CN111387477A - Microcapsule embedding technology for improving digestion stability of lotus leaf flavone - Google Patents
Microcapsule embedding technology for improving digestion stability of lotus leaf flavone Download PDFInfo
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Abstract
A preparation technology of microcapsules for improving the digestive stability of lotus leaf flavone is characterized in that maltodextrin, egg white concentrated protein, soybean lecithin and fish gelatin are used as wall materials, and the lotus leaf flavone microcapsules are prepared by adopting high-pressure homogenization and spray drying technologies to obtain a lotus leaf flavone microcapsule product capable of improving the digestive stability of lotus leaf flavone. The invention uses the water solution of ethanol as solvent to extract the flavonoid compounds in lotus leaves, adds the lotus leaf flavonoid and the soybean lecithin solution into the maltodextrin-fish gelatin solution according to a certain proportion, and adopts the high-pressure homogenization technology to process; the maltodextrin, the egg white concentrated protein, the soybean lecithin and the fish gelatin are used as wall materials to embed the lotus leaf flavone, the embedding rate is high, the prepared flavone microcapsule has better stability, and the release percentage of the lotus leaf flavone is obviously reduced after the lotus leaf microcapsule is stored for 30 days; the modified fish gelatin has a good affinity effect on the flavone, and can help adsorb the flavone in the microcapsule with good stability.
Description
Technical Field
The invention relates to a microcapsule embedding technology for improving the digestive stability of lotus leaf flavone, belonging to the technical field of food processing.
Background
The microcapsule is a powder particle formed by properly mixing protein, polysaccharide, surfactant and the like and then spray-drying, can be used as an embedding system of nutritional efficacy factors such as phenolic acid, flavone, grease, active peptide and the like, wraps sensitive nutrients or functional factors in a wall material or a shell, improves the stability of light, heat and pH, achieves the effects of controlling release and improving the processing application range, and is widely applied to the fields of health products, medicines and the like.
The lotus leaf (Nelumbo nucifera leaf) is a famous dual-purpose medicine and food resource in China, and has the effects of clearing summer heat, removing dampness, clearing away heart-fire, removing heat, stopping bleeding, promoting diuresis and the like. Research shows that the lotus leaf extract has the functions of reducing fat and losing weight, resisting inflammation, resisting oxidation, resisting cancer, whitening, inhibiting atherosclerosis, resisting diabetes and the like, and the flavonoid compound is the main active component in the lotus leaves. However, the lotus leaf flavone has the defects of poor water solubility and digestive stability, and the pH, light, heat and the like are determined, so that the application of the lotus leaf flavone in the fields of functional foods, health-care products, cosmetics and the like is greatly limited.
Based on the current situation, the lotus leaf flavone microcapsule product capable of improving the digestion stability of lotus leaf flavone is obtained by adopting the solvent extraction and column chromatography separation and enrichment technologies to prepare the lotus leaf flavone component, taking maltodextrin, egg white concentrated protein, soybean lecithin and fish gelatin as wall materials and adopting high-pressure homogenization and spray drying technologies. The lotus leaf flavone microcapsule product prepared by the technology has high embedding rate, strong storage stability and digestion stability, and has no report at home and abroad.
Disclosure of Invention
The invention aims to prepare a lotus leaf flavone microcapsule product capable of improving the digestion stability of lotus leaf flavone by using high-pressure homogenization and spray drying technologies by using maltodextrin, egg white concentrated protein, soybean lecithin and fish gelatin as wall materials according to the technologies of unstable storage of the flavone, easy instability of light, heat and oxygen, solvent extraction and column chromatography separation and enrichment. The lotus leaf flavone microcapsule product prepared by the technology has high embedding rate, and strong storage stability and digestion stability.
The preparation method comprises the following steps:
a microcapsule embedding technology for improving the digestion stability of lotus leaf flavone comprises the following steps:
(1) crushing lotus leaves to obtain lotus leaf particles;
(2) treating the lotus leaf particles by using an ethanol water solution as a solvent to obtain an extracting solution, and performing vacuum concentration and drying on the extracting solution to obtain a lotus leaf crude extract;
(3) dissolving the lotus leaf crude extract prepared in the step (2) with water, preparing a lotus leaf crude extract, and separating and enriching by adopting a column chromatography method to obtain a lotus leaf flavone component;
(4) preparing a lotus leaf flavone solution by using absolute ethyl alcohol as a solvent, and preparing a maltodextrin-egg white concentrated protein-fish gelatin-soybean lecithin wall material solution by using distilled water;
(5) slowly injecting the lotus leaf flavone solution prepared in the step (4) into the maltodextrin-egg white concentrated protein-fish gelatin-soybean lecithin mixed wall material solution prepared in the step (4) to form pre-emulsion, and treating by using a high-pressure homogenization technology;
(6) and (4) spray-drying the pre-emulsion subjected to high-pressure homogenization treatment in the step (5) by adopting a spray-drying technology to obtain the lotus leaf flavone microcapsules.
The preparation method of the fish gelatin comprises the following steps:
(1) pretreatment of raw materials: removing impurities from the surface of grass carp, washing with tap water, and oven drying at 40 deg.C
(2) Decalcifying fish scales with 0.3 mol/L hydrochloric acid at a ratio of fish scales to hydrochloric acid of 1:25(g: m L) for 1h, washing with tap water for 3-5 times after decalcification, and oven drying;
(3) the preparation method of the black carp scale gelatin comprises the steps of adding the dried fish scales into distilled water, wherein the feed-liquid ratio of the fish scales to the water is 1:15(g: m L), the pH value is 5.5 (the pH value is adjusted to be a specified value by hydrochloric acid), heating and extracting in a water bath at the temperature of 80 ℃ for 2h, and carrying out freeze drying on an extracting solution after suction filtration.
(4) Performing ultrasonic treatment, namely dissolving freeze-dried fish phosphorus gelatin by using distilled water to obtain a fish scale gelatin solution with the mass ratio of 10%, and adopting a Q700 ultrasonic cell disruption instrument (with the probe size of 1/8 ″ -3 mm), the working frequency of 20kHz, the ultrasonic pulse working time of 5s and the intermittent time of 5s to prepare the fish scale gelatin capsule, wherein the fish scale gelatin capsule is prepared by filling 15m L of the fish scale gelatin solution into a 25m L beaker, and the ultrasonic intensity of 120W/cm2And treating in ice bath for 10min, and freeze drying to obtain the high-surface-activity fish scale gelatin.
Preferably, the lotus leaf is dried lotus leaf, and crushed into lotus leaf particles having a particle size of not more than 1000 μm.
Preferably, the lotus leaf crude extract is extracted at room temperature for 12h by using 75% (v/v) ethanol aqueous solution as an extraction solvent, centrifuged, collected centrifugate, residues are extracted at room temperature for 12h by using 75% ethanol, centrifuged, combined centrifugates, and concentrated and dried under the vacuum of 0.08-0.1Mpa, wherein the concentration temperature is not higher than 60 ℃.
And (3) performing column chromatography, wherein the concentration of the aqueous solution of the lotus leaf flavone crude extract is 50-100 mg/m L, an AB-8 macroporous adsorption resin is used as a fixed phase, wet-process sample loading is performed, the sample loading amount is 0.5BV, the sample loading flow rate is 2-3 BV/h, gradient elution is performed by using 20%, 80% and 100% ethanol after static adsorption is performed for 8-12 h, the elution volume is 3BV, the elution flow rate is 2-3 BV/h, and the concentrated 80% ethanol elution component is collected to obtain the lotus leaf flavone component.
And (4) preparing the wall material solution in the step (4), wherein the dextrose equivalent value of maltodextrin is 21, the maltodextrin, the egg white concentrated protein and the fish gelatin are dissolved by warm water at 70 ℃ and are dissolved for 1h at 120rpm, then the soybean lecithin is added, the contents of the maltodextrin, the egg white concentrated protein, the fish gelatin and the soybean lecithin are respectively 38-42%, 8-10%, 4-5% and 2%, and the concentration of the lotus leaf flavone is 45-55mg/m L.
According to the high-pressure homogenization technology in the step (5), the mass ratio of the lotus leaf flavone solution to the wall material solution is 1:5, the high-pressure homogenization treatment pressure is 60Mpa, and the treatment times are 2 times;
the spray drying technology in the step (6) is characterized in that the inlet air temperature of spray drying is 170-180 ℃, the outlet air temperature is 60-70 ℃, and the flow rate is 15-25m L/min.
The product is characterized in that: the invention adopts the solvent extraction and column chromatography separation enrichment technology to prepare the lotus leaf flavone component, takes maltodextrin, egg white concentrated protein, soybean lecithin and fish gelatin as wall materials, and adopts the high-pressure homogenization and spray drying technology to prepare the lotus leaf flavone microcapsule, thereby obtaining the lotus leaf flavone microcapsule product capable of improving the digestion stability of lotus leaf flavone. The lotus leaf flavone microcapsule product prepared by the technology has high embedding rate and strong storage stability and digestion stability, and can be applied to the fields of functional foods and health-care products.
The invention has the beneficial effects that:
compared with the prior art, the invention has the following advantages:
(1) the lotus leaf flavone is extracted and enriched by using an ethanol water solution as a solvent, the extraction and enrichment efficiency is high, the ethanol can be recycled, and the environmental pollution is small;
(2) the macroporous adsorption resin column is adopted for enrichment, and the enriched macroporous adsorption resin column can be recycled after being activated, so that the cost is low and the operation is simple;
(3) the maltodextrin, the egg white concentrated protein, the soybean lecithin and the fish gelatin are used as wall materials to embed the lotus leaf flavone, the embedding rate is high, the prepared flavone microcapsule has better stability, and the release percentage of the lotus leaf flavone is obviously reduced after the lotus leaf microcapsule is stored for 30 days; the modified fish gelatin has a good affinity effect on the flavone, and can help adsorb the flavone in the microcapsule with good stability.
(4) The microcapsule powder particles are prepared by adopting high-pressure homogenization and spray drying technologies, and the technical problems of large particle size, uneven particle size distribution, poor stability and the like of the microcapsule particles are solved. The produced lotus leaf flavone microcapsule has strong storage stability and digestion stability, and expands the application of lotus leaf flavone in functional foods and health-care products.
Detailed Description
Example 1
(1) Crushing the dried lotus leaves to obtain lotus leaf particles with the particle size not higher than 1 mm;
(2) mixing 75% (v/v) ethanol water solution as solvent with folium Nelumbinis powder at a ratio of 1:20, extracting at room temperature for 12 hr, centrifuging, collecting centrifugate, extracting residue with 75% ethanol at room temperature for 12 hr, centrifuging, mixing centrifugates, vacuum concentrating under 0.08-0.1Mpa, and drying to obtain folium Nelumbinis flavone crude extract at concentration temperature of no higher than 60 deg.C;
(3) dissolving the lotus leaf crude extract prepared in the step (2) by using water, preparing a lotus leaf flavone solution with the concentration of 80mg/m L, performing wet-process sample loading by using AB-8 macroporous adsorption resin as a stationary phase, wherein the sample loading amount is 0.5BV, the sample loading flow rate is 2.5BV/h, performing static adsorption for 8 hours, sequentially performing gradient elution by using 20%, 80% and 100% ethanol, the elution volume is 3BV, the elution flow rate is 2-3 BV/h, collecting the elution component of 80% ethanol, and performing vacuum concentration and drying under 0.08-0.1Mpa to obtain a lotus leaf flavone component;
(4) preparing 50mg/m L lotus leaf flavone solution by using absolute ethyl alcohol as a solvent, dissolving maltodextrin, egg white concentrated protein and fish gelatin by using warm water at 70 ℃, dissolving for 1h at 120rpm, and adding soybean lecithin to obtain a wall material solution, wherein the contents of the maltodextrin, the egg white concentrated protein, the fish gelatin and the soybean lecithin are respectively 42%, 8%, 5% and 2%, and the dextrose equivalent value of the maltodextrin is 21;
(5) slowly injecting the lotus leaf flavone solution prepared in the step (4) into the maltodextrin-fish gelatin-soybean lecithin mixed wall material solution prepared in the step (4) according to the volume ratio of 1:5 to form pre-emulsion, and treating for 2 times at 60Mpa by using a high-pressure homogenization technology;
(6) and (3) spray-drying the pre-emulsion subjected to high-pressure homogenization treatment in the step (5) by adopting a spray-drying technology, wherein the air inlet temperature is 170-180 ℃, the air outlet temperature is 60-70 ℃, and the flow rate is 20m L/min, so that the lotus leaf flavone micro-gel is finally obtained.
The preparation method of the fish gelatin comprises the following steps:
pretreating raw materials, namely removing impurities on the surfaces of grass carp scales, washing the grass carp scales with tap water, drying the grass carp scales at 40 ℃ for later use, decalcifying the grass carp scales with 0.3 mol/L hydrochloric acid, wherein the material-liquid ratio of the grass carp scales to the hydrochloric acid is 1:25(g: m L), the decalcifying time is 1h, washing the fish scales with tap water for 3-5 times after decalcification, drying the black carp scale gelatin, preparing black carp scale gelatin, namely adding the dried fish scales into distilled water, wherein the material-liquid ratio of the fish scales to the water is 1:15(g: m L), the pH is 5.5 (adjusted to a specified pH value with hydrochloric acid), heating the dried fish scales in a water bath at 80 ℃, extracting for 2h, freezing and drying the extract after suction filtration, performing ultrasonic treatment, dissolving freeze-dried fish phosphorus gelatin in the distilled water to obtain a fish scale gelatin solution with the mass ratio of 10%, and using a Q700 ultrasonic cell disruptor (probe size 1/8 mm), the working frequency is 20, the ultrasonic pulse working time is 5s, the intermittent time is 3615 m, and the ultrasonic intensity is 120 cm/L W of the beaker2And treating in ice bath for 10min, and freeze drying to obtain the high-surface-activity fish scale gelatin.
The embedding rate test of the lotus leaf flavone microcapsules prepared in the embodiment shows that the embedding rate of the lotus leaf flavone microcapsules prepared in the embodiment is 98.5%, and the lotus leaf flavone release percentage is 9.6% when the lotus leaf flavone microcapsules are stored for 30 days under the conditions of pH 7.0 and 25 ℃.
Example 2
(1) Crushing the dried lotus leaves to obtain lotus leaf particles with the particle size not higher than 1 mm;
(2) mixing 75% (v/v) ethanol water solution as solvent with folium Nelumbinis powder at a ratio of 1:20, extracting at room temperature for 12 hr, centrifuging, collecting centrifugate, extracting residue with 75% ethanol at room temperature for 12 hr, centrifuging, mixing centrifugates, vacuum concentrating under 0.08-0.1Mpa, and drying to obtain folium Nelumbinis flavone crude extract at concentration temperature of no higher than 60 deg.C;
(3) dissolving the lotus leaf crude extract prepared in the step (2) by using water, preparing a lotus leaf flavone solution with the concentration of 80mg/m L, performing wet-process sample loading by using AB-8 macroporous adsorption resin as a stationary phase, wherein the sample loading amount is 0.5BV, the sample loading flow rate is 2.0BV/h, performing static adsorption for 12h, sequentially performing gradient elution by using 20%, 80% and 100% ethanol, the elution volume is 3BV, the elution flow rate is 2-3 BV/h, collecting the elution component of 80% ethanol, and performing vacuum concentration and drying under 0.08-0.1Mpa to obtain a lotus leaf flavone component;
(4) preparing a lotus leaf flavone solution with the concentration of 45mg/m L by using absolute ethyl alcohol as a solvent, dissolving maltodextrin, egg white concentrated protein and fish gelatin in warm water with the temperature of 70 ℃, dissolving for 1h at 120rpm, and adding soybean lecithin to obtain a wall material solution, wherein the contents of the maltodextrin, the egg white concentrated protein, the fish gelatin and the soybean lecithin are respectively 38%, 10%, 5% and 2%, and the dextrose equivalent value of the maltodextrin is 21;
(5) slowly injecting the lotus leaf flavone solution prepared in the step (4) into the maltodextrin-fish gelatin-soybean lecithin mixed wall material solution prepared in the step (4) according to the volume ratio of 1:4.5 to form pre-emulsion, and treating for 2 times at 60Mpa by using a high-pressure homogenization technology;
(6) and (3) spray-drying the pre-emulsion subjected to high-pressure homogenization treatment in the step (5) by adopting a spray-drying technology, wherein the air inlet temperature is 170-180 ℃, the air outlet temperature is 60-70 ℃, and the flow rate is 22m L/min, and finally obtaining the lotus leaf flavone microcapsules, wherein the preparation method of the fish scale gelatin is the same as that in example 1.
The embedding rate test of the lotus leaf flavone microcapsules prepared in the embodiment shows that the embedding rate of the lotus leaf flavone microcapsules prepared in the embodiment is 97.6%, the lotus leaf flavone microcapsules are stored for 30 days under the conditions of pH 7.0 and 25 ℃, and the release percentage of the lotus leaf flavone is 8.2%.
Example 3
(1) Crushing the dried lotus leaves to obtain lotus leaf particles with the particle size not higher than 1 mm;
(2) mixing 70% (v/v) ethanol water solution as solvent with folium Nelumbinis powder at a ratio of 1:20, extracting at room temperature for 12 hr, centrifuging, collecting centrifugate, extracting residue with 70% ethanol at room temperature for 12 hr, centrifuging, mixing centrifugates, vacuum concentrating under 0.08-0.1Mpa, and drying to obtain folium Nelumbinis flavone crude extract at concentration temperature of no higher than 60 deg.C;
(3) dissolving the lotus leaf crude extract prepared in the step (2) by using water, preparing a lotus leaf flavone solution with the concentration of 80mg/m L, performing wet-process sample loading by using AB-8 macroporous adsorption resin as a stationary phase, wherein the sample loading amount is 0.5BV, the sample loading flow rate is 2.0BV/h, performing static adsorption for 12 hours, sequentially performing gradient elution by using 20%, 80% and 100% ethanol, the elution volume is 3BV, the elution flow rate is 2-3 BV/h, collecting the elution component of 80% ethanol, and performing vacuum concentration and drying under 0.08-0.1Mpa to obtain a lotus leaf flavone component;
(4) preparing 50mg/m L lotus leaf flavone solution by using absolute ethyl alcohol as a solvent, dissolving maltodextrin, egg white concentrated protein and fish gelatin by using warm water at 70 ℃, dissolving for 1h at 120rpm, and adding soybean lecithin to obtain a wall material solution, wherein the contents of the maltodextrin, the egg white concentrated protein, the fish gelatin and the soybean lecithin are 40%, 11%, 4% and 2% respectively, and the dextrose equivalent value of the maltodextrin is 21;
(5) slowly injecting the lotus leaf flavone solution prepared in the step (4) into the maltodextrin-fish gelatin-soybean lecithin mixed wall material solution prepared in the step (4) according to the volume ratio of 1:5 to form pre-emulsion, and treating for 2 times at 60Mpa by using a high-pressure homogenization technology;
(6) and (3) spray-drying the pre-emulsion subjected to high-pressure homogenization treatment in the step (5) by adopting a spray-drying technology, wherein the air inlet temperature is 175-180 ℃, the air outlet temperature is 65-70 ℃, and the flow rate is 20m L/min, and finally obtaining the lotus leaf flavone microcapsules, wherein the preparation method of the fish scale gelatin is the same as that in example 1.
The embedding rate test of the lotus leaf flavone microcapsules prepared in the embodiment shows that the embedding rate of the lotus leaf flavone microcapsules prepared in the embodiment is 98.2%, the lotus leaf flavone microcapsules are stored for 30 days under the conditions of pH 7.0 and 25 ℃, and the release percentage of the lotus leaf flavone is 7.8%.
Comparative example 1
This comparative example differs from example 1 in that no fish gelatin was added to the wall material, as in example 1. The embedding rate test of the lotus leaf flavone microcapsule prepared in the comparative example shows that the embedding rate of the lotus leaf flavone microcapsule prepared in the example is 89.2%, the lotus leaf flavone release percentage is 21.3% when the lotus leaf flavone microcapsule is stored for 30 days under the conditions of pH 7.0 and 25 ℃.
Claims (8)
1. A microcapsule embedding technology for improving the digestion stability of lotus leaf flavone is characterized by comprising the following steps:
(1) crushing lotus leaves to obtain lotus leaf particles;
(2) treating the lotus leaf particles by using an ethanol water solution as a solvent to obtain an extracting solution, and performing vacuum concentration and drying on the extracting solution to obtain a lotus leaf crude extract;
(3) dissolving the lotus leaf crude extract prepared in the step (2) with water, preparing a lotus leaf crude extract, and separating and enriching by adopting a column chromatography method to obtain a lotus leaf flavone component;
(4) preparing a lotus leaf flavone solution by using absolute ethyl alcohol as a solvent, and preparing a maltodextrin-egg white concentrated protein-fish gelatin-soybean lecithin wall material solution by using distilled water;
(5) slowly injecting the lotus leaf flavone solution prepared in the step (4) into the maltodextrin-egg white concentrated protein-fish gelatin-soybean lecithin mixed wall material solution prepared in the step (4) to form pre-emulsion, and treating by using a high-pressure homogenization technology;
(6) and (4) spray-drying the pre-emulsion subjected to high-pressure homogenization treatment in the step (5) by adopting a spray-drying technology to obtain the lotus leaf flavone microcapsules.
2. The fish gelatin according to step (4) of claim 1, which is prepared by:
(1) pretreatment of raw materials: removing impurities on the surfaces of the scales of the grass carps, washing the grass carps clean by tap water, and drying the grass carps at 40 ℃ for later use;
(2) decalcifying fish scales with 0.3 mol/L hydrochloric acid at a ratio of fish scales to hydrochloric acid of 1:25(g: m L) for 1h, washing with tap water for 3-5 times after decalcification, and oven drying;
(3) adding the dried fish scales into distilled water, wherein the ratio of the fish scales to the water is 1:15(g: m L), the pH is 5.5 (the solution is adjusted to the designated pH by hydrochloric acid), heating and extracting in a water bath at 80 ℃ for 2h, and carrying out freeze drying on the extract after suction filtration;
(4) ultrasonic treatment: dissolving lyophilized fish phosphorus gelatin with distilled water to obtain fish scale gelatin solution with weight ratio of 10%, and ultrasonic crushing with Q700 ultrasonic cell disrupter (probe size 1/8 ═ 3mm), working frequency of 20kHz, and ultrasonicThe pulse working time is 5s, the intermittent time is 5s, and the preparation method comprises placing 15m L fish scale gelatin solution into 25m L beaker with ultrasonic intensity of 120W/cm2And treating in ice bath for 10min, and freeze drying to obtain the high-surface-activity fish scale gelatin.
3. The lotus leaf according to step (1) of claim 1, wherein the lotus leaf is dried lotus leaf, pulverized into lotus leaf particles having a particle size of not more than 1000 μm.
4. The crude extract of lotus leaf according to the step (2) of claim 1, wherein 75% (v/v) aqueous ethanol is used as an extraction solvent, the extraction is performed for 12 hours at room temperature, then centrifugation is performed, the centrifugate is collected, the residue is extracted for 12 hours at room temperature by using 75% ethanol, centrifugation is performed, the centrifugate is combined twice, and the vacuum concentration and drying are performed under the pressure of 0.08-0.1MPa, and the concentration temperature is not higher than 60 ℃.
5. The column chromatography method of the step (3) of claim 1, wherein the concentration of the aqueous solution of the lotus leaf flavone crude extract is 50-100 mg/m L, wet-process sample loading is carried out by taking AB-8 macroporous adsorption resin as a stationary phase, the sample loading amount is 0.5BV, the sample loading flow rate is 2-3 BV/h, gradient elution is carried out by 20%, 80% and 100% ethanol after static adsorption is carried out for 8-12 h, the elution volume is 3BV, the elution flow rate is 2-3 BV/h, and the 80% ethanol elution component is collected and concentrated to obtain the lotus leaf flavone component.
6. The preparation of the wall material solution according to the step (4) of claim 1, wherein the dextrose equivalent value of maltodextrin is 21, the maltodextrin, the egg white concentrated protein, and the fish gelatin are dissolved in warm water at 70 ℃ and at 120rpm for 1 hour, and then the soybean lecithin is added, the contents of maltodextrin, the egg white concentrated protein, the fish gelatin, and the soybean lecithin are respectively 38-42%, 8-10%, 4-5%, and 2%, and the concentration of the lotus leaf flavone is 45-55mg/m L.
7. The high-pressure homogenization technique as claimed in step (5) of claim 1, wherein the mass ratio of the lotus leaf flavone solution to the wall material solution is 1:5, the high-pressure homogenization pressure is 60Mpa, and the number of times of treatment is 2.
8. The spray drying technique of step (6) in claim 1, wherein the inlet air temperature of the spray drying is 170-180 ℃, the outlet air temperature is 60-70 ℃, and the flow rate is 15-25m L/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113100377A (en) * | 2021-04-20 | 2021-07-13 | 中国农业大学 | Method for preparing capsaicin microcapsule by microwave concentration modification synergistic spray embedding |
| CN113662191A (en) * | 2021-08-24 | 2021-11-19 | 安徽农业大学 | Preparation method of lecithin propolis alcohol extract double-wall nano-scale vegetable oil microcapsule |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1813710A (en) * | 2005-11-16 | 2006-08-09 | 江南大学 | Method for preparing flavone aglycone micro capsule |
| CN102334685A (en) * | 2011-05-27 | 2012-02-01 | 陕西科技大学 | Preparation method of buckwheat flavone microcapsule and its product |
| CN103479731A (en) * | 2013-09-27 | 2014-01-01 | 徐君 | Method for extracting high-purity lotus leaf flavones |
| CN104342040A (en) * | 2014-10-09 | 2015-02-11 | 江西师范大学 | Preparation method of high-melt-temperature fish scale gelatin |
| CN105434539A (en) * | 2015-10-29 | 2016-03-30 | 中国药科大学 | Composition of lotus flavones |
| KR20180083697A (en) * | 2017-01-13 | 2018-07-23 | 주식회사 한국화장품제조 | Method for poducing microcapsule containing hyaluronic acid and oil with increased stability and microcapsule produced by the same method |
| CN109735590A (en) * | 2019-02-28 | 2019-05-10 | 江西师范大学 | A kind of preparation method of fish scale gelatin high antioxidant peptide |
| CN111374218A (en) * | 2020-05-06 | 2020-07-07 | 江西师范大学 | Method for rapidly improving surface activity of fish scale gelatin |
| CN111471307A (en) * | 2020-03-19 | 2020-07-31 | 江西师范大学 | Preparation method of degradable collagen packaging material |
-
2020
- 2020-05-06 CN CN202010373788.6A patent/CN111387477A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1813710A (en) * | 2005-11-16 | 2006-08-09 | 江南大学 | Method for preparing flavone aglycone micro capsule |
| CN102334685A (en) * | 2011-05-27 | 2012-02-01 | 陕西科技大学 | Preparation method of buckwheat flavone microcapsule and its product |
| CN103479731A (en) * | 2013-09-27 | 2014-01-01 | 徐君 | Method for extracting high-purity lotus leaf flavones |
| CN104342040A (en) * | 2014-10-09 | 2015-02-11 | 江西师范大学 | Preparation method of high-melt-temperature fish scale gelatin |
| CN105434539A (en) * | 2015-10-29 | 2016-03-30 | 中国药科大学 | Composition of lotus flavones |
| KR20180083697A (en) * | 2017-01-13 | 2018-07-23 | 주식회사 한국화장품제조 | Method for poducing microcapsule containing hyaluronic acid and oil with increased stability and microcapsule produced by the same method |
| CN109735590A (en) * | 2019-02-28 | 2019-05-10 | 江西师范大学 | A kind of preparation method of fish scale gelatin high antioxidant peptide |
| CN111471307A (en) * | 2020-03-19 | 2020-07-31 | 江西师范大学 | Preparation method of degradable collagen packaging material |
| CN111374218A (en) * | 2020-05-06 | 2020-07-07 | 江西师范大学 | Method for rapidly improving surface activity of fish scale gelatin |
Non-Patent Citations (6)
| Title |
|---|
| 俞邱豪，等: "类黄酮微胶囊技术及其在食品工业中的应用进展", 《中国食品学报》 * |
| 李双，等: "鱼明胶提取及其品质影响因素", 《食品与发酵工业》 * |
| 李妍，等: "荷叶总黄酮的微胶囊化研究", 《怀化学院学报》 * |
| 涂宗财，等: "鱼鳞明胶的泡沫性能", 《食品与发酵工业》 * |
| 邓源喜，等: "荷叶中黄酮提取及测定方法的研究进展", 《饲料研究》 * |
| 马铁铮，等: "复合凝聚法制备脂溶性食品配料微胶囊的壁材研究进展", 《食品工业科技》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113100377A (en) * | 2021-04-20 | 2021-07-13 | 中国农业大学 | Method for preparing capsaicin microcapsule by microwave concentration modification synergistic spray embedding |
| CN113662191A (en) * | 2021-08-24 | 2021-11-19 | 安徽农业大学 | Preparation method of lecithin propolis alcohol extract double-wall nano-scale vegetable oil microcapsule |
| CN113662191B (en) * | 2021-08-24 | 2023-04-18 | 安徽农业大学 | Preparation method of lecithin propolis alcohol extract double-wall nano-scale vegetable oil microcapsule |
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