CN114177847A - Plant essential oil microcapsule and preparation method thereof - Google Patents
Plant essential oil microcapsule and preparation method thereof Download PDFInfo
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- CN114177847A CN114177847A CN202111484353.XA CN202111484353A CN114177847A CN 114177847 A CN114177847 A CN 114177847A CN 202111484353 A CN202111484353 A CN 202111484353A CN 114177847 A CN114177847 A CN 114177847A
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- essential oil
- plant essential
- cyclodextrin
- microcapsule
- wall material
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- 239000000341 volatile oil Substances 0.000 title claims abstract description 118
- 239000003094 microcapsule Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
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- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 42
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 39
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 38
- 239000000661 sodium alginate Substances 0.000 claims abstract description 38
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 38
- 229920001661 Chitosan Polymers 0.000 claims abstract description 34
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- 239000010410 layer Substances 0.000 claims abstract description 20
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- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
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- 125000000217 alkyl group Chemical group 0.000 claims description 3
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- 229940043377 alpha-cyclodextrin Drugs 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
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- ODLHGICHYURWBS-LKONHMLTSA-N trappsol cyclo Chemical compound CC(O)COC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](COCC(C)O)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)COCC(O)C)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1COCC(C)O ODLHGICHYURWBS-LKONHMLTSA-N 0.000 claims description 3
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
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- 238000004945 emulsification Methods 0.000 claims 1
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- 235000007866 Chamaemelum nobile Nutrition 0.000 description 4
- 244000042664 Matricaria chamomilla Species 0.000 description 4
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/025—Applications of microcapsules not provided for in other subclasses
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention provides a plant essential oil microcapsule and a preparation method thereof, and particularly relates to the technical field of spinning. The preparation method at least comprises the following steps: preparing a core material solution by using plant essential oil; preparing a wall material solution by using cyclodextrin; adding the core material solution into the wall material solution, homogenizing and emulsifying to obtain a cyclodextrin-coated single-layer microcapsule; and then the single-layer microcapsule is embedded for the second time by utilizing chitosan/sodium alginate to obtain the double-layer microcapsule. The preparation method is simple and low in cost. The plant essential oil microcapsule prepared by the invention has good embedding rate, effectively reduces the volatilization of essential oil, improves the stability of essential oil and prolongs the effect and action time.
Description
Technical Field
The invention relates to the technical field of spinning, in particular to a plant essential oil microcapsule and a preparation method thereof.
Background
In recent years, with the acceleration of life rhythm, the pressure of people is getting higher and higher, insomnia becomes a big problem troubling health, the insomnia rate of Chinese adults is up to 40% according to statistics, and long-term insomnia can make people not have effective rest, so that the physical quality is reduced, aging is accelerated, and various health hidden dangers are brought to the body.
Related researches at home and abroad show that aromatic odor of some plants such as lavender, chamomile, vanilla, valerian and the like has the effects of soothing nerves, protecting health, resisting bacteria and the like, so that the plant essential oil is widely applied to various industries such as food, daily chemicals, medicines, textiles and the like. However, the essential oil has the characteristics of unsaturated bonds, easy volatilization and the like, has short fragrance retention period, causes the defects of short fragrance retention time, uncontrollable release and the like, is inconvenient to store, transport, diversify in medicament dosage forms and the like, is easy to deteriorate under the influence of factors such as light, heat, air and the like, and limits the action effect and the application range of the essential oil.
The microcapsule technology is a technology for forming fine particles by coating a solid, liquid or gas with a polymer film-forming material. In order to maintain the relative stability of essential oils during transportation, storage and processing, microencapsulation is often employed to reduce the loss of essential oils. At present, wall materials are mostly used in the existing preparation method for preparing the essential oil microcapsules in a single embedding mode of essential oil, so that the product has certain stability under normal conditions, but the effect is still not ideal under special environments such as friction and heating. Especially in the field of textiles, the aromatic fabric prepared by processing the essential oil needs to be washed and dried in the using process, and in the period, the loss of fragrance is large due to the action of external force, so that the textile cannot play the expected effect after being used for a long time, and the requirements of people cannot be met. Therefore, there is a need to develop a plant essential oil microcapsule for textiles, which can still maintain a lasting fragrance function under the action of external forces such as washing, drying and the like.
Disclosure of Invention
In view of the defects of the prior art, the invention provides a plant essential oil microcapsule and a preparation method thereof, which aim to solve the problems that plant essential oil is unstable and cannot keep fragrance for a long time.
To achieve the above and other related objects, the present invention provides a method for preparing plant microcapsules, which comprises at least the following steps: preparing a core material solution by using plant essential oil; preparing a wall material solution by using cyclodextrin; adding the core material solution into the wall material solution, homogenizing and emulsifying to obtain a cyclodextrin-coated single-layer microcapsule; and carrying out secondary embedding on the single-layer microcapsule by utilizing chitosan/sodium alginate to obtain the double-layer microcapsule.
In one example of the present invention, the step of preparing the core material solution includes: uniformly mixing plant essential oil and absolute ethyl alcohol according to the mass ratio of 1 (2-5), adding lecithin into the mixed solution, and heating to completely dissolve the lecithin, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2.
In one example of the invention, the plant essential oil comprises one or more of lavender essential oil, chamomile essential oil, vanilla essential oil, and valerian essential oil.
In one example of the present invention, the step of preparing the wall material solution comprises: adding the prepared wall material into water, stirring for 1h at 50-70 ℃, adding an emulsifier, mixing and stirring for 20min, wherein the mass ratio of the wall material to the water is 1: (4-10).
In an example of the present invention, the wall material comprises the following components in parts by mass: 60-80 parts of cyclodextrin, 10-25 parts of sodium starch octenyl succinate and 5-12 parts of emulsified modified starch, wherein the mass part of the emulsifier is 5-10 parts.
In one example of the invention, the cyclodextrin includes a mixture of one or more of alpha-cyclodextrin, beta-cyclodextrin, hydroxypropyl beta-cyclodextrin, hydroxymethyl beta-cyclodextrin, hydroxyethyl beta-cyclodextrin.
In one example of the present invention, the emulsifier includes a mixture of one or more of polyether modified silicone, polyether modified organofluorine, alkyl polyether, tween-40, tween-60, tween-80, sodium dodecylbenzenesulfonate, and sodium dodecylsulfate.
In an example of the present invention, the primary embedding includes: adding the core material solution into the wall material solution, and stirring for 20-60 min at 40-60 ℃; and (3) homogenizing and emulsifying the mixed solution of the core material solution and the wall material solution by using a homogenizer to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain the single-layer microcapsule.
In one example of the present invention, the homogenizing and emulsifying includes a first homogenizing and a second homogenizing, wherein the first homogenizing is performed at a rotation speed of 5000-20000 rpm for 5-20 min under a pressure of 100-500 bar; and the secondary homogenization is to add liquid paraffin into the emulsion obtained by the primary homogenization, and homogenize for 5-20 min again, wherein the addition of the liquid paraffin is 0.5-2 wt% of the total mass of the emulsion.
In an example of the present invention, the secondary embedding includes: adding the single-layer microcapsule obtained by primary embedding into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; adding chitosan and calcium chloride into the mixed solution, stirring uniformly, and carrying out ultrasonic treatment for 5 min; filtering and drying to obtain the double-layer microcapsule.
In one example of the invention, the sodium alginate solution comprises 3-8 wt% of sodium alginate, 2-4 wt% of polyethylene glycol and 1 wt% of dibutyl tin dilaurate; the concentration of the chitosan in the mixed system is 2-3 wt% (the mass of the chitosan accounts for the total mass of the mixed system), and the concentration of the calcium chloride in the mixed system is 0.5-2 wt% (the mass of the calcium chloride accounts for the total mass of the mixed system).
The invention also provides a plant essential oil microcapsule, which is prepared by the preparation method.
In an example of the present invention, the plant essential oil microcapsule includes a core material, a first wall material and a second wall material, the first wall material is coated on the outer side of the core material, the second wall material is coated on the outer side of the first wall material, the core material is plant essential oil, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate.
The invention provides a preparation method of plant essential oil microcapsules, which utilizes the special cavity structure of cyclodextrin and the characteristics of internal hydrophobicity and external hydrophilicity to enable essential oil molecules to enter the cavity of the cyclodextrin through non-covalent bonds such as hydrophobic effect, van der Waals force, hydrogen bond and the like to form microcapsules at a molecular level; and the chitosan/sodium alginate is used for secondary embedding of the microcapsule, so that the slow release property and stability of the microcapsule are improved. The method has the advantages of low cost, simple process, and no toxicity or harm. The microcapsule prepared by the method has good embedding rate and small particle size, can reduce the damage to the active ingredients of the essential oil, effectively reduce the volatilization of the essential oil, improve the photo-thermal stability of the essential oil and prolong the effect and action time of the essential oil; storing the liquid essential oil in a solid form while not damaging the essential oil; greatly expands the application range of the plant essential oil.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of a preparation method of the plant essential oil microcapsule of the invention.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It is to be noted that the features in the following embodiments and examples may be combined with each other without conflict. It is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
It should be understood that the terms "upper", "lower", "left", "right", "middle" and "one" used herein are for clarity of description only, and are not intended to limit the scope of the invention, and that changes or modifications in the relative relationship may be made without substantial technical changes and modifications.
Referring to fig. 1, the present invention provides a method for preparing plant essential oil microcapsules and plant essential oil microcapsules prepared by the method, so as to improve the instability of plant essential oil and prolong the efficacy time of the plant essential oil.
Referring to fig. 1, the preparation method of the plant essential oil microcapsule of the present invention at least includes the following steps:
s1, preparing a core material solution by using plant essential oil;
s2, preparing a wall material solution by using cyclodextrin;
s3, adding the core material solution into the wall material solution, homogenizing and emulsifying to realize primary embedding of plant essential oil by cyclodextrin;
s4, carrying out secondary embedding on the plant essential oil by utilizing the chitosan/sodium alginate to obtain the double-layer microcapsule.
Referring to fig. 1, the step of preparing the core material solution in step S1 specifically includes: firstly, mixing plant essential oil and absolute ethyl alcohol in a proportion of 1: and (2) uniformly mixing and stirring the mixture according to the mass ratio of (2-5), adding lecithin into the solution, heating and stirring the mixture to completely dissolve the lecithin into the solution to obtain a core material solution, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2. The plant essential oil can be selected from one or more of lavender essential oil, flos Matricariae Chamomillae essential oil, vanilla essential oil, and rhizoma et radix Valerianae essential oil, and can be selected according to the function of the essential oil. Lecithin is a natural antidote, and a certain amount of lecithin is added into plant essential oil to decompose toxin in vivo and provide sufficient nutrients such as water, oxygen and the like for skin by increasing heme, so that the skin becomes smooth and soft. In some embodiments, the mass ratio of the plant essential oil to the absolute ethyl alcohol can be selected to be 1:2, 1:3, 1:5, etc., and the mass ratio of the plant essential oil to the lecithin can be selected to be 1:2, 3:2, 5:2, etc., and both endpoints and middle values in the above ratio range can be selected.
Referring to fig. 1, the step of preparing the wall material solution in step S2 specifically includes: firstly, adding a prepared wall material into water, stirring for 1h at the temperature of 50-70 ℃, adding an emulsifier, mixing and stirring for 20min to emulsify the wall material, wherein the mass ratio of the wall material to the water is 1: (4-10), for example, 1:4, 1:6, 1:8, 1:10, etc. The wall material comprises 60-80 parts by mass of cyclodextrin, 10-25 parts by mass of sodium starch octenylsuccinate and 5-12 parts by mass of emulsified modified starch, wherein the cyclodextrin comprises one or a mixture of more of alpha-cyclodextrin, beta-cyclodextrin, hydroxypropyl beta-cyclodextrin, hydroxymethyl beta-cyclodextrin and hydroxyethyl beta-cyclodextrin. The cyclodextrin has the characteristics of special cavity structure, internal hydrophobicity and external hydrophilicity, and essential oil molecules enter the cyclodextrin cavity through intermolecular acting forces such as hydrophobic action, van der Waals force, hydrogen bonds and the like to form a microcapsule at a molecular level.
The emulsifier is 5-10 parts by weight, and can be selected from one or a mixture of polyether modified organic silicon, polyether modified organic fluorine, alkyl polyether, tween-40, tween-60, tween-80, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate. The emulsifier can reduce the interfacial tension in the mixing system and prevent the mutual coagulation and aggregation of the liquid drops to form uniform emulsion.
Referring to fig. 1, the primary embedding of step S3 specifically includes: and (3) adding the core material solution prepared in the step (S1) into the wall material solution prepared in the step (S2), uniformly stirring at 40-60 ℃, for example, stirring for 20-60 min, homogenizing the uniformly stirred mixed solution by using a homogenizer to obtain a stable emulsifying system, and drying the emulsifying system to obtain the single-layer microcapsule. Wherein the mass ratio of the core material solution to the wall material solution is 1 (0.5-1.5), for example, 1:0.5, 1:1 or 1: 1.5. The homogenizing treatment comprises primary homogenizing and secondary homogenizing, namely, the uniformly stirred mixed solution is placed in a homogenizing bag, and is homogenized and emulsified for 5-20 min at the rotating speed of 5000-20000 rpm under the pressure of 100-500 bar; and then adding liquid paraffin into the emulsion system, and carrying out secondary homogenization for 5-20 min under the same pressure and rotation speed, wherein the addition amount of the liquid paraffin is 0.5-2% of the total mass of the emulsion during the secondary homogenization. Because the cyclodextrin is in a porous structure, the plant essential oil is wrapped by the cyclodextrin, the plant essential oil can volatilize from the gaps of the cyclodextrin, the gaps of the cyclodextrin can be wrapped by the liquid paraffin, and the loss of the essential oil in the subsequent heating process is reduced.
Referring to fig. 1, the step S4 of secondary embedding specifically includes: slowly adding the single-layer microcapsule obtained in the step S3 into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; adding chitosan and calcium chloride into the mixed solution, mixing and stirring uniformly, performing ultrasonic treatment for 5min, filtering and drying, and wrapping chitosan/sodium alginate on the outer side of the cyclodextrin to form a double-layer microcapsule. The mass of the single-layer microcapsule is 15-30 wt% of a sodium alginate solution, the sodium alginate solution comprises 3-8 wt% of sodium alginate, 2-4 wt% of polyethylene glycol and 1 wt% of dibutyl tin dilaurate, the concentration of chitosan in a mixed system is 2-3 wt%, and the concentration of calcium chloride in the mixed system is 0.5-2 wt%.
The formation mechanism of the chitosan/sodium alginate biological capsule is as follows: the chitosan is a high molecular substance formed by connecting 2-amino-glucose through beta-1, 4 glycosidic bonds, a large amount of primary amino groups exist in molecules, the chitosan is positively charged, the sodium alginate is formed by polymerizing sodium salt (M) of d-type mannuronic acid with a beta-1, 4 structure and L-type guluronic acid (G) with an alpha-1, 4 structure, the molecules are provided with a large amount of carboxyl groups and negatively charged, when the chitosan, the sodium alginate and calcium chloride coexist, the chitosan and the sodium alginate are attracted by the positive and negative charges to form a polyelectrolyte membrane, and the sodium alginate and the Ca are adsorbed by the positive and negative charges2+The complexing forms a cured film, and the mechanism is as follows:
in directly adding chitosan and calcium chloride into sodium alginate solution, at first chitosan and sodium alginate form the complex layer, along with sodium alginate and chitosan further reaction, the complex layer thickens, and chitosan deposits at the inner membrane of complex layer simultaneously, and along with the thickening of complex layer, the liquid drop further contracts, and the Ca in the membrane+Exuding under the action of concentration difference and mechanical force, reacting with sodium alginate, forming calcium alginate coacervate outside the complex layer, and finally forming a three-layer film containing calcium alginate coacervate, chitosan/sodium alginate complex layer and chitosan precipitate layer.
The plant essential oil microcapsule prepared by the preparation method comprises a core material, a first wall material and a second wall material, wherein the first wall material is wrapped on the outer side of the core material, the second wall material is wrapped on the outer side of the first wall material, the core material is plant essential oil such as lavender essential oil, chamomile essential oil, vanilla essential oil, valerian essential oil and the like, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate. The particle size of the prepared plant essential oil microcapsule is less than 50 mu m, most of the plant essential oil microcapsules are concentrated on 1-10 mu m, and the slow release property and stability of the microcapsules can be effectively improved by adopting a double-layer microcapsule preparation method.
The present invention is described in detail below with reference to several specific examples, and the drugs used in the following examples are all commercially available in general.
Example 1
The preparation of the plant essential oil microcapsule comprises the following steps:
preparing a core material solution: mixing lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:2, uniformly stirring, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 1:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin;
preparing a wall material solution: adding 70 parts by mass of beta-cyclodextrin, 20 parts by mass of sodium starch octenylsuccinate and 10 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:4), stirring for 1h at 60 ℃, adding 8 parts by mass of tween-80, and continuing to stir for 20 min;
primary embedding: mixing the core material solution and the wall material solution in a mass ratio of 1:1.5, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe for 20min at the rotation speed of 20000rpm under the pressure of 500bar by using a nano homogenizer; adding 1 wt% of liquid paraffin into the system, homogenizing for 20min to obtain a stable emulsifying system, and drying to obtain a cyclodextrin-coated single-layer microcapsule;
secondary embedding; adding the single-layer microcapsule into a sodium alginate solution (8 wt% of sodium alginate, 3 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 30 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 3 wt% of the total system, and the addition amount of calcium chloride is 2 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Example 2
Preparing a core material solution: mixing lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:3, uniformly stirring, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 3:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin;
preparing a wall material solution: adding 80 parts by mass of beta-cyclodextrin, 10 parts by mass of sodium starch octenylsuccinate and 12 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:10), stirring for 1h at 70 ℃, adding 10 parts by mass of tween-40, and continuing to stir for 20 min;
primary embedding: mixing the core material solution and the wall material solution in a mass ratio of 1:1, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe material for 20min at the rotation speed of 10000rpm under the pressure of 500bar by using a nano homogenizer; adding liquid paraffin accounting for 2 wt% of the system, homogenizing for 20min to obtain a stable emulsifying system, and drying to obtain cyclodextrin-coated single-layer microcapsule;
secondary embedding: adding the single-layer microcapsule into a sodium alginate solution (5 wt% of sodium alginate, 2 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 20 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 2 wt% of the total system, and the addition amount of calcium chloride is 1 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Example 3
Preparing a core material solution: mixing lavender essential oil and absolute ethyl alcohol in a mass ratio of 1:5, uniformly stirring, adding lecithin into the mixed solution, wherein the mass ratio of the plant essential oil to the lecithin is 5:2, and heating and stirring to completely dissolve the plant essential oil and the lecithin;
preparing a wall material solution: adding 60 parts by mass of beta-cyclodextrin, 10 parts by mass of sodium starch octenylsuccinate and 12 parts by mass of emulsified modified starch into water (the mass ratio of the total mass of the components to the water is 1:7), stirring for 1h at 60 ℃, adding 5 parts by mass of tween-60, and continuing to stir for 20 min;
primary embedding: mixing the core material solution and the wall material solution in a mass ratio of 1:0.5, and stirring at 50 ℃ for 40 min; homogenizing the mixed system of the core material and the pipe for 20min at the rotation speed of 20000rpm under the pressure of 500bar by using a nano homogenizer; adding 0.5 wt% of liquid paraffin mixed into the system, homogenizing for 20min to obtain a stable emulsifying system, and drying to obtain cyclodextrin-coated single-layer microcapsule;
secondary embedding: adding the single-layer microcapsule into a sodium alginate solution (3 wt% of sodium alginate, 4 wt% of polyethylene glycol and 1 wt% of dibutyltin dilaurate), wherein the addition amount of the single-layer microcapsule is 15 wt% of the mass of the sodium alginate solution, and uniformly stirring at 50 ℃ to obtain a mixed solution; slowly adding chitosan and calcium chloride (the addition amount of chitosan is 2.5 wt% of the total system, and the addition amount of calcium chloride is 0.5 wt% of the total system), stirring and mixing uniformly, performing ultrasonic treatment for 5min, filtering, and drying to obtain the double-layer microcapsule.
Example 4
The difference of this example compared with example 1 is that lavender essential oil is replaced by chamomile essential oil, and other conditions are not changed.
Example 5
The difference of this example compared with example 2 is that the lavender essential oil is replaced by the vanilla essential oil, and other conditions are not changed.
Example 6
The difference between this example and example 3 is that the lavender essential oil is replaced by valerian essential oil, and other conditions are not changed.
Comparative example 1
Comparative example 1 differs from example 1 in that 1 homogenization treatment was not performed; 2. no secondary embedding was performed.
Indexes of the plant essential oil microcapsules prepared in examples 1 to 6 and comparative example 1 were measured, and the results are shown in table 1:
table 1: results of examination of the products obtained in examples 1 to 6 and comparative example 1
The detection results of the examples 1 to 6 and the comparative example 1 show that the embedding rate of the plant essential oil microcapsule is 60 to 80 percent, the particle size of the microcapsule is less than 50 mu m, and most of the particle sizes are concentrated in 1 to 10 mu m. The embedding rate of the comparative example 1 is 59%, the particle size distribution is 10-200 mu m, and the preparation method provided by the invention has smaller particle size and better embedding rate compared with the comparative example 1.
The retention of the products obtained in examples 1 to 6 and comparative example 1 was examined to evaluate the stability effect:
the products of examples 1 to 6 and comparative example 1 were equally divided into 4 groups of samples, which were respectively left at normal temperature (25 ℃) for 3 months and at high temperature (100 ℃, 130 ℃, 160 ℃) for 72 hours, extracted at regular intervals, and the content of essential oil in each sample was measured by high performance liquid chromatography to determine retention rates at normal temperature and high temperature, and the results are shown in tables 2 and 3:
table 2: retention rate (%). of the products obtained in examples 1 to 6 and comparative example 1 after standing at ordinary temperature for 3 months
Table 3: the products obtained in examples 1 to 7 and comparative example 1 were left at high temperature for 72h retention (%)
As can be seen from tables 2 and 3, the plant essential oil microcapsule of the present invention has good retention of essential oil with retention rate of more than 99% when placed at room temperature for three months. Standing at high temperature for 72h, wherein the retention rate is more than 85% at 100 ℃; at 130 ℃, the retention rate reaches more than 80 percent; at 160 ℃, the retention rate reaches over 75 percent; in contrast, comparative example 1, which was only subjected to one-time embedding, showed a low retention. Therefore, the secondary embedding of the invention can reduce the volatilization of the essential oil and improve the stability of the essential oil, and particularly has good stability under the condition of high temperature.
According to the invention, a secondary embedding method is adopted, firstly, the special cavity structure and the characteristics of internal hydrophobicity and external hydrophilicity of cyclodextrin are utilized, the plant essential oil is wrapped in the cavity of the cyclodextrin to form the microcapsule on the molecular level, and then the chitosan/sodium alginate biological capsule is wrapped on the outer side of the cyclodextrin to form the double-layer plant essential oil microcapsule, so that the slow release property and the stability of the microcapsule are improved. The microcapsule prepared by the method has better embedding rate, can reduce the damage to the active ingredients of the essential oil, effectively reduces the volatility of the essential oil, improves the photo-thermal stability of the essential oil and prolongs the efficacy action time of the essential oil. Therefore, the invention effectively overcomes some practical problems in the prior art, thereby having high utilization value and use significance.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (11)
1. The preparation method of the plant essential oil microcapsule is characterized by at least comprising the following steps:
preparing a core material solution by using plant essential oil;
preparing a wall material solution by using cyclodextrin;
adding the core material solution into the wall material solution, homogenizing and emulsifying to realize primary embedding of plant essential oil by cyclodextrin;
and carrying out secondary embedding on the plant essential oil by utilizing chitosan/sodium alginate to obtain the double-layer microcapsule.
2. The method for preparing plant essential oil microcapsules according to claim 1, wherein the step of preparing the core material solution comprises: uniformly mixing plant essential oil and absolute ethyl alcohol according to the mass ratio of 1 (2-5), adding lecithin into the solution, and heating to completely dissolve the lecithin, wherein the mass ratio of the plant essential oil to the lecithin is (1-5) to 2.
3. The method for preparing plant essential oil microcapsules according to claim 1, wherein the step of preparing a wall material solution comprises: adding the prepared wall material containing cyclodextrin into water, stirring for 1h at 50-70 ℃, adding an emulsifier, mixing and stirring for 20min, wherein the mass ratio of the wall material to the water is 1: (4-10).
4. The preparation method of plant essential oil microcapsules according to claim 3, wherein the wall material comprises the following components in parts by mass: 60-80 parts of cyclodextrin, 10-25 parts of sodium starch octenyl succinate and 5-12 parts of emulsified modified starch, wherein the mass part of the emulsifier is 5-10 parts.
5. A process for the preparation of a plant essential oil microcapsule according to claim 4, wherein the cyclodextrin comprises a mixture of one or more of α -cyclodextrin, β -cyclodextrin, hydroxypropyl β -cyclodextrin, hydroxymethyl β -cyclodextrin, hydroxyethyl β -cyclodextrin; the emulsifier comprises one or more of polyether modified organic silicon, polyether modified organic fluorine, alkyl polyether, tween-40, tween-60, tween-80, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate.
6. The method for preparing plant essential oil microcapsules according to claim 1, wherein the primary embedding comprises: adding the core material solution into the wall material solution, and stirring for 20-60 min at 40-60 ℃; and (3) homogenizing and emulsifying the mixed solution of the core material solution and the wall material solution by using a homogenizer to obtain a stable emulsifying system, and drying the stable emulsifying system to obtain the single-layer microcapsule.
7. The method for preparing plant essential oil microcapsules according to claim 6, wherein the homogenizing emulsification comprises primary homogenization and secondary homogenization, wherein the primary homogenization is homogenization at 5000-20000 rpm for 5-20 min under the pressure of 100-500 bar; and the secondary homogenization is to add liquid paraffin into the emulsion obtained by the primary homogenization, and homogenize for 5-20 min again, wherein the addition of the liquid paraffin is 0.5-2 wt% of the total mass of the emulsion.
8. The method for preparing plant essential oil microcapsules according to claim 1, wherein the secondary embedding comprises: adding the single-layer microcapsule obtained by primary embedding into a sodium alginate solution, and uniformly stirring at 50-60 ℃ to obtain a mixed solution; adding chitosan and calcium chloride into the mixed solution, stirring uniformly, and carrying out ultrasonic treatment for 5 min; filtering and drying to obtain the double-layer microcapsule.
9. The preparation method of the plant essential oil microcapsule as claimed in claim 8, wherein the sodium alginate solution comprises 3-8 wt% of sodium alginate, 2-4 wt% of polyethylene glycol and 1 wt% of dibutyl tin dilaurate; the concentration of the chitosan in the mixed system is 2-3 wt%, and the concentration of the calcium chloride in the mixed system is 0.5-2 wt%.
10. A plant essential oil microcapsule, which is prepared by the preparation method of the plant essential oil microcapsule according to any one of claims 1 to 9.
11. A plant essential oil microcapsule according to claim 10, comprising: the core material is plant essential oil, the first wall material is cyclodextrin, and the second wall material is chitosan/sodium alginate.
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| CN116421642A (en) * | 2023-03-01 | 2023-07-14 | 神威药业集团有限公司 | Xinnaoqing preparation and its preparing process |
| CN116492944A (en) * | 2023-06-21 | 2023-07-28 | 云南省农业科学院农产品加工研究所 | Microcapsule wall material and preparation method and application thereof |
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