CN109966327A - A kind of method of the double assisted extraction passionflower seed oil meal general flavones of ultrasonic wave, microwave - Google Patents
A kind of method of the double assisted extraction passionflower seed oil meal general flavones of ultrasonic wave, microwave Download PDFInfo
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Abstract
The invention discloses a kind of methods using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave.This method comprises the following steps: passionflower seed is dry to constant weight in 55~70 DEG C, it crushes, sieving, obtain kind of a powder of seeds, petroleum ether, mass volume ratio 6:42~58 of control kind powder of seeds and petroleum ether, 85~95 DEG C of 70~85min of condensing reflux progress degreasings are added, it is concentrated by evaporation recycling petroleum ether, the seed oil meal after collecting degreasing；Ethanol-water solution is added, ultrasonic wave extraction is carried out under the conditions of 75~85 DEG C of waters bath with thermostatic control, obtains mixed liquor, carries out Microwave Extraction, filtering obtains general flavone extracting solution.The effect of vibration and cavitation effect of integrated utilization ultrasonic wave extraction of the present invention, the broken wall and heat effect of microwave extraction technology, greatly increase extraction efficiency, while having extraction process easy, the free of contamination advantage of Extraction solvent can maximize passionflower utility value.
Description
Technical field
The invention belongs to natural plant Component Extraction fields.In particular it relates to a kind of double auxiliary using ultrasonic wave, microwave
Help the method for extracting passionflower seed oil meal general flavone.
Background technique
Violet passion fruit (Passiflora edulis Sims) is Passifloraceae Passiflora liana, in China's cloud
The provinces such as south, Guangdong, Guangxi large-scale plantation, fruit juice fragrance is pleasant, and unique flavor occupies importantly on beverage market
Position.Passionfruit generates the seed for accounting for whole fruit quality 11% or so, seed oil content is about 20%, at present after extracting fruit juice
The exploitation of seed oil is focused primarily upon to the research that passionflower seed utilizes both at home and abroad.The research table of violet passion fruit seed effective component
It is bright, contain the effective components such as protein, unsaturated fatty acid, flavones.Flavone compound has antibacterial, anti-oxidant freedom
The pharmacological activity such as base, anticancer have very big booster action to human disease treatment.Containing a large amount of yellow in passionflower seed oil meal
Ketone, however for extracting by-product-oil meal for generating after seed oil, research and using being rarely reported, therefore select a kind of extractions effect
Rate is high, and the few extraction process of loss of effective components is one of key technology of the invention.
Chinese patent literature CN104606262A discloses a kind of method for extracting general flavone from passion flower-fruit peel, by pericarp
Powder carries out ultrasonic wave assisted extraction after alcohol solution dipping is added, and the filtrate filtered obtains crude flavonoid powder particle through evaporation,
Distilled water is added to dissolve crude flavonoid powder particle, sends out to obtain flavones particle by filtration.Its ultrasonic time is longer, and flavonoids
Compound, which is insoluble in water, makes dissolution not exclusively cause extracting flavonoids content lower.Chinese patent literature CN102225080A is disclosed
A kind of method of extracting flavonoid compounds from passion fruit leaves by ethanol-microwave soaking leaching process is added in passion fruit cured leaf powder
Microwave Extraction is carried out after ethanol solution heating extraction 0.5h, continues water bath with thermostatic control extraction later, through filtering after extraction,
Vacuum concentration obtains concentrate.The ratio of its solid-liquid ratio is excessive, keeps the concentration difference of raw material and the alternate flavones of solvent two too small, mass transfer
Motive force is too low, is unfavorable for flavones dissolution, causes extracting flavonoids content lower.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the defect of the above-mentioned prior art and deficiencies, provide a kind of using ultrasound
The method of the double assisted extraction passionflower seed oil meal general flavones of wave, microwave.This method is extracted using passionflower seed oil meal as raw material
Natural activity flavonoid substance therein extends passionflower processing industry chain.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
A method of using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave, include the following steps:
S1. passionflower seed is dry to constant weight in 55~70 DEG C, the sieve that aperture is 0.250~0.425mm is crossed in crushing,
Obtain kind of a powder of seeds；
S2. it takes described kind of powder of seeds and petroleum ether is added, the mass volume ratio 6:42 of control kind of powder of seeds and petroleum ether~
58,85~95 DEG C of 70~85min of condensing reflux carry out degreasing, are concentrated by evaporation recycling petroleum ether, the seed oil meal after collecting degreasing；
S3. ethanol-water solution is added into the above-mentioned seed oil dregs of rice, ultrasonic wave is carried out under the conditions of 75~85 DEG C of waters bath with thermostatic control
It extracts, obtains mixed liquor；
S4. above-mentioned mixed liquor is subjected to Microwave Extraction, filtering obtains general flavone extracting solution.
The effect of vibration and cavitation effect of integrated utilization ultrasonic wave extraction of the present invention, the broken wall of microwave extraction technology and
Heat effect greatly increases extraction efficiency, while having extraction process simplicity, the free of contamination advantage of Extraction solvent.The present invention
It is 35.57~122.61mg/g that obtained general flavone, which extracts content,.
Further, in preferred embodiments of the present invention, in step S3, the useful load of the seed oil meal is 1.0~
2.0g。
Further, in preferred embodiments of the present invention, in step S3, the useful load of the seed oil meal is
1.0g。
Further, in preferred embodiments of the present invention, in step S3, the volume of ethyl alcohol in the ethanol-water solution
Score is 50%~90%.
Further, in preferred embodiments of the present invention, in step S3, the body of ethyl alcohol in the ethanol-water solution
Fraction is 80%.
Further, in preferred embodiments of the present invention, in step S3, the material of the seed oil meal, ethanol-water solution
Liquor ratio is 1:20~1:60g/mL.
Further, in preferred embodiments of the present invention, in step S3, the seed oil meal, ethanol-water solution
Solid-liquid ratio is 1:50g/mL.
Further, in preferred embodiments of the present invention, in step S3, ultrasonic time is 10~60min；Ultrasonic power
For 200~500w.
Further, in preferred embodiments of the present invention, in step S3, ultrasonic time 50min, ultrasonic power is
300w。
Further, in preferred embodiments of the present invention, in step S3, ultrasonic wave extraction number is 2~3 times.
Further, in preferred embodiments of the present invention, in step S4, microwave power is 160~480w；The microwave time
For 30~150s.
Further, in preferred embodiments of the present invention, in step S4, microwave power 320w, the microwave time is
90s。
Further, described to be filtered into miillpore filter or decompression pumping in step S4 in preferred embodiments of the present invention
Filter, the vacuum degree that the decompression filters are -0.08~-0.1MPa；It obtains being washed with distilled water seed after filtering decompression crude extract
Oil meal residue 2~3 times, merging filtrate.
Further, in preferred embodiments of the present invention, in step S4, it is described decompression filter vacuum degree be-
0.09~-0.1MPa.
Further, in preferred embodiments of the present invention, in step S1, the drying temperature of passionflower seed is 60~65
℃。
Further, in preferred embodiments of the present invention, in step S1, smash it through 0.300~0.355mm's of aperture
Sieve.
Further, in preferred embodiments of the present invention, in step S2, the mass body of control kind powder of seeds and petroleum ether
Product is than 6:50~55.
Further, in preferred embodiments of the present invention, seed oil meal, ethanol-water solution solid-liquid ratio be 1:
56.02g/mL, the volume fraction of ethyl alcohol is 73.78% in ethanol-water solution, ultrasonic time 50min, and ultrasonic power is
300w, microwave power 160w, microwave time are 90s.
Further, in preferred embodiments of the present invention, the method also includes the general flavones obtained to step S4 to mention
Liquid is taken to be purified, the purification step are as follows: the general flavone extracting solution that step S4 is obtained is concentrated into no ethanol flavor, medicinal extract is cold
Being lyophilized dry is powder, is isolated and purified using AB-8 macroreticular resin wet method dress post, process conditions are as follows: sample solution general flavone is dense
Degree is 1.0~2.0mg/mL, and adjusting load solution pH is 3~3.5, with 7~9r/min flow velocity loading, with resin weight in wet base: loading
Amount is that the ratio of 25mg:110~120mL prepares the adsorption liquid of resin and general flavone；With 90~100mL distilled water after end of the sample
Washed with impurities are carried out, are eluted later with 70%~75% ethanol solution of 90~100mL, elution flow rate is 10~12r/
min。
In the present invention, the general flavone rate of recovery is 86~90%, and general flavone purity after purification reaches 72~85%.
Further, in preferred embodiments of the present invention, with resin weight in wet base: applied sample amount is 25mg:115~120mL's
The adsorption liquid of ratio preparation resin and general flavone.
Further, in preferred embodiments of the present invention, the freeze-drying is vacuum freeze drying.The freezing is dry
It is dry for by medicinal extract at -80~-60 DEG C vacuum freeze drying 12~for 24 hours.
Compared with prior art, the invention has the following advantages:
(1) flavones is extracted from passionflower seed oil meal, realizes its medical value, it can be maximum by passionflower utility value
Change.
(2) effect of vibration and cavitation effect of integrated utilization ultrasonic wave extraction of the present invention, microwave extraction technology are broken
Wall and heat effect, greatly increase extraction efficiency, while having extraction process simplicity, the free of contamination advantage of Extraction solvent.
(3) it is 35.57~122.61mg/g that the obtained general flavone of the present invention, which extracts content, the general flavone rate of recovery is 86~
90%, general flavone purity after purification reaches 72~85%, and extracting flavonoids content is higher.
Detailed description of the invention
Fig. 1 is influence of the solid-liquid ratio of step S3 oil meal powder, ethanol-water solution to extracting flavonoids content.
Fig. 2 is influence of the volume fraction of ethanol to extracting flavonoids content in step S3 ethanol-water solution.
Fig. 3 is influence of the step S3 ultrasonic time to extracting flavonoids content.
Fig. 4 is influence of the step S3 ultrasonic power to extracting flavonoids content.
Fig. 5 is influence of the step S4 microwave power to extracting flavonoids content.
Fig. 6 is influence of the step S4 microwave time to extracting flavonoids content.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
Unless stated otherwise, following embodiment agents useful for same and material are commercially available.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 1
(1) it crushes: by passionflower seed in 55 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.250mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 42mL, 95 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and volume fraction of ethanol is added by solid-liquid ratio 1:20g/mL and is
50% ethanol-water solution is arranged ultrasonic power 200w, extracts 60min under the conditions of 80 DEG C of waters bath with thermostatic control, obtain mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 160w extracts 150s, is adopted
With general flavone extracting solution is obtained after filtering with microporous membrane, it is 57.49mg/g that general flavone, which extracts content,.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 2
(1) it crushes: by passionflower seed in 70 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.425mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 58mL, 85 DEG C of condensations are added in quartz curette
The 85min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and volume fraction of ethanol is added by solid-liquid ratio 1:60g/mL and is
90% ethanol solution is arranged ultrasonic power 500w, extracts 10min under the conditions of 80 DEG C of waters bath with thermostatic control, obtain mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 480w extracts 30s, is used
General flavone extracting solution is obtained after filtering with microporous membrane, it is 84.90mg/g that general flavone, which extracts content,.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 3
(1) it crushes: passionflower seed is dry to constant weight in 60 DEG C, with pulverizer by the passionflower seed oil meal of drying
It is broken, 0.300mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 50mL, 85 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and volume fraction of ethanol is added by solid-liquid ratio 1:50g/mL and is
80% ethanol solution is arranged ultrasonic power 300w, 30min, ultrasonic wave extraction number is extracted under the conditions of 80 DEG C of waters bath with thermostatic control
It is 2 times, obtains mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 320w extracts 90s, is used
Filtering with microporous membrane obtains general flavone extracting solution, and it is 110.34mg/g that general flavone, which extracts content,.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 4
(1) it crushes: by passionflower seed in 65 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.355mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 55mL, 85 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and ethyl alcohol volume point is added by solid-liquid ratio 1:56.02g/mL
The ethanol solution that number is 73.78% is arranged ultrasonic power 300w, extracts 50min under the conditions of 80 DEG C of waters bath with thermostatic control, ultrasonic wave mentions
Taking number is 3 times, obtains mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 160w extracts 90s, is used
General flavone extracting solution is obtained after filtering with microporous membrane, it is 117.53mg/g that general flavone, which extracts content,.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 5
Passionflower seed oil meal general flavone is extracted according to the method for embodiment 4, wherein first three step and 4 phase of embodiment
Together, first three is walked gained mixed liquor and is placed in microwave treater by (4) step, and setting microwave power 160w extracts 90s, vacuum degree-
Decompression suction filtration is carried out under the conditions of 0.09~-0.1MPa, obtains being washed with distilled water seed oil meal residue 2 after filtering decompression crude extract
~3 times, merging filtrate obtains general flavone extracting solution, and it is 120.36mg/g that general flavone, which extracts content,.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 6
(1) it crushes: by passionflower seed in 60 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.425mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 50mL, 85 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and ethyl alcohol volume point is added by solid-liquid ratio 1:56.02g/mL
The ethanol solution that number is 73.78% is arranged ultrasonic power 300w, extracts 50min under the conditions of 80 DEG C of waters bath with thermostatic control, ultrasonic wave mentions
It takes number 3 times, obtains mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 160w extracts 90s, vacuum
Decompression suction filtration is carried out under the conditions of -0.08~-0.09MPa of degree, obtains being washed with distilled water seed oil meal after filtering decompression crude extract
Residue 2~3 times, merging filtrate obtains general flavone extracting solution, and it is 120.89mg/g that general flavone, which extracts content,；
(5) it purifies: the general flavone extracting solution that step S4 is obtained being concentrated into no ethanol flavor, by medicinal extract at -80~-60 DEG C
Vacuum freeze drying 12~it is for 24 hours powder；Using AB-8 macroreticular resin wet method dress post, preparing sample solution general flavone concentration is
1.0mg/mL, adjusting load solution pH is 3, with 9r/min flow velocity loading, with resin weight in wet base: applied sample amount is the ratio of 25mg:100mL
Example prepares the adsorption liquid of resin and general flavone；Washed with impurities are carried out with 90mL distilled water after end of the sample, use 90mL 70% later
Ethanol solution is eluted, elution flow rate 10r/min.The general flavone rate of recovery is 88.12%, and general flavone purity after purification is
70.14%.
A kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave of embodiment 7
(1) it crushes: by passionflower seed in 60 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.425mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 55mL, 85 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and ethyl alcohol volume point is added by solid-liquid ratio 1:56.02g/mL
The ethanol solution that number is 73.78% is arranged ultrasonic power 300w, extracts 50min under the conditions of 80 DEG C of waters bath with thermostatic control, ultrasonic wave mentions
It takes number 3 times, obtains mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 160w extracts 90s, vacuum
Decompression suction filtration is carried out under the conditions of -0.09~-0.10MPa of degree, obtains being washed with distilled water seed oil meal after filtering decompression crude extract
Residue 2~3 times, merging filtrate obtains general flavone extracting solution, and it is 122.61mg/g that general flavone, which extracts content,；
(5) it purifies: the general flavone extracting solution that step S4 is obtained being concentrated into no ethanol flavor, medicinal extract is freeze-dried as powder
End；AB-8 macroreticular resin wet method dress post, preparation sample solution general flavone concentration are 2.0mg/mL, and adjusting load solution pH is 3.5, with
7r/min flow velocity loading, with resin weight in wet base: applied sample amount is that the ratio of 25mg:120mL prepares the adsorption liquid of resin and general flavone；On
Washed with impurities are carried out with 100mL distilled water after sample, are eluted later with 70% ethanol solution of 100mL, elution flow rate is
12r/min.The general flavone rate of recovery is 90.32%, and general flavone purity after purification is 75.47%.
Comparative example 1
(1) it crushes: by passionflower seed in 60 DEG C of dryings to constant weight, being crushed the passionflower seed of drying with pulverizer,
0.425mm sieve is crossed, kind of a powder of seeds is obtained；
(2) degreasing: weighing 6.0g kind powder of seeds and be put into filtration paper cylinder, and petroleum ether 50mL, 85 DEG C of condensations are added in quartz curette
The 70min that flows back carries out degreasing, and rotary evaporation recycles petroleum ether, the seed oil meal after collecting degreasing；
(3) ultrasonic wave extraction: weighing above-mentioned seed oil meal 1.0g, and ethyl alcohol volume point is added by solid-liquid ratio 1:56.02g/mL
The ethanol solution that number is 73.78% is arranged ultrasonic power 300w, extracts 50min under the conditions of 80 DEG C of waters bath with thermostatic control, ultrasonic wave mentions
It takes number 3 times, obtains mixed liquor；
(4) Microwave Extraction: above-mentioned mixed liquor is placed in microwave treater, and setting microwave power 160w extracts 90s, vacuum
Decompression suction filtration is carried out under the conditions of -0.08~-0.09MPa of degree, obtains being washed with distilled water seed oil meal after filtering decompression crude extract
Residue 2~3 times, merging filtrate obtains general flavone extracting solution, and it is 121.63mg/g that general flavone, which extracts content,.
(5) it purifies: the general flavone extracting solution that step S4 is obtained being concentrated into no ethanol flavor, medicinal extract is freeze-dried as powder
End；Using AB-8 macroreticular resin wet method dress post, preparation sample solution general flavone concentration is 1.0mg/mL, and adjusting load solution pH is 6,
With 9r/min flow velocity loading, with resin weight in wet base: applied sample amount is that the ratio of 25mg:110mL prepares the adsorption liquid of resin and general flavone；
Washed with impurities are carried out with 90mL distilled water after end of the sample, are eluted later with 70% ethanol solution of 90mL, elution flow rate is
8r/min.The general flavone rate of recovery is 74.61%, and general flavone purity after purification is 66.19%.
8 optimal extraction technology of embodiment
1, experiment of single factor
(1) method
According to the method for embodiment 1 extract passionflower seed oil meal general flavone, choose volume fraction of ethanol be 50~90%,
Solid-liquid ratio is 1:20~60g/mL, ultrasonic time is 10~60min, 200~500w of ultrasonic power, 160~480w of microwave power,
30~150s of microwave power investigates influence of each factor to extracting flavonoids content, 3 weights of each test process as influence factor
It is multiple.
(2) result
1) influence of solid-liquid ratio 1: 20,1: 30,1: 40,1: 50,1: 60 (g/mL) to extracting flavonoids content is investigated, as a result such as
Shown in Fig. 1, in solid-liquid ratio 1: 20~50 (g/mL) range, as the ratio of solid-liquid ratio declines, extracting flavonoids content obviously increases
Add, extracting flavonoids content is preferable when solid-liquid ratio 1: 50 (g/mL).
2) volume fraction of ethanol 50%, 60%, 70%, 80%, 90% influence pair extracting flavonoids content are investigated, as a result such as
Shown in Fig. 2, in for examination range, downward trend after extracting flavonoids content first increases with volume fraction of ethanol increase presentation is mentioned
Rate is taken to reach peak value when volume fraction of ethanol is 80%；When volume fraction of ethanol is more than 80%, extracting flavonoids content is instead
Decline.
3) investigate ultrasonic time 10,20,30,40,50, influence of the 60min to extracting flavonoids content, as a result as shown in figure 3,
Extracting flavonoids content increases with the extension of ultrasonic time, and when ultrasonic time is greater than 30min, recovery rate increase is slow, because
For effective component, most of dissolution after being ultrasonically treated 30min, continues to extend the time, and on being promoted, the influence of extracting flavonoids content is micro-
It is weak.Therefore selection ultrasonic time 30min is advisable.
4) ultrasonic power 200,250,300,350,400,450, influence of the 500w to extracting flavonoids content, such as Fig. 4 are investigated
Shown, ultrasonic power is within the scope of 200~300w, and as ultrasonic power increases, extracting flavonoids content is gradually risen, when ultrasonic function
When rate is 300w, extracted amount reaches peak value, increases ultrasonic power, the decline of extracting flavonoids content later.
5) investigate microwave power 160,240,320,400, influence of the 480w to extracting flavonoids content, as a result as shown in figure 5,
With the increase of microwave power, extracting flavonoids content is in first to increase the trend reduced afterwards, when microwave power is 160W, recovery rate
Reach maximum.
6) investigate microwave time 30,60,90,120, influence of the 150s to extracting flavonoids content, as a result as shown in fig. 6, with
The extension of microwave time, flavonoids extract content be gradually increased, when the microwave time be 90s when reach maximum value, further prolong
Long microwave time, extracted amount decline instead.
2, response surface composite test
(1) method
Using extracting flavonoids content as response, from above-mentioned single factor experiment, choosing influences more extracting flavonoids content
Significant volume fraction of ethanol (A), solid-liquid ratio (B), ultrasonic time (C), microwave power (D) are independent variable, establish four factors three
The design of horizontal centre combination experiment.
Response surface experimental program and it the results are shown in Table 1 and table 2.
1 response surface experiments independent variable factor level table of table
2 response surface design scheme of table and experimental result
Optimised process is obtained by the analysis of 8.0 software of Design Expert, and wherein solid-liquid ratio is 1:56.02g/mL, second
Alcohol volume fraction is 73.78%, ultrasonic time 50min, microwave power 160w.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of method using ultrasonic wave, the double assisted extraction passionflower seed oil meal general flavones of microwave, which is characterized in that including
Following steps:
S1. passionflower seed is dry to constant weight in 55~70 DEG C, it crushes, crosses the sieve that aperture is 0.250~0.425mm, obtain
Kind powder of seeds；
S2. it takes described kind of powder of seeds and petroleum ether is added, mass volume ratio 6:42~58 of control kind of powder of seeds and petroleum ether, 85
~95 DEG C of 70~85min of condensing reflux carry out degreasing, are concentrated by evaporation recycling petroleum ether, the seed oil meal after collecting degreasing；
S3. ethanol-water solution is added into the above-mentioned seed oil dregs of rice, ultrasonic wave is carried out under the conditions of 75~85 DEG C of waters bath with thermostatic control and is mentioned
It takes, obtains mixed liquor；
S4. above-mentioned mixed liquor is subjected to Microwave Extraction, filtering obtains general flavone extracting solution.
2. the method according to claim 1, wherein in step S3, the volume of ethyl alcohol in the ethanol-water solution
Score is 50%~90%；The seed oil meal, ethanol-water solution solid-liquid ratio be 1:20~1:60g/mL；Ultrasonic time is
10~60min；Ultrasonic power is 200~500w.
3. the method according to claim 1, wherein ultrasonic wave extraction number is 2~3 times in step S3.
4. the method according to claim 1, wherein microwave power is 160~480w in step S4；When microwave
Between be 30~150s.
It is described to be filtered into miillpore filter or decompression is taken out 5. the method according to claim 1, wherein in step S4
Filter, the vacuum degree that the decompression filters are -0.08~-0.1MPa；It obtains being washed with distilled water seed after filtering decompression crude extract
Oil meal residue 2~3 times, merging filtrate.
6. the method according to claim 1, wherein the drying is vacuum drying, the drying in step S1
Temperature is 60~65 DEG C.
7. according to the method described in claim 6, it is characterized in that, smashing it through 0.300~0.355mm of aperture in step S1
Sieve.
8. the method according to claim 1, wherein controlling the quality of kind of powder of seeds and petroleum ether in step S2
Volume ratio 6:50~55.
9. any method according to claim 1~8, which is characterized in that further include being mentioned to the obtained general flavone of step S4
Liquid is taken to be purified, the purification step are as follows: the general flavone extracting solution that step S4 is obtained is concentrated into no ethanol flavor, medicinal extract is cold
Being lyophilized dry is powder, is isolated and purified using AB-8 macroreticular resin wet method dress post, process conditions are as follows: sample solution general flavone is dense
Degree is 1.0~2.0mg/mL, and adjusting load solution pH is 3~3.5, with 7~9r/min flow velocity loading, with resin weight in wet base: loading
Amount is that the ratio of 25mg:100~120mL prepares the adsorption liquid of resin and general flavone；With 90~100mL distilled water after end of the sample
Washed with impurities are carried out, are eluted later with 70%~75% ethanol solution of 90~100mL, elution flow rate is 10~12r/
min。
10. according to the method described in claim 9, it is characterized in that, with resin weight in wet base: applied sample amount is the matter of 25:115~120
Measure the adsorption liquid than preparing general flavone and resin.
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| CN114894930A (en) * | 2022-04-28 | 2022-08-12 | 浙江师范大学 | Method for detecting content of alkylphenol ethoxylates in textile by high performance liquid chromatography |
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| CN110951277A (en) * | 2019-12-10 | 2020-04-03 | 苏州经贸职业技术学院 | Preparation method of environment-friendly functional coloring agent |
| CN112957344A (en) * | 2021-02-25 | 2021-06-15 | 广西大学 | Nanometer preparation containing passionflower flavone and its preparation method |
| CN112957344B (en) * | 2021-02-25 | 2022-08-26 | 广西大学 | Nanometer preparation containing passionflower flavone and its preparation method |
| CN114894930A (en) * | 2022-04-28 | 2022-08-12 | 浙江师范大学 | Method for detecting content of alkylphenol ethoxylates in textile by high performance liquid chromatography |
| CN114894930B (en) * | 2022-04-28 | 2023-10-20 | 浙江师范大学 | Method for detecting alkylphenol ethoxylate content in textile by high performance liquid chromatography |
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