bitter buckwheat seed |
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