CN102816637A - Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids - Google Patents
Combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids Download PDFInfo
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Abstract
The invention relates to a combined extraction method of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids. The method includes: crushing dry Paeonia ostii seeds, conducting ultrasonic assisted extraction to obtain Paeonia ostii seed primary oil, separating Paeonia ostii seed powder in a petroleum ether suspending solution, drying a petroleum ether solution under reduced pressure, drying degreased Paeonia ostii seed powder, carrying out ultrasonic extraction to obtain Paeonia ostii seed total flavonoids, separating Paeonia ostii seed powder from an ethanol suspending solution, and performing pressure reduced evaporation on an ethanol solution so as to obtain the Paeonia ostii seed total flavonoids. Specifically, petroleum ether or a mixed solvent of petroleum ether and n-hexane is adopted for ultrasonic assisted extraction of the Paeonia ostii seed primary oil, and the ethanol solution is employed for assisting ultrasonic extraction of Paeonia ostii seed total flavonoids. The method is characterized by simultaneous extraction of Paeonia ostii seed oil and Paeonia ostii seed total flavonoids, and the technological process is coherent and compact. The extraction rates of the Paeonia ostii seed oil and the Paeonia ostii seed total flavonoids are high. The extracted Paeonia ostii seed powder has high purity and a good color, and can reach the national standards through simple refining. The Paeonia ostii seed total flavonoids extracted by the method have high activity, strong antioxidant capacity, and good bacteriostatic capacity.
Description
Technical field: the invention belongs to the natural product extracting technique field, particularly a kind of associating process for extracting obtains red seed oil of phoenix and the red seed total flavones of phoenix successively.
Background technology: Feng Dan (Paeonia ostii T. Hong et J. X. Zhang), promptly Tongling tree peony belongs to south of the River tree peony population, belongs to medicinal tree peony kind.The phoenix root bark of tree peony is one of Anhui four big Chinese medicinal materialss, has very high health care and pharmaceutical use.
Feng Dan mainly originated in Tongling Shun Anzhen, Zhong Ming town and He Wan town, Nanling County, Wuhu City, because its unique soil and weather condition, the root bark of tree peony that is produced facts have proved to drug effect best, and Feng Dan was classified as " national geography sign protection product " in 2006.Through detecting: lipid content is 34.31%-38.06% in the white seed of medicinal tree peony kind Feng Dan; Starch content is 19.42%-20.25%; Reducing sugar content is 12.29%-15.28%, and protein contnt is 12.03-13.75%, and absolute water content is 11.46%-17.17%; General flavone content is 1.03%, and research shows that the red seed total flavones of phoenix is anti-oxidant remarkable with bacteriostatic action.
Through retrieval, the patent of invention of Beijing Technology and Business University's application, the patent No.: CN200810246716.4, the day for announcing: on 06 03rd, 2009, classification number: A23D9/02.This invention relates to a kind of method of extracting peony seed oil that the invention discloses.This method is that the tree peony powder of seeds is put into supercritical CO
2Carry out supercritical extraction in the abstraction instrument, collect grease, obtain peony seed oil provided by the invention.In this method, the temperature of supercritical extraction is 30-50 ℃, and preferred 45 ℃, the pressure of supercritical extraction is 20-35MPa, preferred 30MPa; The time of supercritical extraction is 0.5-2 hour, preferred 1 hour.The particle diameter of tree peony powder of seeds is at the 20-60 order.The supercritical CO of the extraction peony seed oil that this invention provides
2Process for extracting does not need organic reagent, and extraction and separation method is easy; Extraction yield is up to 27%, and the grease unsaturated fatty acids of gained is compared with existing organic solvent extracting access method up to 90%; Linolenic and linoleic content in the tree peony oil all raises to some extent, extracts more complete.
Through retrieving domestic and international related data, do not find a kind of combined extraction technology so far as yet, can disposablely extract red seed oil of phoenix and the red seed total flavones of phoenix respectively.Therefore, the present invention provides a kind of combined extraction technology method, can be successively from the red seed of fresh phoenix, extract red seed oil of phoenix and the red seed total flavones of phoenix, for the development and use of phoenix pellet seed provide powerful guarantee.
Summary of the invention
The object of the present invention is to provide the associating process for extracting of red seed oil of a kind of phoenix and the red seed total flavones of phoenix, extract successively and obtain red seed oil of phoenix and the red seed total flavones of phoenix.
Technical scheme of the present invention is following: the associating process for extracting, particularly this method of red seed oil of a kind of phoenix and the red seed total flavones of phoenix extracts successively from the red seed of fresh phoenix and obtains red seed oil of phoenix and the red seed total flavones of phoenix, and its process step is:
A. pulverize and the red seed of dry phoenix: with disintegrating apparatus the red seed of the phoenix of cleaning is pulverized, made its granularity between the 40-100 order, adopting vacuum dryer is 10 ℃-55 ℃ in temperature, the red powder of seeds of drying under reduced pressure phoenix under the condition of vacuum tightness 20-80kPa;
B. the red seed crude oil of supersound extraction phoenix: adopt ultrasonic assisted extraction equipment; Selecting sherwood oil for use is to extract solvent, the red seed crude oil of ultrasonic assisted extraction phoenix from the red powder of seeds of the phoenix of drying under reduced pressure, and the condition of ultrasonic assisted extraction apparatus settings is: extraction time 30min-60min; Extract 40 ℃-60 ℃ of temperature; Ultrasonic power 200w-800w, the red powder of seeds ratio of sherwood oil and phoenix is 8:1 ~ 10:1mL/g, obtains containing the sherwood oil suspension liquid of the red powder of seeds of phoenix after the red seed crude oil of ultrasonic assisted extraction phoenix is accomplished;
C. separate the red powder of seeds of phoenix in the sherwood oil suspension liquid: after the red seed crude oil of ultrasonic assisted extraction phoenix is accomplished, adopt the straining installation clarification and filter the sherwood oil suspension liquid that contains the red powder of seeds of phoenix, obtain the red powder of seeds of petroleum ether solution and degreasing phoenix;
D. reduction vaporization petroleum ether solution: adopt vacuum dryer; The petroleum ether solution that reduction vaporization step c obtains, the processing parameter of reduction vaporization is: vacuum tightness 20-60kPa, temperature 15-40 ℃; And recovery sherwood oil; Be evaporated fully up to the sherwood oil composition, obtain the red seed crude oil of phoenix, be used for the red seed oil of refining finished product phoenix;
E. the red powder of seeds of drying defatted phoenix: adopting vacuum dryer, is 20-105kPa in vacuum tightness, and under temperature-10-40 ℃ the condition, residual water and sherwood oil on the red powder of seeds of evaporate to dryness degreasing phoenix obtain the red powder of seeds of exsiccant degreasing phoenix;
F. the red seed total flavones of supersound extraction phoenix: adopt ultrasonic assisted extraction equipment; Selecting ethanolic soln for use is to extract solvent; The red seed total flavones of supersound extraction phoenix from the red powder of seeds of exsiccant degreasing phoenix that step e obtains, the extraction conditions of ultrasonic assisted extraction equipment is: alcohol concn 50%-95%, extraction time 30min-60min; Extract 20 ℃-50 ℃ of temperature; Ultrasonic power 200w-300w, the red powder of seeds ratio of ethanolic soln and degreasing phoenix 10:1 ~ 30:1mL/g obtains containing the alcohol suspending liquid of the red powder of seeds of phoenix after the red seed total flavones of supersound extraction phoenix is accomplished;
G. the red powder of seeds of the phoenix in the separating alcohol suspension liquid: after the red seed total flavones of supersound extraction phoenix is accomplished, adopt the straining installation clarification also to filter the alcohol suspending liquid that contains the red powder of seeds of phoenix, obtain ethanolic soln and phoenix pellet seed residue;
H. reduction vaporization ethanolic soln: adopt vacuum dryer; The ethanolic soln that reduction vaporization step h obtains, the processing parameter of reduction vaporization is: vacuum tightness is 0-40kPa, temperature 30-60 ℃; And recovery ethanol; By evaporation fully, obtain the red seed total flavones of phoenix crude extract up to the ethanolic soln composition, be used for refining and produce the red seed total flavones of phoenix product.
Clean the red seed of phoenix as the further improvement to prior art: step a or with the aqueous solution that contains tensio-active agent;
Among the step b, the optimum extraction conditions of ultrasonic assisted extraction equipment is: extraction time 45min, extract 50 ℃ of temperature, and ultrasonic power 250w, the red powder of seeds ratio of sherwood oil and phoenix is 8:1mL/g.
Among the step f, the optimum extraction conditions of ultrasonic assisted extraction equipment is: alcohol concn 75%, extraction time 49min extracts 30 ℃ of temperature, ultrasonic power 240w, the red powder of seeds ratio of ethanolic soln and degreasing phoenix 21:1mL/g.
Step a or adopt freeze drying equipment red powder of seeds of lyophilize phoenix under the condition of temperature-40 ℃-0 ℃.
Among steps d, the step h, vacuum dryer or be vacuum concentration equipment or for reduction vaporization equipment.
Among the step b, extract solvent or be the mixed solvent of sherwood oil and normal hexane, the volume ratio of sherwood oil and normal hexane is 8:1 ~ 20:1.
In the straining installation of step c, step g, the aperture of its filtration medium is 0.01-10 μ m.
The operation room interval between step c, steps d, the step e is 0-2 hour.
Steps d reclaims sherwood oil and to step b, reuses, and step h reclaims ethanol and to step f, reuses.
The beneficial effect that the present invention is equivalent to prior art is:
One of which; Method of the present invention can be successively extracted from the red seed of fresh phoenix and is obtained red seed oil of phoenix and phoenix pellet seed total flavones, associating extraction method of the present invention with soxhlet extraction, ultrasonic-assisted extraction method, do not adopt ultrasonic auxiliary process for extracting to compare remarkable advantages.(seeing Figure of description 2, Fig. 3), wherein the oil yield of the red seed oil of phoenix is 33.7% among Fig. 2, the red seed oil of phoenix oil yield is higher; The extraction yield of the red seed total flavones of phoenix is 92.53% among Fig. 3, and it is less that the extraction yield of the red seed total flavones of phoenix receives the technogenic influence that extracts the red seed oil of phoenix, and extraction yield is higher.
The present invention unites the red seed oil of the phoenix purity height that extraction method obtains, and transparent color and luster only need be added the national standard that simple refinery practice can reach oil and fat product.The present invention extracts the red seed flavones of the phoenix that obtains and do not compare with the ultrasonic-assisted extraction method with adopting ultrasonic auxiliary process for extracting, and is active higher, and red seed total flavones resistance of oxidation of the phoenix that extracts and bacteriostasis be (seeing Fig. 4, Fig. 5) better.Wherein: Fig. 4 adopt to remove the resistance of oxidation that DPPH radical ability is measured the red seed total flavones of the phoenix solution that Different Extraction Method obtains; The average DPPH free radical scavenging activity of the red seed total flavones of the phoenix that the inventive method obtains solution is 84.47%, and is higher than the average clearance rate that does not adopt ultrasonic auxiliary process for extracting and ultrasonic-assisted extraction method; Fig. 5 adopts phosphorus molybdenum complex method that the total antioxidation property of the red seed total flavones of phoenix is measured, and the red seed total flavones of its phoenix total antioxidant activity is compared and do not adopted ultrasonic auxiliary process for extracting, ultrasonic-assisted extraction method height.
Its two, the mixed solvent that the present invention adopts sherwood oil or sherwood oil and normal hexane is as extracting solvent.Adopt the mixed solvent of sherwood oil or sherwood oil and normal hexane to extract; The oil yield of the red seed oil of phoenix is higher, and after uniting extraction, less to the influence of the red seed general flavone content of phoenix; The experimental result of embodiment 2 shows; After adopting sherwood oil or sherwood oil and normal hexane mixed solvent to extract the red seed oil of phoenix, the average loss rate of the total brass of the red seed of phoenix is 1.94%, extracts the red seed oil of phoenix much smaller than conventional solvent.It is thus clear that after adopting this method to extract the red seed oil of phoenix, the loss of the red seed total flavones of phoenix is less; And adopting the average DPPH free radical scavenging activity of the red seed total flavones of the phoenix solution of this solvent extraction is 84.47%, explains that the red seed total flavones of phoenix has very strong oxidation-resistance.
Its three, extraction process of the present invention is simple to operate, the equipment interoperability of employing is good, the equipment that can reach the processing parameter condition all can use, the less investment of production, whole process flow link up compact, are applicable to the biological food enterprise of various scales.Extraction cost of the present invention is lower; Extract solvent sherwood oil and ethanol and all can be recycled, improved extraction efficiency, unite and extracted red seed oil of phoenix and the red seed total flavones of phoenix; Making does not have the red seed resource of the phoenix of exploitation to be fully utilized originally, and the red Products Development of phoenix is had directive significance.
Description of drawings
Fig. 1: unite the overview flow chart that extracts red seed oil of phoenix and the red seed total flavones of phoenix method under the laboratory condition;
Fig. 2: the present invention compares the red seed oil of phoenix oil yield figure with other process for extracting;
Fig. 3: the present invention compares the red seed total flavones of phoenix extraction yield figure with other process for extracting;
Fig. 4: the present invention compares the red seed total flavones of phoenix DPPH free radical scavenging activity figure with other process for extracting;
Fig. 5: the present invention compares the red seed total flavones of phoenix TAC figure with other process for extracting.
Embodiment is done further to explain to embodiment of the present invention below in conjunction with accompanying drawing of the present invention and embodiment:
Fig. 1 is for uniting the overview flow chart that extracts red seed oil of phoenix and the red seed total flavones of phoenix method under the laboratory condition; Comprise following flow process, and combine embodiment 1 to specify:
Embodiment 1, unites the method for extracting red seed oil of phoenix and the red seed total flavones of phoenix under the laboratory condition
1. pluck the red seed of phoenix: choosing does not have disease and pest, and the red seed of phoenix that full grains are fresh is cleaned the earth on the red seed of phoenix, and is dry under the natural condition.
2. pulverize dry: the red seed of the phoenix of cleaning is put into medicinal herb grinder pulverize, cross 40 mesh sieves, adopt Vacuumdrier at 25 ℃, drying under reduced pressure obtains the red powder of seeds of phoenix under the condition of vacuum tightness 50kPa.
3. the red seed crude oil of ultrasonic assisted extraction phoenix: Erlenmeyer flask is put into ultrasonic washing instrument; Select the red seed crude oil of the ultrasonic assisted extraction phoenix of sherwood oil for use, extraction time is 45 min, and extracting temperature is 50 ℃; Ultrasonic power is 250 w, and the red powder of seeds ratio of sherwood oil and phoenix is 8:1 mL/g.
4. separating and filtering: extract accomplish after, with the mixed solution of the red powder of seeds of filter paper filtering phoenix with sherwood oil, filter paper lower floor obtains sherwood oil and filtrates, the filter paper upper strata obtains the phoenix pellet powder of seeds of degreasing.
5. drying under reduced pressure: adopting Rotary Evaporators is 50kPa in vacuum tightness, and under the condition that temperature is 40 ℃, rotary evaporation also reclaims sherwood oil, in sherwood oil filtrating, does not have the taste of sherwood oil, obtains the red seed crude oil of phoenix.
6. the red seed crude oil refining of phoenix: with the red seed heating crude oil to 50 of phoenix ℃, add massfraction and be in 5% the red seed crude oil of KOH solution to phoenix, and stir the red seed crude oil of phoenix, in the red seed crude oil of phoenix, the soap stock particle occurs, stop to stir.Under 70 ℃ condition, leave standstill 10h, this moment, the soap stock particle all was deposited in the solution bottom, isolated the soap stock particle that is deposited in the solution bottom, left and took the red seed oil reservoir of phoenix in the solution, through distilled water wash 1 time, obtained the red seed oil of finished product purified phoenix.
7. the red powder of seeds of drying defatted phoenix: adopting Rotary Evaporators is 50kPa in vacuum tightness, and under the condition that temperature is 40 ℃, the sherwood oil on the red powder of seeds of evaporate to dryness degreasing phoenix obtains the red powder of seeds of exsiccant degreasing phoenix.
8. the red seed total flavones of supersound extraction phoenix: select for use the ethanol assisting ultrasonic to extract the red seed total flavones of phoenix; Ethanolic soln concentration is: 75%, and extraction time is 49min, extracting temperature is 30 ℃; Ultrasonic power is 240w, and the red powder of seeds ratio of ethanolic soln and degreasing phoenix is 21:1mL/g.
9. filter: after extracting completion, with the mixed solution of red powder of seeds of filter paper filtering degreasing phoenix and ethanolic soln, filter paper lower floor obtains ethanol filtrating and the filter paper upper strata obtains the red seed residue of phoenix.
10. drying under reduced pressure: adopting Rotary Evaporators is 20kPa in vacuum tightness, under the condition that temperature is 40 ℃, and the rotary evaporation ethanolic soln, and reclaim ethanol, and in ethanol filtrating, there is not the alcoholic acid taste, obtain the crude extract of the red seed total flavones of phoenix.
11. ethyl acetate extraction: adopt the crude extract of the red seed total flavones of ethyl acetate extraction phoenix, obtain the ETHYLE ACETATE phase.
12. drying under reduced pressure: in vacuum tightness is 40kPa, and under the condition that temperature is 30 ℃, rotary evaporation also reclaims ETHYLE ACETATE, does not have the taste of ETHYLE ACETATE in mutually up to ETHYLE ACETATE, obtains the extract of the red seed total flavones of phoenix.
Fig. 2 is that the present invention compares the red seed oil of phoenix oil yield figure with other process for extracting; Fig. 3 is that the present invention compares the red seed total flavones of phoenix extraction yield figure with other process for extracting; Detect through Fig. 2, using the oil yield of the red seed oil of this method phoenix is 33.7%, and the additive method oil yield is higher relatively; Detect through Fig. 3, the extraction yield of the red seed total flavones of phoenix is 92.53%, has not compared remarkable advantages with adopting ultrasonic auxiliary process for extracting with the ultrasonic-assisted extraction method.
Fig. 4 is that the present invention compares the red seed total flavones of phoenix DPPH free radical scavenging activity figure with other process for extracting;
Fig. 4 adopts the red seed total flavones of DPPH free radical scavenging activity evaluation phoenix crude extract oxidation-resistance; The measuring method of DPPH free radical scavenging activity is: get the red seed total flavones of 2.0 mL phoenix extracting solution and shake up with the vibration of 4.0 mL 0.1mmol/L DPPH solution (95% ethanol is at present with join at present); Control samples is that 2.0 mL, 95% ethanol and 4.0 mL 0.1mM DPPH mix; In reacting at normal temperature without light after the identical time in 517 nm colorimetrics, do reference zeroing with 95% ethanol.Through measuring, the average clearance rate of DPPH radical of the red seed total flavones of the phoenix that the employing of 100mg/L process for extracting of the present invention obtains solution is 84.47%, and is higher than the average clearance rate that does not adopt ultrasonic auxiliary process for extracting and ultrasonic-assisted extraction method.
Fig. 5 is that the present invention compares the red seed total flavones of phoenix TAC figure with other process for extracting; Adopt phosphorus molybdenum complex method that the total antioxidation property of the red seed total flavones of phoenix is measured, its concrete steps are: at first preparing final concentration is 0.6M H
2SO
4, 28mM Na
3PO
4, 4mM Na
2Mo
4Sulfuric acid, sodium phosphate and Sodium orthomolybdate mix reagent solution; Get 0.4 mL, the red seed total flavones of 100mg/L phoenix solution adds 4.0 mL mix reagents again in 10 mL tool plug scale tube comparison tubess; Vibration evenly; Be incubated 90min under 95 ℃ of conditions, take out water-cooled 15min, under the wavelength of 695nm, survey absorbancy.And absorbance brought into the typical curve regression equation A=0.0206+0.02803C of xitix; Wherein, A is an absorbancy; C is an ascorbic acid concentrations, calculates total antioxidation property, and the total flavones that its total antioxidant activity does not adopt ultrasonic auxiliary process for extracting and ultrasonic-assisted extraction method to extract is higher.
In addition, the total flavones solution that obtains with the inventive method has certain restraining effect to Salmonellas, adopts the minimum inhibition zone method of half strength to measure, and obtaining the red seed total flavones of phoenix is 5% to the minimum inhibitory concentration of Salmonellas.
Embodiment 2, and the method for extracting red seed oil of phoenix and the red seed total flavones of phoenix is united in the laboratory
1. pluck the red seed of phoenix: choose the red seed of phoenix of full grains, clean the earth on the red seed of phoenix, dry under the natural condition.
2. pulverize dry: the red seed of the phoenix of cleaning is put into the herbal medicine pulverising mill pulverize, cross 100 mesh sieves, adopt freeze drier lyophilize under-20 ℃ of conditions to obtain the red powder of seeds of phoenix.
3. the red seed crude oil of ultrasonic assisted extraction phoenix: Erlenmeyer flask is put into ultrasonic washing instrument; Select sherwood oil for use: the red seed crude oil of the ultrasonic assisted extraction phoenix of the mixed solvent of normal hexane=10:1; Extraction time is 60 min; Extracting temperature is 40 ℃, and ultrasonic power is 800 w, and the red powder of seeds ratio of sherwood oil and phoenix is 10:1 mL/g.
4. separating and filtering: extract accomplish after, with the mixed solution of the red powder of seeds of filter paper filtering phoenix with sherwood oil, filter paper lower floor obtains sherwood oil and filtrates, the filter paper upper strata obtains the phoenix pellet powder of seeds of degreasing.
5. drying under reduced pressure: adopting Rotary Evaporators is 50kPa in vacuum tightness, and under the condition that temperature is 40 ℃, rotary evaporation also reclaims sherwood oil, is steamed fully up to sherwood oil, obtains the red seed crude oil of phoenix.
6. the red powder of seeds of drying defatted phoenix: adopting Rotary Evaporators is 50kPa in vacuum tightness, and under the condition that temperature is 40 ℃, the sherwood oil on the red powder of seeds of evaporate to dryness degreasing phoenix obtains the red powder of seeds of exsiccant degreasing phoenix.
7. the red seed total flavones of supersound extraction phoenix: select for use the ethanol assisting ultrasonic to extract the red seed total flavones of phoenix; Alcohol concn is: 95 %, and extraction time is 40min, extracting temperature is 30 ℃; Ultrasonic power is 300 w, and the red powder of seeds ratio of ethanolic soln and degreasing phoenix is 10:1mL/g.
8. filter: after extracting completion, with the mixed solution of red powder of seeds of filter paper filtering degreasing phoenix and ethanolic soln, filter paper lower floor obtains ethanolic soln and the filter paper upper strata obtains the red seed residue of phoenix.
9. drying under reduced pressure: in vacuum tightness is 40kPa, under the condition that temperature is 60 ℃, adopts Rotary Evaporators reduction vaporization ethanolic soln, and reclaims ethanol, is steamed fully up to ethanolic soln, obtains the crude extract of the red seed total flavones of phoenix.
Adopt the method for embodiment 2; The average extraction yield of the red seed total flavones of phoenix is 91.25%; And adopt the red seed of fresh phoenix directly to extract the total brass of the red seed of phoenix through step 7; The average extraction yield of the red seed total flavones of phoenix is 93.19%, and after employing sherwood oil or sherwood oil and normal hexane mixed solvent extracted the red seed oil of phoenix, the average loss rate of the total brass of the red seed of phoenix was 1.94%.
Embodiment 3, unite the method for extracting red seed oil of phoenix and the red seed total flavones of phoenix in the industrial production
1. pulverize dry: the helical feed hammer mill is pulverized the red seed of the phoenix of cleaning; The red powder of seeds of the phoenix that pulverizing is obtained can pass through 40 mesh sieves; And adopting freeze drier under 25 ℃, the condition of vacuum tightness 50kPa, the red powder of seeds of vacuum-drying phoenix obtains the red powder of seeds of exsiccant phoenix after the drying.
2. the red seed crude oil of ultrasonic assisted extraction phoenix, separate the red powder of seeds of phoenix in the sherwood oil suspension liquid: select the continuous countercurrent ultrasonic extractor for use, the extraction solvent is a sherwood oil; The red seed crude oil of continuous countercurrent supersound extraction phoenix; Wherein, the processing parameter that the continuous countercurrent ultrasonic extractor is set is: extraction time is 30 min, and extracting temperature is 50 ℃; Ultrasonic power is 200 w, and the red powder of seeds ratio of sherwood oil and phoenix is 8:1 mL/g; After extracting completion, the continuous countercurrent ultrasonic extractor will be accomplished the clarification and the filtration of extracting the back suspension liquid automatically, and liquid outlet obtains the mixing solutions of clarifying sherwood oil and the red seed oil of phoenix, and discharge port obtains the phoenix pellet powder of seeds of degreasing.
3. drying under reduced pressure sherwood oil; The red powder of seeds of drying defatted phoenix: adopting continuous slag charge solvent to steam and take off recovery and dryer, is 50kPa in vacuum tightness, under the condition that temperature is 20 ℃; Evaporate to dryness also reclaims the sherwood oil on the red powder of seeds of degreasing phoenix, obtains the red powder of seeds of exsiccant degreasing phoenix.
4. the red seed total flavones of supersound extraction phoenix, the red powder of seeds of the phoenix in the separating alcohol suspension liquid: with the red powder of seeds of exsiccant degreasing phoenix is raw material, adopts the continuous countercurrent ultrasonic extractor; Selecting ethanol for use is to extract solvent, the red seed total flavones of ultrasonic assisted extraction phoenix, wherein; The processing parameter that the continuous countercurrent ultrasonic extractor is set is: alcohol concn 75 %, and extraction times 49 min extracts 20 ℃ of temperature; Ultrasonic power 240 w, the red powder of seeds ratio of ethanolic soln and degreasing phoenix is 21:1mL/g; After extracting completion, the continuous countercurrent ultrasonic extractor will be accomplished the clarification and the filtration of extracting the back suspension liquid automatically, and liquid outlet obtains the clarifying ethanolic soln that contains the red seed total flavones of phoenix, and discharge port obtains the red powder of seeds of phoenix of degreasing.
5. steam and take off ethanolic soln: adopt continuous slag charge solvent to steam to take off and reclaim and dryer steams and takes off ethanolic soln, processing condition are: vacuum tightness 20kPa, under the condition that temperature is 40 ℃, evaporate to dryness also reclaims the ethanolic soln on the red seed residue of the phoenix powder.
6. the purifying of the red seed total flavones of phoenix: the crude extract that adopts extracter and ethyl acetate extraction phoenix pellet seed total flavones; Repeat 3 times; Adopt continuous slag charge solvent to steam and take off recovery and dryer recovery ETHYLE ACETATE, the processing condition of recovery are that vacuum tightness is 40kPa, 30 ℃ of temperature; Evaporate to dryness solution also reclaims ethanol, obtains the red seed extractive of general flavone of phoenix.
Claims (9)
1. the associating process for extracting of red seed oil of a phoenix and the red seed total flavones of phoenix is characterized in that this method is united to extract red seed oil of phoenix and phoenix pellet seed total flavones, and method steps is:
A. pulverize and the red seed of dry phoenix: with disintegrating apparatus the red seed of the phoenix of cleaning is pulverized, made its granularity between the 40-100 order, adopting vacuum dryer is 10 ℃-55 ℃ in temperature, the red powder of seeds of drying under reduced pressure phoenix under the condition of vacuum tightness 20-80kPa;
B. the red seed crude oil of ultrasonic assisted extraction phoenix: adopt ultrasonic assisted extraction equipment; Selecting sherwood oil for use is to extract solvent; The red seed crude oil of ultrasonic assisted extraction phoenix from the red powder of seeds of the phoenix of drying under reduced pressure; The condition of ultrasonic assisted extraction apparatus settings is: extraction time 30min-60min, extract 40 ℃-60 ℃ of temperature, ultrasonic power 200w-800w; The red powder of seeds ratio of sherwood oil and phoenix is 8:1 ~ 10:1mL/g, obtains containing the sherwood oil suspension liquid of the red powder of seeds of phoenix after the red seed crude oil of ultrasonic assisted extraction phoenix is accomplished;
C. separate the red powder of seeds of phoenix in the sherwood oil suspension liquid: after the red seed crude oil of ultrasonic assisted extraction phoenix is accomplished, adopt the straining installation clarification and filter the sherwood oil suspension liquid that contains the red powder of seeds of phoenix, obtain the red powder of seeds of petroleum ether solution and degreasing phoenix;
D. reduction vaporization petroleum ether solution: adopt vacuum dryer; The petroleum ether solution that reduction vaporization step c obtains, the processing parameter of reduction vaporization is: vacuum tightness 20-60kPa, temperature 15-40 ℃; And recovery sherwood oil; Be evaporated fully up to the sherwood oil composition, obtain the red seed crude oil of phoenix, be used for the red seed oil of refining finished product phoenix;
E. the red powder of seeds of drying defatted phoenix: adopting vacuum dryer, is 20-105kPa in vacuum tightness, and under temperature-10-40 ℃ the condition, residual water and sherwood oil on the red powder of seeds of evaporate to dryness degreasing phoenix obtain the red powder of seeds of exsiccant degreasing phoenix;
F. the red seed total flavones of ultrasonic assisted extraction phoenix: adopt ultrasonic assisted extraction equipment; Selecting ethanolic soln for use is to extract solvent; The red seed total flavones of ultrasonic assisted extraction phoenix from the red powder of seeds of exsiccant degreasing phoenix that step e obtains, the extraction conditions of ultrasonic assisted extraction equipment is: alcohol concn 50%-95%, extraction time 30min-60min; Extract 30 ℃-50 ℃ of temperature; Ultrasonic power 200w-300w, the red powder of seeds ratio of ethanolic soln and degreasing phoenix 10:1 ~ 30:1mL/g obtains containing the alcohol suspending liquid of the red powder of seeds of phoenix after the red seed total flavones of ultrasonic assisted extraction phoenix is accomplished;
G. the red powder of seeds of the phoenix in the separating alcohol suspension liquid: after the red seed total flavones of ultrasonic assisted extraction phoenix is accomplished, adopt the straining installation clarification also to filter the alcohol suspending liquid that contains the red powder of seeds of phoenix, obtain ethanolic soln and phoenix pellet seed residue powder;
H. reduction vaporization ethanolic soln: adopt vacuum dryer; The ethanolic soln that reduction vaporization step h obtains, the processing parameter of reduction vaporization is: vacuum tightness is 0-40kPa, temperature 30-60 ℃; And recovery ethanol; By evaporation fully, obtain the red seed total flavones of phoenix crude extract up to the ethanolic soln composition, be used for refining and produce the red seed total flavones of phoenix product.
2. according to the associating process for extracting of red seed oil of the said a kind of phoenix of claim 1 and phoenix pellet seed total flavones; It is characterized in that; Among the step b, the optimum extraction conditions of ultrasonic assisted extraction equipment is: extraction time 45min, extract 50 ℃ of temperature; Ultrasonic power 250w, the red powder of seeds ratio of sherwood oil and phoenix is 8:1mL/g.
3. according to the associating process for extracting of red seed oil of the said a kind of phoenix of claim 1 and phoenix pellet seed total flavones; It is characterized in that among the step f, the optimum extraction conditions of ultrasonic assisted extraction equipment is: alcohol concn 75%; Extraction time 49min; Extract 30 ℃ of temperature, ultrasonic power 240w, the red powder of seeds ratio of ethanolic soln and degreasing phoenix 21:1mL/g.
4. according to the associating process for extracting of red seed oil of the said a kind of phoenix of claim 1 and the red seed total flavones of phoenix, it is characterized in that, wherein, step a or adopt freeze drying equipment lyophilize phoenix pellet powder of seeds under the condition of temperature-40 ℃-0 ℃.
5. according to the associating process for extracting of red seed oil of the said a kind of phoenix of claim 1 and the red seed total flavones of phoenix, it is characterized in that, wherein, among steps d, the step h, vacuum dryer or be vacuum concentration equipment or be reduction vaporization equipment.
6. according to the associating process for extracting of red seed oil of the said a kind of phoenix of claim 1 and the red seed total flavones of phoenix, it is characterized in that, wherein, among the step b, extraction solvent or be the mixed solvent of sherwood oil and normal hexane, the volume ratio of sherwood oil and normal hexane is 8:1 ~ 20:1.
7. according to the associating process for extracting of red seed oil of each said a kind of phoenix and the red seed total flavones of phoenix in the claim 1 ~ 6, it is characterized in that: wherein, in the straining installation of step c, step g, the aperture of its filtration medium is 0.01-10 μ m.
8. according to the associating process for extracting of red seed oil of each said a kind of phoenix and the red seed total flavones of phoenix in the claim 1 ~ 6, it is characterized in that: wherein, the operation room interval between step c, steps d, the step e is 0-2 hour.
9. according to the associating process for extracting of red seed oil of each said a kind of phoenix and the red seed total flavones of phoenix in the claim 1 ~ 6, it is characterized in that: wherein, steps d reclaims sherwood oil and to step b, reuses, and step h reclaims ethanol and to step f, reuses.
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