CN102885379B - Preparation method of dual bacteriostatic cinnamyl aldehyde microcapsule - Google Patents
Preparation method of dual bacteriostatic cinnamyl aldehyde microcapsule Download PDFInfo
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- CN102885379B CN102885379B CN2012103713425A CN201210371342A CN102885379B CN 102885379 B CN102885379 B CN 102885379B CN 2012103713425 A CN2012103713425 A CN 2012103713425A CN 201210371342 A CN201210371342 A CN 201210371342A CN 102885379 B CN102885379 B CN 102885379B
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Abstract
The invention discloses a preparation method of a dual bacteriostatic cinnamyl aldehyde microcapsule, which comprises the following steps of: dissolving chitosan in glacial acetic acid to prepare chitosan solution; adding cellulose and performing enzymolysis reaction to obtain modified chitosan solution; dissolving Arabic gum in water to prepare Arabic gum solution; adding cinnamyl aldehyde, and emulsifying and dispersing at high speed to obtain emulsion; dropwise adding the modified chitosan solution into the emulsion, performing coagulation reaction, adding geniposide, and solidifying; and leaching, drying, and thus obtaining the dual bacteriostatic cinnamyl aldehyde microcapsule. The preparation method has the advantages that cinnamyl aldehyde bacteriostatic component loss is reduced, irritation and spicy of cinnamyl are covered, and cinnamyl aldehyde is slowly released in high-temperature and high-humidity environments; the modified chitosan and cinnamyl aldehyde simultaneously have dual bacteria-resistant effects, and can generate a good bacteria-resistant effect when added into a minced fish product; bacteria-resistant concentration is low, the lowest bacteria-resistant concentration of Escherichia coli can reach 0.10 percent, and the lowest bacteria-resistant concentration of staphylococcus aureus can reach 0.15 percent.
Description
Technical field
The present invention relates to a kind of preparation method of cinnamic acid microcapsules, particularly a kind of preparation method of dual antibacterial cinnamic acid microcapsules.
Background technology
Cinnamic acid is a kind of aldehydes organic compound, is the sticky shape liquid of yellow, is present in a large number in the plants such as Chinese cassia tree, has strong cassia oil and the fragrance of cinnamon oil, without pungent.Cinnamic acid has very strong inhibition and killing action to various fungies, mould, especially better to fungistatic effects such as aspergillus flavus, aspergillus niger, Penicillium citrinum, fusarium moniliforme, Alternaria, geotrichum candidum, yeast, can prevent food spoilage, cooling meat is had to obvious preservation, can make freshness date extend about 15 days, have advantages of that consumption is few, cost is low, have no side effect.But cinnamic acid is insoluble in water, volatile, easily oxidized, is difficult for carrying out preservation, and has the fragrant hot flavor of strong impulse, thereby has affected its result of use.Adopt microcapsules technology that cinnamic acid is wrapped up, not only can effectively delay the release of cinnamic acid, also can change fat-soluble cinnamic acid into the pressed powder state, thereby enlarge its range of application in food industry.
At present; the most frequently used microcapsules technology of food industry is spray drying process; but adopt microcapsules prepared by spray drying process very unstable under the processing of high temperature, high humidity or holding conditions; the cyst wall of its glassy state very easily water absorption and swelling breaks; cause the release of core; can not protect well cinnamic acid, bring into play the effect of its long-acting bacteriostatic.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of dual antibacterial cinnamic acid microcapsules, and these dual antibacterial cinnamic acid microcapsules can slowly discharge cinnamic acid in high temperature, high humidity environment, to guarantee the long-acting bacteriostatic effect of cinnamic acid.
Technical solution of the present invention is:
A kind of preparation method of dual antibacterial cinnamic acid microcapsules, its concrete steps are:
1) shitosan being dissolved in to preparation quality percentage composition in glacial acetic acid is 0.5%～2.0% chitosan solution, add cellulase, described cellulase is 1:1～1:6 with the chitosan mass ratio, the enzyme of cellulase is lived as 500U/mg～2000U/mg, under 40 ℃～60 ℃, carry out enzyme digestion reaction 1h～4h, obtain modification of chitosan solution;
2) by Arabic gum preparation quality soluble in water percentage composition, being 0.5%～1.0% gumwater, is that 1:0.5～1:4 adds cinnamic acid according to the mass ratio with Arabic gum and shitosan gross mass, and emulsify at a high speed disperses, and obtains emulsion;
3) in emulsion, drip modification of chitosan solution, wherein, the mass ratio of Arabic gum and shitosan is 5:1～8:1, under 30 ℃～50 ℃, carries out aggregation 10min～30min; After aggregation, add Gardenoside, the mass ratio of described Gardenoside and shitosan is 1:0.25～1:4, at room temperature, is cured 1h～4h;
4) after solidifying, carry out suction filtration, obtain wet dual antibacterial cinnamic acid microcapsules, drying, obtain dual antibacterial cinnamic acid microcapsules.
The mass concentration of described glacial acetic acid is 1.0%～3.0%.
When emulsify at a high speed disperseed, emulsifying rate was 8000 rpm～12000 rpm, and the time is 3 min～5min.
When dry, adopt spray-drying, EAT is 180 ℃～220 ℃, and leaving air temp is 80 ℃～100 ℃.
The present invention is usingd Arabic gum and modification of chitosan as the wall material, with Arabic gum and modification of chitosan, by complex coacervation, cinnamic acid is wrapped up, and prepares dual antibacterial cinnamic acid microcapsules.Its beneficial effect is:
1, solved the too fast problem of cinnamic acid volatilization in the storage process, reduced the loss of cinnamic acid antipathogenic composition, and the fragrant hot flavor of the excitant of having sheltered cinnamic acid, the dual antibacterial cinnamic acid microcapsules of preparation can slowly discharge cinnamic acid in high temperature, high humidity environment.
2, by enzymatic hydrolysis, carry out modification of chitosan, can make the Chitosan Reducing molecular weight, reduce viscosity, improve solubility, be conducive to modification of chitosan and by complex coacervation, prepare dual antibacterial cinnamic acid microcapsules as the wall material.
3, using modification of chitosan as the wall material, with shitosan, compare and more easily form the microcapsules with spherical coenocytism; And modification of chitosan has antibacterial activity preferably, with cinnamic acid, can bring into play simultaneously dual bacteriostasis, is added in surimi product, can produce good fungistatic effect; Select in the wall material and do not contain gelatin, add in food, the Moslem also can eat.
4, the Mlc of dual antibacterial cinnamic acid microcapsules is low, to colibacillary minimum inhibitory concentration, can reach 0.10%, to the minimum inhibitory concentration of staphylococcus aureus, can reach 0.15%.
The accompanying drawing explanation
Fig. 1 is the microscope figure of dual antibacterial cinnamic acid microcapsules of the present invention.
The specific embodiment
Embodiment 1
1, the 3g shitosan being dissolved in to the 300g mass concentration is to prepare chitosan solution in 1.0% glacial acetic acid, adds 3g cellulase (enzyme live 500u/mg), under 40 ℃, carries out enzyme digestion reaction 4h, obtains modification of chitosan solution;
2, the 15g Arabic gum is dissolved in 2000ml water and prepares gumwater, add the 9g cinnamic acid, under 10000 rpm emulsifying rates, emulsify at a high speed disperses 4min, obtains emulsion;
3, the modification of chitosan solution that step 1 is made drops in the emulsion that step 2 makes (mass ratio of Arabic gum and shitosan is 1:4), at 30 ℃ of lower constant temperature, stirs 30min, carries out aggregation; After aggregation, add the 0.75g Gardenoside, at room temperature be cured 1h;
4, after solidifying, carry out suction filtration, obtain wet dual antibacterial cinnamic acid microcapsules, adopt spray-drying, EAT is 180 ℃, and leaving air temp is 80 ℃, and charging rate is 500ml/h, obtains dual antibacterial cinnamic acid microcapsules, as shown in Figure 1.
After testing, dual antibacterial cinnamic acid microcapsules are 0.10% to colibacillary minimum inhibitory concentration, to the minimum inhibitory concentration of staphylococcus aureus, are 0.15%.
Embodiment 2
1, the 0.75g shitosan being dissolved in to the 40g mass concentration is to prepare chitosan solution in 2.0% glacial acetic acid, adds 0.5g cellulase (enzyme live 2000u/mg), under 60 ℃, carries out enzyme digestion reaction 1h, obtains modification of chitosan solution;
2, the 6g Arabic gum is dissolved in 600ml water and prepares gumwater, add the 13.5g cinnamic acid, under the 8000rpm emulsifying rate, emulsify at a high speed disperses 3min, obtains emulsion;
3, the modification of chitosan solution that step 1 is made drops in the emulsion that step 2 makes (mass ratio of Arabic gum and shitosan is 1:0.25), at 40 ℃ of lower constant temperature, stirs 20min, carries out aggregation; After aggregation, add the 3.0g Gardenoside, at room temperature be cured 4h;
4, after solidifying, carry out suction filtration, obtain wet dual antibacterial cinnamic acid microcapsules, adopt spray-drying, EAT is 220 ℃, and leaving air temp is 100 ℃, and charging rate is 500ml/h, obtains dual antibacterial cinnamic acid microcapsules.
After testing, dual antibacterial cinnamic acid microcapsules are 0.25% to colibacillary minimum inhibitory concentration, to the minimum inhibitory concentration of staphylococcus aureus, are 0.35%.
Embodiment 3
1, the 3g shitosan being dissolved in to the 600g mass concentration is to prepare chitosan solution in 3.0% glacial acetic acid, adds 1g cellulase (enzyme live 1400u/mg), under 50 ℃, carries out enzyme digestion reaction 3h, obtains modification of chitosan solution;
2, the 18g Arabic gum is dissolved in 3600ml water and prepares gumwater, add the 5.25g cinnamic acid, under the 12000rpm emulsifying rate, emulsify at a high speed disperses 5min, obtains emulsion;
3, the modification of chitosan solution that step 1 is made drops in the emulsion that step 2 makes (mass ratio of Arabic gum and shitosan is 1:1), at 50 ℃ of lower constant temperature, stirs 10min, carries out aggregation; After aggregation, add the 3g Gardenoside, at room temperature be cured 2h;
4, after solidifying, carry out suction filtration, obtain wet dual antibacterial cinnamic acid microcapsules, adopt spray-drying, EAT is 200 ℃, and leaving air temp is 90 ℃, and charging rate is 500ml/h, obtains dual antibacterial cinnamic acid microcapsules.
After testing, dual antibacterial cinnamic acid microcapsules are 0.20% to colibacillary minimum inhibitory concentration, to the minimum inhibitory concentration of staphylococcus aureus, are 0.25%.
Claims (4)
1. the preparation method of dual antibacterial cinnamic acid microcapsules is characterized in that concrete steps are as follows:
1.1 it is 0.5%～2.0% chitosan solution that shitosan is dissolved in to preparation quality percentage composition in glacial acetic acid, add cellulase, described cellulase is 1:1～1:6 with the chitosan mass ratio, the enzyme of cellulase is lived as 500U/mg～2000U/mg, under 40 ℃～60 ℃, carry out enzyme digestion reaction 1h～4h, obtain modification of chitosan solution;
1.2 by Arabic gum preparation quality soluble in water percentage composition, be 0.5%～1.0% gumwater, according to the mass ratio with Arabic gum and shitosan gross mass, be that 1:0.5～1:4 adds cinnamic acid, emulsify at a high speed disperses, and obtains emulsion;
1. 3 in emulsion, drip modification of chitosan solution, wherein, the mass ratio of Arabic gum and shitosan is 5:1～8:1, under 30 ℃～50 ℃, carries out aggregation 10min～30min; After aggregation, add Gardenoside, the mass ratio of described Gardenoside and shitosan is 1:0.25～1:4, at room temperature, is cured 1h～4h;
1.4, after solidifying, carry out suction filtration, obtain wet dual antibacterial cinnamic acid microcapsules, drying, obtain dual antibacterial cinnamic acid microcapsules.
2. the preparation method of dual antibacterial cinnamic acid microcapsules according to claim 1, it is characterized in that: the mass concentration of described glacial acetic acid is 1.0%～3.0%.
3. the preparation method of dual antibacterial cinnamic acid microcapsules according to claim 1 is characterized in that: when emulsify at a high speed disperseed, emulsifying rate was 8000rpm～12000rpm, and the time is 3min～5min.
4. the preparation method of dual antibacterial cinnamic acid microcapsules according to claim 1 is characterized in that: when dry, adopt spray-drying, EAT is 180 ℃～220 ℃, and leaving air temp is 80 ℃～100 ℃.
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| CN104138356A (en) * | 2013-05-09 | 2014-11-12 | 烟台职业学院 | Cinnamaldehyde crosslinked chitosan drug-loading microsphere preparation method |
| CN104042719B (en) * | 2014-07-07 | 2016-04-27 | 江苏瑞京科技发展有限公司 | A kind of antibacterial modified chitosan spray and preparation method thereof |
| CN104472646B (en) * | 2014-11-10 | 2018-02-09 | 天津科技大学 | A kind of preparation method of Nisin bilayered microcapsules suitable for high temperature bakery |
| CN106467619B (en) * | 2016-09-29 | 2019-05-28 | 山东师范大学 | A kind of preparation method of controlled degradation O- carboxymethyl cinnamic acid modified chitosan anti-bacteria film |
| CN111904948B (en) * | 2020-07-08 | 2022-08-19 | 中国农业科学院农业环境与可持续发展研究所 | Preparation method of cinnamaldehyde nano microsphere suspending agent |
| CN114916658B (en) * | 2022-05-06 | 2023-07-28 | 江南大学 | Method for prolonging high-quality shelf life of low-salt conditioned edible fungi |
| CN115260652A (en) * | 2022-08-16 | 2022-11-01 | 江西同益高分子材料科技有限公司 | High-performance antibacterial PP (polypropylene) plate and preparation method thereof |
| CN115868541A (en) * | 2022-12-22 | 2023-03-31 | 黑龙江辰鹰乳业有限公司 | Formula liquid milk suitable for infants of 12-36 months old and preparation method thereof |
| CN117771175A (en) * | 2024-02-23 | 2024-03-29 | 中国农业科学院农业环境与可持续发展研究所 | Enrofloxacin nano suspension and preparation method and application thereof |
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