CN109966327B - Method for extracting passion flower seed oil meal total flavonoids by ultrasonic and microwave double-auxiliary extraction - Google Patents
Method for extracting passion flower seed oil meal total flavonoids by ultrasonic and microwave double-auxiliary extraction Download PDFInfo
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Abstract
The invention discloses a method for extracting passion flower seed oil meal total flavonoids by adopting ultrasonic and microwave double-auxiliary. The method comprises the following steps: drying passion flower seeds at 55-70 ℃ to constant weight, crushing, sieving to obtain seed powder, adding petroleum ether, and controlling the mass-volume ratio of the seed powder to the petroleum ether to be 6: condensing and refluxing for 70-85 min at the temperature of 42-58 ℃ for degreasing, evaporating and concentrating to recover petroleum ether, and collecting degreased seed oil meal; adding an ethanol-water solution, performing ultrasonic extraction under the condition of a constant-temperature water bath at 75-85 ℃ to obtain a mixed solution, performing microwave extraction, and filtering to obtain a total flavone extracting solution. The invention integrates and utilizes the vibration effect and the cavitation effect of the ultrasonic extraction technology and the wall breaking and heating effect of the microwave extraction technology, greatly increases the extraction efficiency, has the advantages of simple and convenient extraction process and no pollution of an extraction solvent, and can maximize the utilization value of passion flower.
Description
Technical Field
The invention belongs to the technical field of plant natural component extraction. In particular to a method for extracting passion flower seed oil meal total flavonoids by adopting ultrasonic and microwave double-auxiliary.
Background
The passion fruit passion flower (Passiflora edulis Sims) is a liana vine of the passion genus of the Passifloraceae family, is planted in provinces such as Yunnan, Guangdong, Guangxi and the like in China in a large scale, has pleasant juice fragrance and unique flavor, and plays an important role in the beverage market. After the passion fruit is extracted with juice, seeds which account for about 11 percent of the whole fruit are generated, the oil content of the seeds is about 20 percent, and the research on the utilization of the passion fruit seeds at home and abroad mainly focuses on the development of seed oil at present. Research on the active ingredients of passion fruit seeds shows that the passion fruit seeds contain active ingredients such as protein, unsaturated fatty acid, flavone and the like. The flavonoid compounds have pharmacological activities of resisting bacteria, resisting oxidation free radicals, resisting cancer and the like, and have great auxiliary effects on the treatment of human diseases. The passion flower seed oil meal contains a large amount of flavone, but the research and the utilization of the byproduct oil meal generated after the seed oil is extracted are reported, so that the extraction process with high extraction efficiency and less loss of effective components is selected and is one of the key technologies of the invention.
Chinese patent document CN104606262A discloses a method for extracting total flavonoids from passion fruit peel, which comprises the steps of adding peel powder into ethanol solution for soaking, then carrying out ultrasonic-assisted extraction, carrying out suction filtration to obtain filtrate, evaporating to obtain crude flavone particles, adding distilled water to dissolve the crude flavone particles, and carrying out filtration and evaporation to obtain the flavone particles. The ultrasonic treatment time is long, and the flavonoid compound is difficult to dissolve in water so as to be incompletely dissolved, so that the flavone extraction content is low. Chinese patent document CN102225080A discloses a method for extracting flavonoids from passion fruit leaves by an ethanol-microwave soaking extraction method, wherein ethanol solution is added into passion fruit dry leaf powder, the temperature is increased, the extraction is carried out for 0.5h, then microwave extraction is carried out, then constant temperature water bath extraction is carried out continuously, and after the extraction is finished, a concentrated solution is obtained by filtering and vacuum concentration. The ratio of the material-liquid ratio is too large, so that the concentration difference of the flavone between the raw material and the solvent is too small, the mass transfer driving force is too low, the dissolution of the flavone is not facilitated, and the extraction content of the flavone is low.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings of the prior art and provide a method for extracting passion flower seed oil meal total flavonoids by adopting ultrasonic and microwave double-assistance. The method takes passion flower seed oil meal as a raw material, extracts natural active flavone substances in the passion flower seed oil meal, and extends the processing industrial chain of the passion flower.
The above purpose of the invention is realized by the following technical scheme:
a method for extracting passion flower seed oil meal total flavonoids by adopting ultrasonic and microwave double-assistance comprises the following steps:
s1, drying passion flower seeds at 55-70 ℃ to constant weight, crushing, and sieving with a sieve with the aperture of 0.250-0.425 mm to obtain seed powder;
s2, taking the seed powder, adding petroleum ether, and controlling the mass-to-volume ratio of the seed powder to the petroleum ether to be 6: condensing and refluxing for 70-85 min at the temperature of 42-58 ℃ for degreasing, evaporating and concentrating to recover petroleum ether, and collecting degreased seed oil meal;
s3, adding an ethanol-water solution into the seed oil meal, and performing ultrasonic extraction under the condition of a constant-temperature water bath at 75-85 ℃ to obtain a mixed solution;
and S4, performing microwave extraction on the mixed solution, and filtering to obtain a total flavone extracting solution.
The invention integrates and utilizes the vibration effect and cavitation effect of the ultrasonic extraction technology and the wall breaking and heating effect of the microwave extraction technology, greatly increases the extraction efficiency, and has the advantages of simple extraction process and no pollution of extraction solvent. The total flavone extraction content obtained by the method is 35.57-122.61 mg/g.
Further, in a preferred embodiment of the present invention, in step S3, the loading amount of the seed oil cake is 1.0-2.0 g.
Further, in the preferred embodiment of the present invention, in step S3, the loading of the seed meal is 1.0 g.
Further, in a preferred embodiment of the present invention, in step S3, the volume fraction of ethanol in the ethanol-water solution is 50% to 90%.
Further, in a preferred embodiment of the present invention, in step S3, the volume fraction of ethanol in the ethanol-water solution is 80%.
Further, in a preferred embodiment of the present invention, in step S3, the feed-liquid ratio of the seed oil meal to the ethanol-water solution is 1: 20-1: 60 g/mL.
Further, in a preferred embodiment of the present invention, in step S3, the ratio of the seed oil cake to the ethanol-water solution is 1: 50 g/mL.
Further, in the preferred embodiment of the present invention, in step S3, the ultrasound time is 10-60 min; the ultrasonic power is 200-500 w.
Further, in the preferred embodiment of the present invention, in step S3, the ultrasound time is 50min, and the ultrasound power is 300 w.
Further, in the preferred embodiment of the present invention, in step S3, the number of times of ultrasonic wave extraction is 2-3.
Further, in the preferred embodiment of the present invention, in step S4, the microwave power is 160-480 w; the microwave time is 30-150 s.
Further, in the preferred embodiment of the present invention, in step S4, the microwave power is 320w and the microwave time is 90S.
Further, in a preferred embodiment of the present invention, in step S4, the filtering is performed by a microporous membrane or vacuum filtration, and the vacuum degree of the vacuum filtration is-0.08 to-0.1 MPa; and (3) after the crude extraction liquid is subjected to suction filtration and reduced pressure is obtained, washing the seed oil meal residues for 2-3 times by using distilled water, and combining the filtrate.
Further, in the preferred embodiment of the present invention, in step S4, the vacuum degree of the vacuum filtration is-0.09 MPa to-0.1 MPa.
Further, in a preferred embodiment of the present invention, in step S1, the drying temperature of the passion fruit seeds is 60-65 ℃.
Further, in the preferred embodiment of the present invention, in step S1, the crushed material is passed through a sieve with a diameter of 0.300-0.355 mm.
Further, in the preferred embodiment of the present invention, in step S2, the mass-to-volume ratio of the seed powder to the petroleum ether is controlled to 6: 50-55.
Further, in a preferred embodiment of the present invention, the feed-liquid ratio of the seed oil meal to the ethanol-water solution is 1: 56.02g/mL, wherein the volume fraction of ethanol in the ethanol-water solution is 73.78%, the ultrasonic time is 50min, the ultrasonic power is 300w, the microwave power is 160w, and the microwave time is 90 s.
Further, in a preferred embodiment of the present invention, the method further comprises purifying the total flavone extract obtained in step S4, wherein the purifying step comprises: concentrating the total flavone extract obtained in the step S4 until no ethanol smell exists, freeze-drying the extract into powder, and separating and purifying by adopting AB-8 macroporous resin wet column packing, wherein the process conditions are as follows: the concentration of total flavonoids in the sample loading solution is 1.0-2.0 mg/mL, the pH of the sample loading solution is adjusted to 3-3.5, the sample is loaded at the flow rate of 7-9 r/min, and the weight of the resin is measured by the following steps: the loading amount is 25 mg: preparing an adsorption solution of resin and total flavonoids at a ratio of 110-120 mL; and after the sample loading is finished, washing with 90-100 mL of distilled water to remove impurities, and then eluting with 90-100 mL of 70% -75% ethanol solution at an elution flow rate of 10-12 r/min.
In the invention, the recovery rate of the total flavone is 86-90%, and the purity of the purified total flavone reaches 72-85%.
Further, in a preferred embodiment of the present invention, the resin is wet-weight: the loading amount is 25 mg: preparing an adsorption solution of resin and total flavonoids at a ratio of 115-120 mL.
Further, in a preferred embodiment of the present invention, the freeze-drying is vacuum freeze-drying. The freeze drying is to freeze dry the extract for 12 to 24 hours in vacuum at a temperature of between 80 ℃ below zero and 60 ℃ below zero.
Compared with the prior art, the invention has the following beneficial effects:
(1) the flavone is extracted from the passion flower seed oil meal, so that the medicinal value of the flavone is realized, and the utilization value of the passion flower can be maximized.
(2) The invention integrates and utilizes the vibration effect and cavitation effect of the ultrasonic extraction technology and the wall breaking and heating effect of the microwave extraction technology, greatly increases the extraction efficiency, and has the advantages of simple extraction process and no pollution of extraction solvent.
(3) The extraction content of the total flavone obtained by the method is 35.57-122.61 mg/g, the recovery rate of the total flavone is 86-90%, the purity of the purified total flavone reaches 72-85%, and the extraction content of the flavone is high.
Drawings
FIG. 1 shows the influence of the oil meal powder and ethanol-water solution ratio on the extraction content of flavone in step S3.
FIG. 2 is a graph showing the effect of the volume fraction of ethanol in the ethanol-water solution on the content of extracted flavonoids in step S3.
FIG. 3 shows the effect of the sonication time on the content of flavonoids in step S3.
FIG. 4 shows the effect of the ultrasonic power on the flavone extraction content in step S3.
FIG. 5 shows the effect of microwave power on the content of flavone extracted in step S4.
FIG. 6 shows the effect of microwave time on the content of flavone extract in step S4.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave double assistance
(1) Crushing: drying passion fruit seeds at 55 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.250mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 42mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 95 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: adding 20g/mL ethanol-water solution with 50% ethanol volume fraction, setting ultrasonic power at 200w, and extracting in 80 deg.C constant temperature water bath for 60min to obtain mixed solution;
(4) microwave extraction: placing the above mixed solution in a microwave processor, setting microwave power of 160w for extraction for 150s, and filtering with microporous membrane to obtain total flavone extractive solution with total flavone extraction content of 57.49 mg/g.
Example 2A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
(1) Crushing: drying passion fruit seeds at 70 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.425mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 58mL of petroleum ether into a quartz cup, condensing and refluxing for 85min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: adding an ethanol solution with the volume fraction of 90% ethanol into 60g/mL, setting the ultrasonic power at 500w, and extracting for 10min under the condition of 80 ℃ constant-temperature water bath to obtain a mixed solution;
(4) microwave extraction: placing the mixed solution in a microwave processor, setting the microwave power to 480w for extraction for 30s, and filtering by adopting a microporous filter membrane to obtain a total flavone extracting solution, wherein the total flavone extracting content is 84.90 mg/g.
Example 3A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
(1) Crushing: drying passion flower seeds at 60 ℃ to constant weight, crushing the dried passion flower seed oil meal by using a crusher, and sieving by using a 0.300mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 50mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: adding 50g/mL of ethanol solution with ethanol volume fraction of 80%, setting ultrasonic power of 300w, extracting for 30min under the condition of 80 ℃ constant-temperature water bath, wherein ultrasonic extraction frequency is 2 times to obtain mixed solution;
(4) microwave extraction: placing the mixed solution in a microwave processor, setting the microwave power to 320w for extracting for 90s, and filtering by adopting a microporous filter membrane to obtain a total flavone extracting solution, wherein the total flavone extracting content is 110.34 mg/g.
Example 4A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
(1) Crushing: drying passion fruit seeds at 65 deg.C to constant weight, pulverizing the dried passion fruit seeds with a pulverizer, and sieving with a 0.355mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 55mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: 56.02g/mL, adding an ethanol solution with ethanol volume fraction of 73.78%, setting ultrasonic power of 300w, extracting for 50min under the condition of 80 ℃ constant-temperature water bath, wherein the ultrasonic extraction frequency is 3 times, and obtaining a mixed solution;
(4) microwave extraction: placing the mixed solution in a microwave processor, setting the microwave power to 160w for extraction for 90s, and filtering by adopting a microporous filter membrane to obtain a total flavone extracting solution, wherein the total flavone extracting content is 117.53 mg/g.
Example 5A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
Extracting passion flower seed oil meal total flavonoids according to the method of example 4, wherein the previous three steps are the same as example 4, the step (4) is to place the mixed solution obtained in the previous three steps in a microwave processor, set the microwave power of 160w for extraction for 90s, carry out vacuum filtration under the condition that the vacuum degree is-0.09 to-0.1 MPa, obtain vacuum filtration reduced pressure crude extract, wash the seed oil meal residue with distilled water for 2-3 times, and combine the filtrates to obtain total flavonoids extract, wherein the total flavonoids extract content is 120.36 mg/g.
Example 6A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
(1) Crushing: drying passion fruit seeds at 60 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.425mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 50mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: 56.02g/mL, adding an ethanol solution with ethanol volume fraction of 73.78%, setting ultrasonic power of 300w, extracting for 50min under the condition of 80 ℃ constant-temperature water bath, and performing ultrasonic extraction for 3 times to obtain a mixed solution;
(4) microwave extraction: placing the mixed solution in a microwave processor, setting microwave power to extract for 90s, carrying out vacuum filtration under the conditions that the vacuum degree is-0.08 to-0.09 MPa, obtaining vacuum filtration reduced-pressure crude extract, washing seed oil meal residues for 2-3 times by using distilled water, and combining filtrates to obtain total flavone extract with the total flavone extraction content of 120.89 mg/g;
(5) and (3) purification: concentrating the total flavone extract obtained in the step S4 until no ethanol smell exists, and carrying out vacuum freeze drying on the extract at a temperature of between 80 ℃ below zero and 60 ℃ below zero for 12 to 24 hours to obtain powder; loading the column with AB-8 macroporous resin by wet method, preparing a loading solution with total flavone concentration of 1.0mg/mL, adjusting pH of the loading solution to 3, loading at flow rate of 9r/min, and loading according to wet weight of resin: the loading amount is 25 mg: preparing adsorption solution of resin and total flavonoids at a ratio of 100 mL; after the sample loading is finished, 90mL of distilled water is used for washing and removing impurities, and then 90mL of 70% ethanol solution is used for eluting, and the elution flow rate is 10 r/min. The recovery rate of the total flavone is 88.12%, and the purity of the purified total flavone is 70.14%.
Example 7A method for extracting Passiflora edulis seed oil meal total flavonoids by ultrasonic wave and microwave assistance
(1) Crushing: drying passion fruit seeds at 60 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.425mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 55mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: 56.02g/mL, adding an ethanol solution with ethanol volume fraction of 73.78%, setting ultrasonic power of 300w, extracting for 50min under the condition of 80 ℃ constant-temperature water bath, and performing ultrasonic extraction for 3 times to obtain a mixed solution;
(4) microwave extraction: placing the mixed solution in a microwave processor, setting microwave power to extract for 90s, carrying out vacuum filtration under the vacuum degree of-0.09-0.10 MPa, obtaining vacuum filtration reduced pressure crude extract, washing the seed oil meal residue with distilled water for 2-3 times, and combining filtrates to obtain total flavone extract with total flavone extraction content of 122.61 mg/g;
(5) and (3) purification: concentrating the total flavone extract obtained in the step S4 until no ethanol smell exists, and freeze-drying the extract into powder; loading AB-8 macroporous resin into a column by a wet method, preparing a loading solution with the total flavone concentration of 2.0mg/mL, adjusting the pH of the loading solution to 3.5, loading at the flow rate of 7r/min, and loading according to the wet weight of the resin: the loading amount is 25 mg: preparing an adsorption solution of resin and total flavonoids at a ratio of 120 mL; after the sample loading is finished, the sample is washed by 100mL of distilled water to remove impurities, and then eluted by 100mL of 70% ethanol solution with the elution flow rate of 12 r/min. The recovery rate of the total flavone is 90.32%, and the purity of the purified total flavone is 75.47%.
Comparative example 1
(1) Crushing: drying passion fruit seeds at 60 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.425mm sieve to obtain seed powder;
(2) degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 50mL of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
(3) ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: 56.02g/mL, adding an ethanol solution with ethanol volume fraction of 73.78%, setting ultrasonic power of 300w, extracting for 50min under the condition of 80 ℃ constant-temperature water bath, and performing ultrasonic extraction for 3 times to obtain a mixed solution;
(4) microwave extraction: placing the mixed solution into a microwave processor, setting microwave power to extract for 90s, carrying out vacuum filtration under the vacuum degree of-0.08-0.09 MPa, obtaining vacuum filtration reduced pressure crude extract, washing the seed oil meal residue with distilled water for 2-3 times, and combining filtrates to obtain total flavone extract with total flavone extraction content of 121.63 mg/g.
(5) And (3) purification: concentrating the total flavone extract obtained in the step S4 until no ethanol smell exists, and freeze-drying the extract into powder; loading the column with AB-8 macroporous resin by wet method, preparing a loading solution with total flavone concentration of 1.0mg/mL, adjusting pH of the loading solution to 6, loading at flow rate of 9r/min, and loading according to wet weight of resin: the loading amount is 25 mg: preparing an adsorption solution of resin and total flavonoids at a ratio of 110 mL; after the sample loading is finished, 90mL of distilled water is used for washing and removing impurities, and then 90mL of 70% ethanol solution is used for eluting, and the elution flow rate is 8 r/min. The recovery rate of the total flavone is 74.61%, and the purity of the purified total flavone is 66.19%.
Example 8 extraction Process optimization
1. Single factor experiment
(1) Method of producing a composite material
Extracting passionflower seed oil meal total flavonoids according to the method of example 1, selecting the raw materials of 50-90% of ethanol volume fraction and 1: 20-60 g/mL, 10-60 min of ultrasonic time, 200-500 w of ultrasonic power, 160-480 w of microwave power and 30-150 s of microwave power are taken as influence factors, the influence of each factor on the extraction content of the flavone is inspected, and each test treatment is repeated for 3 times.
(2) Results
1) The influence of the feed-liquid ratio of 1: 20, 1: 30, 1: 40, 1: 50 and 1: 60(g/mL) on the flavone extraction content is examined, and the result is shown in FIG. 1, wherein the flavone extraction content is obviously increased along with the decrease of the ratio of the feed-liquid ratio within the range of 1: 20-50 (g/mL), and the flavone extraction content is better when the feed-liquid ratio is 1: 50 (g/mL).
2) The influence of 50%, 60%, 70%, 80% and 90% of ethanol volume fraction on flavone extraction content is examined, and the result is shown in fig. 2, in a test range, the flavone extraction content shows a trend of increasing firstly and then decreasing along with the increase of ethanol volume fraction, and the extraction rate reaches a peak value when the ethanol volume fraction is 80%; when the volume fraction of ethanol exceeds 80%, the extraction content of flavone is reduced.
3) Examining the influence of the ultrasonic time of 10, 20, 30, 40, 50 and 60min on the flavone extraction content, the result is shown in fig. 3, the flavone extraction content increases with the prolonging of the ultrasonic time, when the ultrasonic time is more than 30min, the extraction rate increases slowly, because most of the effective components are dissolved out after the ultrasonic treatment for 30min, the influence on the improvement of the flavone extraction content is weak after the effective components are continuously prolonged. Therefore, the ultrasound time is preferably 30 min.
4) Examining the influence of the ultrasonic power of 200, 250, 300, 350, 400, 450 and 500w on the flavone extraction content, as shown in fig. 4, the ultrasonic power is in the range of 200-300 w, the flavone extraction content gradually increases with the increase of the ultrasonic power, when the ultrasonic power is 300w, the extraction amount reaches the peak value, and then the ultrasonic power is increased, and the flavone extraction content is reduced.
5) Examining the influence of microwave power 160, 240, 320, 400, 480W on the flavone extraction content, the result is shown in fig. 5, as the microwave power increases, the flavone extraction content tends to increase first and then decrease, and when the microwave power is 160W, the extraction rate reaches the maximum.
6) As a result of examining the influence of the microwave time of 30, 60, 90, 120, 150s on the content of extracted flavonoids, as shown in FIG. 6, the content of extracted flavonoids gradually increased with the increase of the microwave time, and reached the maximum value when the microwave time was 90s, and the extraction amount decreased with the further increase of the microwave time.
2. Response surface combination test
(1) Method of producing a composite material
And (3) taking the flavone extraction content as a response value, selecting ethanol volume fraction (A), material-liquid ratio (B), ultrasonic time (C) and microwave power (D) which have more remarkable influence on the flavone extraction content as independent variables from the single-factor test, and establishing a four-factor three-horizontal-center combined experimental design.
The response surface experimental protocol and results are shown in tables 1 and 2.
TABLE 1 response surface test independent variable factor horizon
TABLE 2 design of response surface and experimental results
And analyzing by Design Expert 8.0 software to obtain the optimal process, wherein the ratio of material to liquid is 1: 56.02g/mL, ethanol volume fraction of 73.78%, ultrasonic time of 50min, and microwave power of 160 w.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (1)
1. A method for extracting passion flower seed oil meal total flavonoids by adopting ultrasonic wave and microwave double assistance is characterized by comprising the following steps:
s1, crushing: drying passion fruit seeds at 60 ℃ to constant weight, crushing the dried passion fruit seeds by using a crusher, and sieving by using a 0.425mm sieve to obtain seed powder;
s2, degreasing: weighing 6.0g of seed powder, putting the seed powder into a filter paper cylinder, adding 55ml of petroleum ether into a quartz cup, condensing and refluxing for 70min at 85 ℃, degreasing, recovering the petroleum ether by rotary evaporation, and collecting degreased seed oil meal;
s3, ultrasonic extraction: weighing 1.0g of the seed oil meal, and mixing the raw materials in a material-liquid ratio of 1: 56.02g/mL, adding an ethanol solution with ethanol volume fraction of 73.78%, setting ultrasonic power of 300w, extracting for 50min under the condition of 80 ℃ constant-temperature water bath, and performing ultrasonic extraction for 3 times to obtain a mixed solution;
s4, microwave extraction: placing the mixed solution in a microwave processor, setting microwave power to 160w for extraction for 90s, carrying out reduced pressure suction filtration under the condition that the vacuum degree is-0.09 to-0.10 MPa, washing seed oil meal residues for 2-3 times after obtaining suction filtration reduced pressure crude extract, and combining filtrates to obtain total flavone extract;
s5, purification: concentrating the total flavone extract obtained in the step S4 until no ethanol smell exists, and freeze-drying the extract into powder; loading AB-8 macroporous resin into a column by a wet method, preparing a loading solution with the total flavone concentration of 2.0mg/mL, adjusting the pH of the loading solution to 3.5, loading at the flow rate of 7r/min, and loading according to the wet weight of the resin: the loading amount is 25 mg: preparing an adsorption solution of resin and total flavonoids at a ratio of 120 mL; after the sample loading is finished, the sample is washed by 100mL of distilled water to remove impurities, and then eluted by 100mL of 70% ethanol solution with the elution flow rate of 12 r/min.
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