CN104069187B - The processing method of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici - Google Patents

The present invention discloses the processing method of a kind of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici, comprise the steps: (1) extraction using alcohol: get Radix Et Rhizoma Fagopyri Tatarici raw material, add its weight 3-6 times amount, massfraction is the ethanol of 50%-80%, heating and refluxing extraction 2 times under 60 DEG C of-80 DEG C of conditions, each 2 hours, extracted twice liquid is merged, separation, collect parting liquid; (2) reclaim ethanol: by parting liquid concentrating under reduced pressure, reclaim ethanol, concentrate and contain the bitter buckwheat raw material of 1g to every 1ml concentrated solution, obtain concentrated solution; (3) aqueous precipitation: add 3-6 times amount pure water in concentrated solution, be heated to 60 DEG C-70 DEG C, and after stirring 30-60 minute, it is cooled to 5 DEG C-20 DEG C, leave standstill 2-10 hour, make tartary buckwheat flavone precipitated and separated; (4) precipitate and separate: centrifugation precipitates, and is drying to obtain tartary buckwheat flavone; The inventive method environmental friendliness, technique are simple, production cost is low, be easy to popularization.

The processing method of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici

Technical field

The present invention relates to a kind of method of extraction and isolation active substance from plant, specifically the processing method of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici.

Background technology

Radix Et Rhizoma Fagopyri Tatarici (FagopyrumtatariumGaertn.) also claim hull buckwheat, English Buckwheat by name, belong to polygonaceae (Polygonaceae) Fagopyrum (Fagopyrum), it it is medicine-food two-purpose crop very few in nature, more in Southwestern China mountain area and Shaanxi plantation, mainly it is distributed in high and cold more than 2000 meters areas, belongs to free of contamination green food resource. Containing abundant Vitamin P complex in Radix Et Rhizoma Fagopyri Tatarici, and almost do not have in other cereal, tartary buckwheat flavone is a kind of Polyphenols natural product being present in the flower of Radix Et Rhizoma Fagopyri Tatarici, stem, leaf and seed grain, mainly comprises four kinds of main components such as rutin, Quercetin, kaempferol and morin. Tartary buckwheat flavone has hypoglycemic, reducing blood-fat, anti-oxidant, strengthening immunity, smelting to treat the effects such as cardiovascular and cerebrovascular diseases. Therefore, from Radix Et Rhizoma Fagopyri Tatarici, extract flavonoid substance, as the raw materials for production of protective foods and medicine, become one of direction of bitter buckwheat exploitation.

It is alcohol immersion refluxing extraction that the preparation method of current tartary buckwheat flavone mainly contains following three kinds: one, it is by Radix Et Rhizoma Fagopyri Tatarici united extraction liquid after the immersion refluxing extraction of repeatedly ethanol, reclaim ethanol through concentrating under reduced pressure, then obtain the thick product of tartary buckwheat flavone through drying and crushing; Due in crude product with the black impurity being rich in chlorophyll content, flavones content not high (about 50%). Two is by alcohol reflux concentrated solution, by macroporous resin adsorption, then with ethanol elution, finally reclaim ethanol and dry content higher than 70% tartary buckwheat flavone. Owing to macroporous resin is expensive, the cost of large-scale commercial production is higher, and elution process also needs with a large amount of ethanol, and after having reclaimed ethanol, the Flavonoid substances being insoluble to water precipitates out formation precipitation from solution, thus cause resin to block, cause difficulty to scale operation, further increase its production cost. Three is utilize organic solvent repeatedly to extract alcohol reflux concentrated solution, separation lower sediment dry tartary buckwheat extract. And human body is had certain toxicity by overwhelming majority organic solvent, and environment is had certain harm, it is unfavorable for large-scale industrial production.

Summary of the invention

It is an object of the invention to provide a kind of environmental friendliness, technique is simple, production cost is low, the tartary buckwheat flavone extracting and purifying method of easy popularization; Tartary buckwheat flavone content >=85% that present method obtains.

The processing method of the present invention's extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici, comprises the steps:

(1) extraction using alcohol: get Radix Et Rhizoma Fagopyri Tatarici raw material, adds its weight 3-6 times amount, massfraction is the ethanol of 50%-80%, heating and refluxing extraction 2 times under 60 DEG C of-80 DEG C of conditions, each 2 hours, is merged by extracted twice liquid, and parting liquid is collected in separation;

(2) reclaiming ethanol: by parting liquid concentrating under reduced pressure, reclaim ethanol, thickening temperature controls below 75 DEG C, concentrates and contains the bitter buckwheat raw material of 1g to every 1ml concentrated solution, obtains concentrated solution;

(3) aqueous precipitation: add 3-6 times amount pure water in concentrated solution, be heated to 60 DEG C-70 DEG C, and after stirring 30-60 minute, it is cooled to 5 DEG C-20 DEG C, leave standstill 2-10 hour, make tartary buckwheat flavone precipitated and separated;

(4) precipitate and separate: centrifugation precipitates, and is drying to obtain at being deposited in 60-80 DEG C; Tartary buckwheat flavone content >=85%.

The preferred technical solution of the present invention is:

(1) extraction using alcohol: take Radix Et Rhizoma Fagopyri Tatarici raw material, add its weight 3 times, massfraction be 80% food-grade ethanol carry out circumfluence distillation, Extracting temperature is 60 DEG C, 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, obtaining centrifugate, it is desired to centrifugate clear, the precipitation after centrifugal is directly drained;

(2) reclaim ethanol: the extracting solution after centrifugal adopts economic benefits and social benefits thickener to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 DEG C, concentrate and contain Radix Et Rhizoma Fagopyri Tatarici raw material 1g to 1ml concentrated solution, obtain concentrated solution;

(3) aqueous precipitation: add 3 times amount pure water in concentrated solution, be heated to 65 DEG C, and stir 30 minutes, then cooling down is to 5 DEG C;

(4) precipitate and separate: leave standstill 5 hours, tartary buckwheat flavone precipitated and separated, adopts horizontal helical type whizzer precipitation separation, and rotating speed is 5400r/min, is drying to obtain tartary buckwheat flavone at being deposited in 70 DEG C, and after testing, tartary buckwheat flavone content is 86.5%.

The present invention utilizes tartary buckwheat flavone to be insoluble to the feature of water, by the concentrated solution aqueous precipitation of bitter buckwheat extracting solution after reclaiming ethanol, removes the water-soluble impurity in concentrated solution, and filtering separation precipitates, thus reaches the object of separation tartary buckwheat flavone.

The present invention compared with prior art, has following feature:

1. environmental friendliness, technique is simple, and with short production cycle, cost is low, easily promotes; Only use ethanol as Extraction solvent in extraction step, decrease production cost than existing processing method; 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 improving tartary buckwheat flavone content;

2. extraction yield height: owing to production process is simple, decrease the loss in technological process, extraction rate reached, to 1.5%, improves 0.2-0.3 percentage point than existing technique;

3. DNA purity height: bitter buckwheat concentrated solution heats after adding water, then cooling precipitates, and can remove the water-soluble impurity of major part, tartary buckwheat flavone content >=85% of gained; Higher than prior art 3-4 percentage point.

Embodiment

Embodiment 1

(1) extraction using alcohol: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, adding 300L food grade 80% ethanol and carry out circumfluence distillation, Extracting temperature is 60 DEG C, 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, obtaining centrifugate, it is desired to centrifugate clear, the precipitation after centrifugal is directly drained;

(2) ethanol is reclaimed: the extracting solution after centrifugal adopts economic benefits and social benefits thickener to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 DEG C, concentrates to 100L, obtains concentrated solution;

(3) aqueous precipitation: add 3 times amount pure water in concentrated solution, be heated to 65 DEG C, and stir 30 minutes, then cooling down is to 5 DEG C;

(4) precipitate and separate: leave standstill 5 hours, tartary buckwheat flavone precipitated and separated, adopts horizontal helical type whizzer precipitation separation, and rotating speed is 5400r/min, is drying to obtain tartary buckwheat flavone at being deposited in 70 DEG C, and after testing, tartary buckwheat flavone content is 86.5%.

Embodiment 2

(1) extraction using alcohol: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, adding 400L food grade 60% ethanol and carry out circumfluence distillation, Extracting temperature is 70 DEG C, 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, obtaining centrifugate, it is desired to centrifugate clear, the precipitation after centrifugal is directly drained;

(2) ethanol is reclaimed: the extracting solution after centrifugal adopts economic benefits and social benefits thickener to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 65 DEG C, concentrates to 100L, obtains concentrated solution;

(3) aqueous precipitation: add 4 times amount pure water in concentrated solution, be heated to 60 DEG C, and stir 45 minutes, then cooling down is to 10 DEG C;

(4) precipitate and separate: leave standstill 2 hours, tartary buckwheat flavone precipitated and separated, adopts horizontal helical type whizzer precipitation separation, and rotating speed is 5400r/min, is drying to obtain at being deposited in 60 DEG C, and after testing, tartary buckwheat flavone content is 85.2%.

Embodiment 3

(1) extraction using alcohol: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, adding 600L food grade 50% ethanol and carry out circumfluence distillation, Extracting temperature is 80 DEG C, 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, obtaining centrifugate, it is desired to centrifugate clear, the precipitation after centrifugal is directly drained;

(2) ethanol is reclaimed: the extracting solution after centrifugal adopts economic benefits and social benefits thickener to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 65 DEG C, concentrates to 100L, obtains concentrated solution;

(3) aqueous precipitation: add 6 times amount pure water in concentrated solution, be heated to 70 DEG C, and stir 60 minutes, then cooling down is to 15 DEG C;

(4) precipitate and separate: leave standstill 10 hours, tartary buckwheat flavone precipitated and separated, adopts horizontal helical type whizzer precipitation separation, and rotating speed is 5400r/min, is drying to obtain tartary buckwheat flavone at being deposited in 80 DEG C, and after testing, tartary buckwheat flavone content is 85.3%.

The following is the inventive method and existing methodical contrast situation:

From above contrast it can be seen that comprehensive tartary buckwheat flavone content and receipts rate, it is low that the inventive method has cost really, receipts rate height, the advantage that content is high, and easy and simple to handle, environmental protection.

1. the processing method of extraction purification tartary buckwheat flavone from Radix Et Rhizoma Fagopyri Tatarici, it is characterised in that comprise the steps:

(1) extraction using alcohol: take Radix Et Rhizoma Fagopyri Tatarici raw material double centner, adding 300L food grade 80% ethanol and carry out circumfluence distillation, Extracting temperature is 60 DEG C, 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, obtaining centrifugate, it is desired to centrifugate clear, the precipitation after centrifugal is directly drained;

(2) ethanol is reclaimed: the extracting solution after centrifugal adopts economic benefits and social benefits thickener to carry out concentrating under reduced pressure, and reclaims ethanol, and thickening temperature is 60 DEG C, concentrates to 100L, obtains concentrated solution;

(3) aqueous precipitation: add 3 times amount pure water in concentrated solution, be heated to 65 DEG C, and stir 30 minutes, then cooling down is to 5 DEG C;

(4) precipitate and separate: leave standstill 5 hours, tartary buckwheat flavone precipitated and separated, adopts horizontal helical type whizzer precipitation separation, and rotating speed is 5400r/min, is drying to obtain tartary buckwheat flavone at being deposited in 70 DEG C, and after testing, tartary buckwheat flavone content is 86.5%.