CN105248460A - Compound antimicrobial composition containing microcapsules and preparation method and application of compound antimicrobial composition - Google Patents
Compound antimicrobial composition containing microcapsules and preparation method and application of compound antimicrobial composition Download PDFInfo
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Abstract
The invention discloses a compound antimicrobial composition containing microcapsules and a preparation method and application of the compound antimicrobial composition. The method includes the steps of firstly, homogenizing and evenly mixing folium artemisiae argyi essential oil, pogostemon cablin essential oil, fennel fruit essential oil and emulgator to obtain emulsified liquid I; secondly, dissolving tremella heteropolysaccharide and pectin in water, adding the emulsified liquid I to the mixture at the temperature of 45-50 DEG C, and evenly mixing the mixture to obtain emulsified liquid II; thirdly, dissolving polyamino acid in water, and dropwise adding the emulsified liquid II at the temperature of 65-75 DEG C in the stirring state; fourthly, continuing to conduct heat preservation and heating after the emulsified liquid II is dropwise added; fifthly, lowering the temperature to 40-45 DEG C, adding polyhydric alcohol, stabilizer and bispyrithione dispersion liquid, and conducting even stirring to obtain the compound antimicrobial composition containing microcapsules. The compound antimicrobial composition has the advantages of having the broad-spectrum antibacterial capacity and being high in antibacterial property and stability, and the like, and the market application potential is large.
Description
Technical field
The present invention relates to household chemicals technical field, particularly a kind of composite antibacterial composition containing microcapsules and preparation method thereof and application.
Background technology
Antibacterial agent (Anti-bacterialagents) refers to and can within a certain period of time, make the growth of certain micro-organisms (bacterium, fungi, saccharomycete, algae and virus etc.) or breeding remain on necessary material below horizontal or product.Antibacterial agent is generally divided into inorganic antiseptic, organic antibacterial agent and natural antibacterial agent.
In household chemicals field, the antibacterial agent mainly organic antibacterial agent of application, principal item has anilid class, imidazoles, thiazoles, isothiazolone derivative, quaternary ammonium salt, biguanides, phenols etc.But these antibacterial agents are poisonous, harmful or belong to specified risk material often.Especially in the product directly contacted with human body skin, require higher, the product that can select is also few.
In recent years, along with people are to the pay attention to day by day of safety, the natural antibacterial agent based on natural component obtains and develops faster.In this field, natural plant essential oils has had a lot of research as antibacterial agent, if publication number is relate to the preparation of a kind of lotus leaf/Pogostemon cablin composite essential oil microcapsules and its application in Haircare composition in the patent of invention of 103769019A and 103767967A; In the patent of invention of publication number 102274280A, relate to a kind of patchouli oil antibacterial microcapsule and the application in field of textiles thereof; A kind of Blumea oil antibacterial microcapsule and the application at field of textiles thereof is related in the patent of invention of patent No. ZL200910040420.1 and ZL200910040418.4; A kind of tea tree oil antibacterial microcapsule is related in the patent of invention of ZL201310047112.8.
Researcher of the present invention finds through large quantifier elimination, independent plants essential oil often exists " fence effect " as antibacterial agent, namely may have potent antibacterial action to the microorganism of certain kind, but reasonable antibacterial action is not just had to the microorganism of certain kind other; On the other hand, even if by complex technique, composite plant essential oil often produces the antibacterial effect that 1+1 is less than 2.In a word, natural plant essential oils antibacterial agent still has larger limitation, and mainly antibacterial ability is limited, and sterilizing rate is low, without broad-spectrum long-acting etc.
Summary of the invention
Primary and foremost purpose of the present invention is that the shortcoming overcoming prior art natural plant essential oils antibacterial agent is with not enough, provides a kind of preparation method of the composite antibacterial composition containing microcapsules.
Another object of the present invention is to provide the composite antibacterial composition containing microcapsules obtained by above-mentioned preparation method.
Another object of the present invention is the application providing the described composite antibacterial composition containing microcapsules.
Object of the present invention is achieved through the following technical solutions: a kind of preparation method of the composite antibacterial composition containing microcapsules, comprises the steps:
(1) 0.1 ~ 0.2 mass parts P-Cymene, 0.2 ~ 0.4 mass parts Pogostemon cablin essential and 0.4 ~ 0.7 mass parts Fructus Foeniculi quintessence oil are added in 2 ~ 3 mass parts emulsifier, homogeneous, for subsequent use;
(2) the different poly-polysaccharide of 0.5 ~ 1 mass parts white fungus and 1 ~ 2 mass parts pectin being joined 50 mass parts temperature is in the water of 65 ~ 85 DEG C, is stirred to the different glycan of white fungus and pectin dissolves completely; Be cooled to 45 ~ 50 DEG C, add the solution that step (1) finally obtains, stir, for subsequent use;
(3) 0.3 ~ 0.8 mass parts polyaminoacid is dissolved in 50 mass parts water, is stirred to polyaminoacid and dissolves completely; Be warming up to 65 ~ 75 DEG C, under stirring, be added dropwise to the solution that step (2) obtains; After dropwising, continue insulated and stirred;
(4) solution that step (3) obtains is cooled to 40 ~ 45 DEG C, add 3 ~ 8 mass parts polyalcohols successively, 0.5 ~ 1.5 mass parts stabilizing agent, 20 ~ 40 mass parts concentration be 2% Bispyrithione dispersion liquid, stir, obtain a kind of composite antibacterial composition containing microcapsules.
P-Cymene described in step (1), described Pogostemon cablin essential and described Fructus Foeniculi quintessence oil, be all delicatessen food level or cosmetics-stage commodity.
Emulsifier described in step (1) is at least one in laruyl alcohol phosphate, C9-15 alcohol phosphate, stearyl alcohol phosphate and C20-22 alcohol phosphate, is all commercial cosmetic products contain level commodity.
The condition of the homogeneous described in step (1) is preferably 3000 ~ 5000rpm homogeneous, 15 ~ 30min.
The different poly-Polyose extraction of white fungus described in step (2) is in white fungus, and relative molecular mass is about 8.0 × 10
5, be delicatessen food level or cosmetics-stage commodity.
Pectin described in step (2) is the one in Sugar beet pectin or citrus pectin.
The condition stirred that is stirred to during the different glycan of white fungus and pectin dissolve completely described in step (2) is preferably 200 ~ 400rpm and stirs 10 ~ 20min.
The condition of the middle stirring that stirs described in step (2) is preferably 300 ~ 600rpm and stirs 30 ~ 45min.
Polyaminoacid described in step (3) is at least one in polylysine, polyglutamic acid and poly-aspartate.
The temperature of the water described in step (3) is preferably 20 ~ 25 DEG C.
The condition stirred that is stirred to during polyaminoacid dissolves completely described in step (3) is preferably 200 ~ 400rpm stirring, 10 ~ 20min.
Described in step (3) under stirring in mixing speed be preferably 300 ~ 600rpm.
The time of the dropping described in step (3) is preferably 45 ~ 60min.
The time of the continuation insulated and stirred described in step (3) is preferably 30 ~ 45min.
Stabilizing agent described in step (4) is at least one in sodium phosphate trimer, calgon, sodium pyrophosphate, tertiary sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, SAPP and Sodium Acid Pyrophosphate, is all analytical reagent.
Polyalcohol described in step (4) is at least one in 1,2-pentanediol, 1,2-ethohexadiol and Sensiva SC50, is all commercial cosmetic products contain level commodity.
Bispyrithione dispersion liquid described in step (4), from commercially available, is mainly used in the auxiliary antibacterial, antibacterial of fabric, and activity concentration is 2.0%.
The speed of the stirring described in step (4) is preferably 200 ~ 400rpm.
A composite antibacterial composition containing microcapsules, is obtained by above-mentioned preparation method.
The described composite antibacterial composition containing microcapsules is applied in household chemicals field.
The present invention has following advantage and effect relative to prior art:
(1) tarragon, Pogostemon cablin and Fructus Foeniculi volatile oil are natural plants essential oils, have certain antibacterial, disinfective action, by compound, obtain composite essential oil, can play synergy, promote antibacterial effect.
(2) microcapsules technology is adopted, tarragon, Pogostemon cablin and fennel seeds compound volatile oil are made microcapsules, and with there is polyalcohols and the Bispyrithione compound of fungistatic effect, obtain the composite antibacterial composition containing microcapsules, the defect of current natural plant essential oils antibacterial agent can be overcome.
(3) the present invention is with the different poly-polysaccharide of white fungus, pectin, polyaminoacid for wall material, by microencapsulation process, compound volatile oil is made volatile oil microcapsule, improves the stability of essential oil on the one hand, indirectly extends the time of antibacterial action on the other hand.
(4) by optimizing the ratio of the different poly-polysaccharide of white fungus, pectin, polyaminoacid, the microcapsule wall material of better effects is obtained.Microcapsules directly present in the form of an emulsion, and without the need to adopting the crosslinking agent of aldehydes, degree of scatter is better, and particle diameter is about 0.5 ~ 5.0 μm, and stability is also better.
Accompanying drawing explanation
Fig. 1 is the microphotograph figure of the composite antibacterial composition containing microcapsules that embodiment prepares.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
(I) by (commercially available for 0.1 mass parts P-Cymene, food-grade or cosmetics-stage, down together), 0.2 mass parts Pogostemon cablin essential is (commercially available, food-grade or cosmetics-stage, lower same) and 0.7 mass parts Fructus Foeniculi quintessence oil (commercially available, food-grade or cosmetics-stage, add down together) 2 mass parts laruyl alcohol phosphates (commercially available, cosmetics-stage) in, 3000rpm homogeneous 15min, for subsequent use.
(II) by (commercially available for the different poly-polysaccharide of 0.5 mass parts white fungus, food-grade or cosmetics-stage, lower with), 1 mass parts citrus pectin (commercially available, food-grade or cosmetics-stage, lower with) to join 50 mass parts temperature be successively in the water of 65 DEG C, 200rpm stirs 10min, the different poly-polysaccharide of white fungus and pectin dissolve completely, are cooled to 45 DEG C, add the solution that step (I) obtains, 300rpm stirs 30min, for subsequent use.
(III) by 0.3 mass parts polylysine (commercially available, cosmetics-stage, lower with) be dissolved in the water of 50 mass parts 20 DEG C, 200rpm stirs 10min, and polylysine dissolves completely; Be warming up to 65 DEG C, stir with the speed of 300rpm, be slowly added dropwise to the solution that step (II) obtains, 45min dropwises.After dropwising, continue insulated and stirred 30min.
(IV) solution that step (III) obtains is cooled to 40 DEG C, add 3 mass parts 1 successively, 2-pentanediol is (commercially available, cosmetics-stage), 0.5 mass parts calgon is (commercially available, analyze pure), 20 mass parts Bispyrithione dispersion liquids (purchase from Guangzhou Run Pusen Chemical Industry Science Co., Ltd, trade names: Sentex
tMtBS, lower same), 200rpm stirs, and obtains a kind of composite antibacterial composition 1 containing microcapsules.
With the distribution of microcapsules in biology microscope sem observation composite antibacterial composition 1, as shown in Figure 1, the particle diameter of microcapsules is about 3.0 μm, and degree of scatter is higher.
Embodiment 2
(I) 0.2 mass parts P-Cymene, 0.4 mass parts Pogostemon cablin essential and 0.4 mass parts Fructus Foeniculi quintessence oil are added in 3 mass parts emulsifier (stearyl alcohol phosphate), 5000rpm homogeneous 30min, for subsequent use.
(II) the different poly-polysaccharide of 1 mass parts white fungus, 2 mass parts pectin being joined 50 mass parts temperature is successively in the water of 85 DEG C, 400rpm stirs 20min, the different poly-polysaccharide of white fungus and pectin dissolve completely, be cooled to 50 DEG C, add step (I) solution, 600rpm stirs 45min, for subsequent use.
(III) be dissolved in by 0.8 mass parts polyglutamic acid in the water of 50 mass parts 25 DEG C, 400rpm stirs 20min, and polyglutamic acid dissolves completely; Be warming up to 75 DEG C, stir with 600rpm, be slowly added dropwise to the solution that step (II) obtains, 60min dropwises.After dropwising, continue insulated and stirred 45min.
(IV) solution that step (III) obtains is cooled to 45 DEG C, add 8 mass parts 1 successively, 2-ethohexadiol, 1.5 mass parts tertiary sodium phosphates, 40 mass parts Bispyrithione dispersion liquids, 400rpm stirs, and obtains a kind of composite antibacterial composition 2 containing microcapsules.
With the distribution of microcapsules in biology microscope sem observation composite antibacterial composition 2, particle diameter is about 0.5 μm, and degree of scatter is higher.
Embodiment 3
(I) 0.15 mass parts P-Cymene, 0.3 mass parts Pogostemon cablin essential and 0.55 mass parts Fructus Foeniculi quintessence oil are added in 2.5 mass parts emulsifier (C20-22 alcohol phosphate), 4500rpm homogeneous 20min, for subsequent use.
(II) the different poly-polysaccharide of 0.75 mass parts white fungus, 1.5 mass parts pectin being joined 50 mass parts temperature is successively in the water of 70 DEG C, 300rpm stirs 15min, the different poly-polysaccharide of white fungus and pectin dissolve completely, be cooled to 48 DEG C, add step (I) solution, 450rpm stirs 40min, for subsequent use.
(III) be dissolved in by 0.5 mass parts poly-aspartate in the water of 50 mass parts 23 DEG C, 300rpm stirs 15min, and poly-aspartate dissolves completely; Be warming up to 70 DEG C, stir with 450rpm, be slowly added dropwise to the solution that step (II) obtains, 50min dropwises.After dropwising, continue insulated and stirred 40min.
(IV) solution that step (III) obtains is cooled to 43 DEG C, add 0.5 mass parts 1 successively, 2-ethohexadiol, 5 mass parts Sensiva SC50s, 0.5 mass parts calgon, 0.5 mass parts sodium pyrophosphate, 30 mass parts Bispyrithione dispersion liquids, 300rpm stirs, and obtains a kind of composite antibacterial composition 3 containing microcapsules.
With the distribution of microcapsules in biology microscope sem observation composite antibacterial composition 3, particle diameter is about 5.0 μm, and degree of scatter is higher.
Embodiment 4
(I) 0.12 mass parts P-Cymene, 0.25 mass parts Pogostemon cablin essential and 0.63 mass parts Fructus Foeniculi quintessence oil are added in 2.2 mass parts emulsifier (C9-15 alcohol phosphate), 4000rpm homogeneous 30min, for subsequent use.
(II) the different poly-polysaccharide of 1 mass parts white fungus and 1 mass parts pectin being joined 50 mass parts temperature is successively in the water of 85 DEG C, 200rpm stirs 20min, the different poly-polysaccharide of white fungus and pectin dissolve completely, be cooled to 48 DEG C, add step (I) solution, 600rpm stirs 35min, for subsequent use.
(III) join in the water of 50 mass parts 20 DEG C by 0.2 mass parts polylysine and 0.2 mass parts poly-aspartate, 250rpm stirs 15min, and polylysine and poly-aspartate dissolve completely; Be warming up to 68 DEG C, stir with 300rpm, be slowly added dropwise to the solution that step (II) obtains, 45min dropwises.After dropwising, continue insulated and stirred 35min.
(IV) solution that step (III) obtains is cooled to 45 DEG C, add 8 mass parts 1 successively, 2-pentanediol, 1.5 mass parts calgons, 35 mass parts Bispyrithione dispersion liquids, 200rpm stirs, and obtains a kind of composite antibacterial composition 4 containing microcapsules.
With the distribution of microcapsules in biology microscope sem observation composite antibacterial composition 4, particle diameter is about 3.0 μm, and degree of scatter is higher.
Comparative example 1 ~ 3
The bactericidal composition of preparation containing P-Cymene microcapsules, the bactericidal composition containing Pogostemon cablin essential microcapsules and the bactericidal composition containing Fructus Foeniculi volatile oil microcapsules, respectively called after comparison 1 ~ 3 respectively.
Preparation process, substantially with embodiment 1, is distinguished as follows: preparation is add 0.1 mass parts P-Cymene in step (I) containing the bactericidal composition of P-Cymene microcapsules, does not add other essential oils; Preparation just adds 0.2 mass parts Pogostemon cablin essential containing the bactericidal composition of Pogostemon cablin essential microcapsules; Preparation just adds 0.7 mass parts Fructus Foeniculi quintessence oil containing the bactericidal composition of Fructus Foeniculi volatile oil microcapsules.
Comparative example 4
The solution that embodiment 1 step (III) obtains is cooled to 40 DEG C, and add 0.5 mass parts calgon, 200rpm stirs, and obtains composite essential oil microcapsule emulsion (called after comparison 4).
Comparative example 5
Preparation process is substantially with embodiment 1, and difference is not add Bispyrithione dispersion liquid, the composite essential oil microcapsule emulsion called after comparison 5 obtained.
Comparative example 6
Preparation process is substantially with embodiment 1, and difference is not add polyalcohol, the composite essential oil microcapsule emulsion called after comparison 6 obtained.
Comparative example 7
By the Bispyrithione dispersion liquid of 2% as comparison 7.
Comparative example 8
In embodiment 1, the ratio of the different poly-polysaccharide of adjustment white fungus, pectin, polyaminoacid, is respectively the different poly-polysaccharide of 2 mass parts white fungus, 0.5 mass parts pectin, 1 mass parts polyaminoacid, the composite essential oil microcapsule emulsion called after comparison 8 obtained.
Measure of merit example
1, stability test
(1) stability of study group's compound 1 ~ 4.
Organoleptic properties: visual observations under room temperature and non-direct sunlight of materialsing.
Heat-resistant stability: pour sample into 2 respectively
in vitro, make liquid level be about 80mm, clean plug beyond the Great Wall, a test tube to be checked is placed in the constant incubator being adjusted to (40 ± 1) DEG C in advance.Take out after 24h, carry out range estimation with the sample of another test tube after returning to room temperature and compare.
Cold-resistant stability: pour sample into 2 respectively
in vitro, make liquid level be about 80mm, clean plug beyond the Great Wall, a test tube to be checked is placed in the refrigerator being adjusted to-5 DEG C ~-10 DEG C in advance.Take out after 24h, carry out range estimation with the sample of another test tube after returning to room temperature and compare.
(2) stability test result is as shown in table 1: the heat-resisting and cold-resistant stability of composition 1 ~ 4, comparative example 1 ~ 7 is all up to standard; And have changed the comparative example 8 of wall material ratio, layering is serious.
Table 1 stability test result
| Project | Composition 1 ~ 4 | Comparison 1 ~ 7 | Comparison 8 |
| Organoleptic indicator | Have no layering, evenly | Have no layering, evenly | Slight layering |
| Heat-resistant stability | Stable | Stable | Layering is serious |
| Cold-resistant stability | Stable | Stable | Layering is serious |
2, antibacterial experiment
(1) testing bacterial classification is colon bacillus (Escherichiacoli, ATCC8739), staphylococcus aureus (Staphylococcusaureus, ATCC6538), pseudomonas aeruginosa (Pseudomonasaeruginosa, ATCC9027), candida albicans (Candidaalbicans, ATCC10231), aspergillus niger (Aspergillusniger, ATCC16404), Guangdong Microbes Inst DSMZ is all derived from.
(2) detection method: with reference to American Pharmacopeia USP32<51> antimicrobial preservation efficacy test.
(3) testing result is as shown in table 2 ~ 3.As can be seen from the anti-bacterial result of table 2, the composite antibacterial composition containing microcapsules shows good antibacterial ability, and shows good broad-spectrum sterilization, bacteriostasis.As can be seen from the anti-bacterial result of table 3, composite antibacterial composition (comparison 1 ~ 3) antibacterial effect containing single essential oil microcapsules is weaker than composite essential oil, this demonstrate the composite essential oil obtained through rational proportion compound by P-Cymene, Pogostemon cablin essential and Fructus Foeniculi volatile oil, there is good synergistic function; The anti-bacterial result of comparison 4 ~ 7 is also weaker than composite antibacterial composition, illustrates also have Synergistic between bactericidal composition; And change the comparison 8 that wall material ratio obtains, due to stability not, substantially not there is antibacterial ability.
Table 2 composition 1 ~ 4 anti-bacteria test result
Table 3 comparison 1 ~ 8 anti-bacteria test result
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a preparation method for the composite antibacterial composition containing microcapsules, is characterized in that comprising the steps:
(1) 0.1 ~ 0.2 mass parts P-Cymene, 0.2 ~ 0.4 mass parts Pogostemon cablin essential and 0.4 ~ 0.7 mass parts Fructus Foeniculi quintessence oil are added in 2 ~ 3 mass parts emulsifier, homogeneous, for subsequent use;
(2) the different poly-polysaccharide of 0.5 ~ 1 mass parts white fungus and 1 ~ 2 mass parts pectin being joined 50 mass parts temperature is in the water of 65 ~ 85 DEG C, is stirred to the different glycan of white fungus and pectin dissolves completely; Be cooled to 45 ~ 50 DEG C, add the solution that step (1) finally obtains, stir, for subsequent use;
(3) 0.3 ~ 0.8 mass parts polyaminoacid is dissolved in 50 mass parts water, is stirred to polyaminoacid and dissolves completely; Be warming up to 65 ~ 75 DEG C, under stirring, be added dropwise to the solution that step (2) obtains; After dropwising, continue insulated and stirred;
(4) solution that step (3) obtains is cooled to 40 ~ 45 DEG C, add 3 ~ 8 mass parts polyalcohols successively, 0.5 ~ 1.5 mass parts stabilizing agent, 20 ~ 40 mass parts concentration be 2% Bispyrithione dispersion liquid, stir, obtain a kind of composite antibacterial composition containing microcapsules.
2. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that: the emulsifier described in step (1) is at least one in laruyl alcohol phosphate, C9-15 alcohol phosphate, stearyl alcohol phosphate and C20-22 alcohol phosphate.
3. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that: the polyaminoacid described in step (3) is at least one in polylysine, polyglutamic acid and poly-aspartate.
4. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that: the stabilizing agent described in step (4) is at least one in sodium phosphate trimer, calgon, sodium pyrophosphate, tertiary sodium phosphate, sodium hydrogen phosphate, sodium dihydrogen phosphate, SAPP and Sodium Acid Pyrophosphate.
5. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that: the polyalcohol described in step (4) is at least one in 1,2-pentanediol, 1,2-ethohexadiol and Sensiva SC50.
6. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that:
The relative molecular mass of the different poly-polysaccharide of the white fungus described in step (2) is 8.0 × 10
5;
Pectin described in step (2) is the one in Sugar beet pectin or citrus pectin.
7. the preparation method of the composite antibacterial composition according to claim 1 containing microcapsules, is characterized in that:
The condition of the homogeneous described in step (1) is 3000 ~ 5000rpm homogeneous, 15 ~ 30min;
The condition stirred that is stirred to during the different glycan of white fungus and pectin dissolve completely described in step (2) is that 200 ~ 400rpm stirs 10 ~ 20min;
The condition of the middle stirring that stirs described in step (2) is that 300 ~ 600rpm stirs 30 ~ 45min;
The condition stirred that is stirred to during polyaminoacid dissolves completely described in step (3) is that 200 ~ 400rpm stirs 10 ~ 20min;
Described in step (3) under stirring in mixing speed be 300 ~ 600rpm;
The time of the dropping described in step (3) is 45 ~ 60min;
The time of the continuation insulated and stirred described in step (3) is 30 ~ 45min;
The speed of the stirring described in step (4) is 200 ~ 400rpm.
8. the composite antibacterial composition containing microcapsules, is characterized in that being obtained by the preparation method described in any one of claim 1 ~ 7.
9. the composite antibacterial composition containing microcapsules according to claim 8 is applied in household chemicals field.
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