CN112843102B - Method for extracting flavonoids compounds from hypsizygus marmoreus - Google Patents
Method for extracting flavonoids compounds from hypsizygus marmoreus Download PDFInfo
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- 241001534815 Hypsizygus marmoreus Species 0.000 title claims abstract description 53
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- 235000017173 flavonoids Nutrition 0.000 title claims abstract description 47
- -1 flavonoids compounds Chemical class 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 238000000605 extraction Methods 0.000 claims abstract description 59
- 239000000843 powder Substances 0.000 claims abstract description 34
- 230000008595 infiltration Effects 0.000 claims abstract description 25
- 238000001764 infiltration Methods 0.000 claims abstract description 25
- 230000002195 synergetic effect Effects 0.000 claims abstract description 20
- 230000008878 coupling Effects 0.000 claims abstract description 10
- 238000010168 coupling process Methods 0.000 claims abstract description 10
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- 239000007788 liquid Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 17
- 230000001808 coupling effect Effects 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000007710 freezing Methods 0.000 claims description 8
- 230000008014 freezing Effects 0.000 claims description 8
- 230000003287 optical effect Effects 0.000 claims description 8
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- 150000002215 flavonoids Chemical class 0.000 abstract description 15
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- 238000000874 microwave-assisted extraction Methods 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
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- 208000024172 Cardiovascular disease Diseases 0.000 description 1
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Abstract
The invention discloses a method for extracting flavonoids from hypsizygus marmoreus, which comprises the steps of carrying out ethanol infiltration on hypsizygus marmoreus powder by light wave-ultrasonic wave coupling, carrying out light wave-microwave synergistic extraction, and finally drying to obtain the flavonoids with higher purity. The invention ensures that the purity and the extraction rate of the extracted flavonoid compound are high by strictly controlling various parameters of the extraction process.
Description
Technical Field
The invention relates to the technical field of hypsizygus marmoreus processing, in particular to a method for extracting flavonoids compounds from hypsizygus marmoreus.
Background
The Flavonoids (flavanoids compounds) exist in free state or with glycoside form, have complex and diverse structure types, show diverse pharmacological actions, have important effects on cardiovascular and cerebrovascular disease resistance, cancer resistance, tumor resistance, immunoregulation and the like, and have the characteristic of low toxicity, so the Flavonoids (flavanoids compounds) are the hot spots for research and development of natural medicines and functional foods for a long time. Although the pharmacological action of flavonoid in fungi has not been studied thoroughly, the flavonoid is also paid extensive attention and becomes a new research hotspot.
Hypsizygus marmoreus (Hypsizygus marmoreus) also called Hypsizygus marmoreus and Hypsizygus marmoreus is an important factory-cultivated rare edible mushroom integrating edible, medicinal and dietetic functions, is one of the main varieties of factory cultivation of Chinese edible mushrooms at present, has high nutritional value and delicious taste due to the fact that the Hypsizygus marmoreus contains abundant vitamins, amino acids, mineral substances and the like, and is deeply loved by consumers.
In recent years, China has been greatly developed for researching seafood mushrooms, most of the seafood mushrooms are concentrated on the extraction and efficacy research of polysaccharide in the aspect of active substances, the research on flavonoid compounds is less, the research on yellow allergy and the like discusses the ultrasonic extraction process conditions of seafood mushroom total flavonoids, the best extraction conditions are determined by experiments, the material-liquid ratio is 1:40, the ultrasonic crushing is carried out for 4 times at 70 ℃ by 75% ethanol, the extraction time is 20min, and the total flavonoids yield is 0.061%; the hypsizygus marmoreus root total flavone is extracted from lupeng waves and the like by an ultrasonic auxiliary extraction method, wherein the volume fraction of ethanol is 70%, and the material-liquid ratio is 1: 50(g/mL), 6min of ultrasonic time and 150W of ultrasonic power, the yield of the total flavone is 2.178 mg/g. The current extraction methods of the flavonoid compounds in the hypsizygus marmoreus have the problems of low extraction rate and the like, so that the research and development of a time-saving, energy-saving and efficient extraction method is an urgent priority for extracting the flavonoid compounds in the hypsizygus marmoreus.
Disclosure of Invention
Based on the problems, the invention aims to provide a method for extracting flavonoids from hypsizygus marmoreus, which has a short extraction period and high extraction efficiency. The method comprises the steps of utilizing light wave-ultrasonic wave coupling infiltration, utilizing light wave-microwave synergistic extraction, and finally drying to obtain the flavonoid compound with higher purity.
The extraction method of the hypsizygus marmoreus flavonoid compound comprises the following steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 85-95% ethanol solution into the hypsizygus marmoreus powder, and then performing infiltration treatment for 300-420S under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 150-250W, and the ultrasonic wave power is 400-500W, so that the hypsizygus marmoreus powder is fully infiltrated by the ethanol solution;
(2) light wave-microwave synergistic extraction: after the infiltration is finished, adding the material obtained in the step (1) into hot water at 85-100 ℃, and adopting light wave-microwave synergistic extraction for 110-190S, wherein the light wave power is 70-120W, and the microwave power is 700-850W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
Preferably, the fineness of the seafood mushroom powder in the step (1) is 190-250 meshes.
Preferably, the feed-liquid ratio of the seafood mushroom powder to the ethanol solution in the step (1) is 1: 8-1: 10 g/mL.
Preferably, the ratio of the material to the hot water in the step (2) is 1: 0.5-1: 1.5 g/mL.
The purity of the hypsizygus marmoreus flavonoid compound obtained by the extraction method of the invention reaches 40-45%, and the extraction rate is as high as 3.5-4.5 mg/g.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention selects high-concentration ethanol solution as the impregnating compound, and the infiltration of the high-concentration ethanol solution is enhanced under the coupling action of light wave and ultrasonic wave, so that the hypsizygus marmoreus powder is quickly and fully infiltrated by the ethanol solution, and the problems of high hardness, difficult infiltration or uneven wetting of the hypsizygus marmoreus powder are solved.
(2) According to the invention, hot water is added in the extraction process, so that the seafood mushroom powder is extracted into the lower-concentration ethanol solution to obtain the flavonoid compounds, meanwhile, under the synergistic effect of the light wave and the microwave, the light wave and the microwave provide enough heat to maintain the continuous boiling of the low-concentration ethanol, the ethanol is instantly vaporized to cause the boiling of the seafood mushroom, the convection diffusion of the active ingredients such as the flavonoid compounds is quicker, the flavonoid compounds enter the solvent more quickly, the yield and the purity of the flavonoid compounds are improved, and the extraction time is shortened.
(3) Microwave extraction is to improve extraction efficiency, reduce extraction time, and reduce feed liquid consumption by generating efficient internal heat and dielectric heat, but has problems of uneven heating, destruction of material structure, and the like. The light wave extraction is to use a lamp to generate heat, then use a high-efficiency reflecting disc to transmit the generated heat energy to a high-temperature resistant glass panel, and transmit the heat energy to a container to be heated at high speed through the glass panel. The method adopts the light wave-microwave synergistic extraction of the flavonoid compounds in the hypsizygus marmoreus, simultaneously utilizes the uniformity of the light wave and the strong selectivity of the microwave, and avoids the problems of uneven heating and damage to the structure of the substance by using the microwave, thereby improving the extraction efficiency and the purity of the flavonoid compounds.
(4) The hypsizygus marmoreus flavonoid compound extracted by the technology does not need to be purified again, and the flavonoid compound with higher purity can be obtained.
Detailed Description
The extraction method of the hypsizygus marmoreus flavonoid compound comprises the following steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 85-95% ethanol solution into the hypsizygus marmoreus powder, and then performing infiltration treatment for 300-420S under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 150-250W, and the ultrasonic wave power is 400-500W, so that the hypsizygus marmoreus powder is fully infiltrated by the ethanol solution;
(2) light wave-microwave synergistic extraction: after the infiltration is finished, adding the material obtained in the step (1) into hot water at 85-100 ℃, and adopting light wave-microwave synergistic extraction for 110-190S, wherein the light wave power is 70-120W, and the microwave power is 700-850W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
Specifically, in some embodiments, the fineness of the seafood mushroom powder in the step (1) is 190-250 meshes. When the fineness of the seafood mushroom powder is too small, the seafood mushroom powder is very easy to be gelatinized when being mixed with hot water; when the fineness of the hypsizygus marmoreus is too large, the extraction efficiency is extremely easy to reduce and the extraction time is extremely easy to prolong.
Specifically, in some embodiments, the feed-liquid ratio of the seafood mushroom powder to the ethanol solution in the step (1) is 1: 8-1: 10 g/mL.
Specifically, in some embodiments, the feed-liquid ratio of the material to the hot water in the step (2) is 1: 0.5-1: 1.5 g/mL.
The purity of the hypsizygus marmoreus flavonoid compound obtained by the extraction method provided by the invention reaches 40-45%, and the extraction rate is as high as 3.5-4.5 mg/g.
The present invention will be further described with reference to the following specific examples.
Example 1
A method for extracting flavonoids from hypsizygus marmoreus comprises the following specific steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 95% ethanol solution into 200-mesh seafood mushroom powder, wherein the feed-liquid ratio of the seafood mushroom powder to the ethanol solution is 10 g/mL; then, soaking for 420S under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 250W and the ultrasonic wave power is 500W, so that the hypsizygus marmoreus powder is fully soaked by the ethanol solution;
(2) light wave-microwave synergistic extraction: after infiltration, adding the material obtained in the step (1) into hot water at 100 ℃, wherein the material-liquid ratio of the material to the hot water is 1:1g/mL, and adopting light wave-microwave synergistic extraction for 110S, wherein the light wave power is 120W and the microwave power is 850W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
The purity of the obtained hypsizygus marmoreus flavonoid compound is 41.6%, and the extraction rate is 3.6 mg/g.
Example 2
A method for extracting flavonoids from hypsizygus marmoreus comprises the following specific steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 95% ethanol solution into 250-mesh seafood mushroom powder, wherein the feed-liquid ratio of the seafood mushroom powder to the ethanol solution is 1:8 g/mL; then, performing infiltration treatment for 400S under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 200W and the ultrasonic wave power is 450W, so that the hypsizygus marmoreus powder is fully infiltrated by the ethanol solution;
(2) light wave-microwave synergistic extraction: after infiltration, adding the material obtained in the step (1) into hot water at 100 ℃, wherein the material-liquid ratio of the material to the hot water is 1:0.5g/mL, and performing light wave-microwave synergistic extraction for 150S, wherein the light wave power is 100W and the microwave power is 800W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
The purity of the hypsizygus marmoreus flavonoid compound obtained by the invention is 40.2%, and the extraction rate is 3.7 mg/g.
Example 3
A method for extracting flavonoid compounds from hypsizygus marmoreus comprises the following specific steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding an ethanol solution with the mass concentration of 95% into the seafood mushroom powder with the fineness of 210 meshes, wherein the feed-liquid ratio of the seafood mushroom powder to the ethanol solution is 1: 8-1: 10 g/mL; then, under the coupling action of light wave and ultrasonic wave, the sea fresh mushroom powder is soaked for 300-420S, the light wave power is 150-250W, and the ultrasonic wave power is 400-500W, so that the sea fresh mushroom powder is fully soaked by the ethanol solution;
(2) light wave-microwave synergistic extraction: after infiltration, adding the material obtained in the step (1) into hot water at 85-100 ℃, wherein the material-liquid ratio of the material to the hot water is 1:1.2g/mL, and adopting light wave-microwave synergistic extraction for 110-190S, the light wave power is 80W and the microwave power is 820W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
The purity of the obtained hypsizygus marmoreus flavonoid compound is 41.2-44.3%, and the extraction rate is 3.7-4.3 mg/g.
Example 4
A method for extracting flavonoids from hypsizygus marmoreus comprises the following specific steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 95% ethanol solution into 190-mesh seafood mushroom powder, wherein the material-liquid ratio of the seafood mushroom powder to the ethanol solution is 1:9 g/mL; then, soaking 320 seconds under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 180W, and the ultrasonic wave power is 430W, so that the hypsizygus marmoreus powder is fully soaked by the ethanol solution;
(2) light wave-microwave synergistic extraction: after infiltration, adding the material obtained in the step (1) into hot water at 100 ℃, wherein the material-liquid ratio of the material to the hot water is 1:1.5g/mL, and adopting light wave-microwave synergistic extraction for 110S, wherein the light wave power is 70W, and the microwave power is 700W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
The purity of the hypsizygus marmoreus flavonoid compound obtained by the invention is 43.1%, and the extraction rate is 4.4 mg/g.
Example 5
A method for extracting flavonoids from hypsizygus marmoreus comprises the following specific steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding 95% ethanol solution into 250-mesh seafood mushroom powder, wherein the material-liquid ratio of the seafood mushroom powder to the ethanol solution is 1:10 g/mL; then, performing infiltration treatment for 350 seconds under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 200W and the ultrasonic wave power is 500W, so that the hypsizygus marmoreus powder is fully infiltrated by the ethanol solution;
(2) light wave-microwave synergistic extraction: after infiltration is finished, adding the material obtained in the step (1) into hot water at 90 ℃, wherein the material-liquid ratio of the material to the hot water is 1:0.8g/mL, extracting 120S by adopting light wave-microwave synergy, and the light wave power is 120W and the microwave power is 700W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
The purity of the hypsizygus marmoreus flavonoid compound obtained by the invention is 41.6%, and the extraction rate is 3.9 mg/g.
Example 6 Effect of different extraction methods on Hypsizygus marmoreus Flavonoids
Different extraction methods such as ethanol extraction, microwave extraction, light wave extraction and light wave-microwave synergistic extraction are selected, and the influence of the different extraction methods on the extraction yield and purity of the flavonoid compounds in the hypsizygus marmoreus is examined. The results are shown in Table 1.
TABLE 1 Effect of different extraction methods on Flavonoids of Hypsizygus marmoreus
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (4)
1. A method for extracting flavonoids compounds from hypsizygus marmoreus is characterized by comprising the following steps:
(1) optical wave-ultrasonic wave coupling infiltration: adding an ethanol solution with the mass concentration of 85-95% into the hypsizygus marmoreus powder, and then performing infiltration treatment for 300-420S under the coupling action of light wave and ultrasonic wave, wherein the light wave power is 150-250W, and the ultrasonic wave power is 400-500W, so that the hypsizygus marmoreus powder is fully infiltrated by the ethanol solution, and the material-liquid ratio of the hypsizygus marmoreus powder to the ethanol solution is 1: 8-1: 10 g/mL;
(2) light wave-microwave synergistic extraction: after the infiltration is finished, adding the material obtained in the step (1) into hot water with the temperature of 85-100 ℃, and adopting light wave-microwave synergistic extraction for 110-190S, wherein the light wave power is 70-120W, and the microwave power is 700-850W; vacuum filtering, centrifuging, and concentrating;
(3) and (3) drying: and quickly freezing the concentrated filtrate, and then carrying out vacuum freeze drying.
2. The extraction method of hypsizygus marmoreus flavonoids compounds according to claim 1, characterized in that: the fineness of the seafood mushroom powder in the step (1) is 190-250 meshes.
3. The extraction method of hypsizygus marmoreus flavonoids compounds according to claim 1, characterized in that: the ratio of the material to the hot water in the step (2) is 1: 0.5-1: 1.5 g/mL.
4. The extraction method of hypsizygus marmoreus flavonoids compounds according to claim 1, characterized in that: the extraction yield of the hypsizygus marmoreus flavonoid compounds reaches 3.5-4.5 mg/g, and the purity reaches 40-45%.
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