CN106148004B - Essential oil microcapsule and preparation method thereof - Google Patents
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Abstract
The invention discloses an essential oil microcapsule and a preparation method thereof; the essential oil microcapsule comprises the following components in parts by weight: 12.5-100 parts of lemon grass essential oil, 50-100 parts of wall materials and 3.125-35 parts of emulsifier; compared with the existing products, the invention is natural and safe, and has better affinity; the production process completely isolates oxygen, so that an antioxidant does not need to be added in the formula; compared with the prior art, the operation temperature is lower, and the loss of flavor substances is effectively reduced; after elution, the residual oil on the surface of the product is less and the stability is strong; the yield of the essential oil microcapsule product is improved, particularly the effective loading capacity can be obviously improved, the oil content can reach more than 10 percent, and the yield is more than 60 percent; the product has a complete structure, small particle size, uniform distribution and small surface pore area, can effectively slow down the volatilization of core materials and the entrance of external oxygen in the storage period, prolongs the shelf life and increases the market value; can be continuously produced and is more suitable for industrial requirements.
Description
Technical Field
The invention relates to a microcapsule, in particular to an essential oil microcapsule and a preparation method thereof, and especially relates to a lemongrass essential oil microcapsule and a preparation method thereof.
Background
The lemon grass essential oil is an essential oil extracted from a natural aromatic plant lemon grass, and has multiple effects of repelling mosquitoes, sterilizing, diminishing inflammation, resisting depression, improving spirit and the like. Along with the increasing demand of people for natural, green and safe products, the lemongrass essential oil is widely used, such as aromatherapy, mosquito repellent daily chemical products, textile perfume addition and the like.
The microcapsule technology is to coat solid or liquid components with reactivity, sensitivity or volatility in small nano or micron capsule with the function of protecting core material with natural or synthetic polymer material. At present, the application in the fields of medicine, food, cosmetics, textile and the like is more and more extensive, and a plurality of related products and patent technologies appear at home and abroad.
The essential oil microcapsule provides a more superior approach for the application of the aromatic plant essential oil in products, and enlarges the application range of the essential oil. The concrete points are as follows: on the one hand, the aromatic plant essential oil has many and complex organic compound components, extremely unstable and volatile chemical properties, and the components are easy to lose quickly during use and storage. The essential oil microcapsule can effectively stabilize the effective components of essential oil, improve the stability of the product, slowly release the effect at a certain speed, and improve the slow release property of the product. On the other hand, essential oil is in a single liquid form and is limited in application range, and essential oil microcapsules can be added in a solid powder form to prepare products (such as cream cosmetics and fragrant textiles), so that the application of essential oil in the aspects is filled.
At present, most of the existing microcapsule products are directed at the coating of monomer compounds, while the microcapsules of volatile multi-component compounds such as essential oil have few types, and some of the volatile multi-component compounds are made of synthetic polymer materials, so that the volatile multi-component compounds are not natural and safe enough, or antioxidants with poor compatibility are added; in some production processes, the temperature is too high, or oxygen cannot be isolated, so that the loss of the core material is caused; some related microencapsulation process indexes, particularly low oil content, incomplete microcapsule structure, insufficient surface smoothness and extremely uneven particle size distribution; some stability is poor, the essential oil is volatilized or oxidized quickly, and the shelf life is short; particularly, some production methods cannot realize continuous production and are not suitable for industrialized requirements. It is clear that these drawbacks, to a certain extent, greatly affect the use of essential oil microcapsules.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an essential oil microcapsule and a preparation method thereof, and the preparation method of the lemon grass essential oil microcapsule solves the problems, adopts natural, green and safe materials, can effectively improve the yield and the oil content, and has good product-related properties, strong stability and longer shelf life. Wherein, the selected wall material is HI-CAP100 type modified starch which is prepared by introducing hydrophobic groups through chemical modification, and the emulsion produced by the modified starch has fine particles and high stability. Compared with the traditional wall materials such as cyclodextrin and maltodextrin, the traditional wall materials of cyclodextrin and maltodextrin have lower surface activity and poorer emulsifying capacity, can only stabilize emulsion by increasing viscosity, and the formed emulsion has large and rough particles. In the process of implementing the invention, the effect of compounding the monoglyceride and the sucrose ester is found to be obviously superior to the effect of the existing emulsifiers such as Tween 80, span 80 and polyoxyethylene lauryl ether and the emulsifier such as monoglyceride and sucrose ester which are used independently. Experiments show that the emulsifier obtained by compounding monoglyceride and sucrose ester has the best emulsification effect on the lemongrass essential oil, and meanwhile, the sucrose ester can form a complex with starch, so that the structure of a wall material can be improved, the stability of a microcapsule structure is facilitated, the slow release effect of the microcapsule is prolonged, the sucrose ester has the antioxidant and mildewproof effects, and an antioxidant does not need to be added in the production process of the microcapsule, so that the emulsification function of the sucrose ester is only utilized. Compared with the conventional microcapsule, the microcapsule reduces the introduction of other additives, ensures the naturalness of the microcapsule to the maximum extent, and meets the requirement of natural plant essential oil microencapsulation.
The purpose of the invention is realized by the following technical scheme:
in a first aspect, the invention provides a lemongrass essential oil microcapsule, which comprises the following components in parts by weight:
12.5 to 100 parts of lemon grass essential oil,
50 to 100 parts of wall material,
3.125-35 parts of an emulsifier;
wherein the wall material comprises modified starch with the model number of HI-CAP 100;
the emulsifier is compounded by monoglyceride and sucrose ester.
Preferably, the weight parts of the monoglyceride and the sucrose ester in the lemon grass essential oil microcapsule are 0.278-3.115 and 2.847-31.885 respectively; more preferably, the weight percentages of the monoglyceride and the sucrose ester in the emulsifier are respectively 8.9-26.8% and 73.2-91.9%, the HLB (hydrophile-lipophile balance) value of the emulsifying system is 12-14, the emulsion is stable, and after standing for 5 hours, emulsion breaking phenomena such as flocculation and layering do not occur, when the amount of the emulsifier is insufficient, the emulsification is insufficient, the emulsion is easy to layer, and when the amount of the emulsifier is excessive, the emulsifier is wasted;
preferably, the core-wall ratio of the lemongrass essential oil microcapsules is 1: 8-2: 1, and the weight of the emulsifier is 20-35% of that of the lemongrass essential oil; more preferably, the lemongrass essential oil microcapsule has a core-wall ratio of 1: 8; the weight of the emulsifier is 25% of that of the lemongrass essential oil, the performance is best at the moment, if the core-wall ratio is too low, the wrapping is insufficient, the phenomena of empty capsules, uneven outer wall thickness and the like occur, and if the core-wall ratio is too high, the essential oil is wrapped incompletely, the floating oil on the outer wall is too much, and the waste is caused.
In a second aspect, the invention provides a preparation method of lemongrass essential oil microcapsules, which comprises the following steps:
step one, preparing a saturated aqueous solution of a wall material, uniformly stirring at 150-200 rpm, adding an emulsifier, and after the emulsifier is completely added, adding the lemon grass essential oil in a corresponding weight part at a speed of 60-80 drops/min under a stirring state to form a mixed system;
step two, uniformly stirring the mixed system at constant temperature and under the condition of 150-200 rpm, and homogenizing until a uniform emulsion is formed;
extruding the emulsion into a dehydration solvent at 0-4 ℃ under the condition of air isolation, and removing contained water to obtain a dehydration product; filtering the dehydration product, and removing the dehydrating agent to obtain a glassy essential oil microcapsule primary product;
and step four, drying the essential oil microcapsule primary product at constant temperature until the essential oil microcapsule primary product is solid, and obtaining the lemongrass essential oil microcapsule.
Preferably, in step one, the emulsifier is added at a rate of 10 g/min.
Preferably, in the second step, the constant temperature is 45-55 ℃; the stirring adopts a digital display stirrer, the viscosity of the mixture is too low and the mixture is not easy to stir in the stirring process, and the temperature is too high, so that the essential oil with multiple components can be damaged for the thermosensitive essential oil, and the characteristics of the original substances are changed.
Preferably, in the second step, the time of the homogenization treatment is 4-6 min, the temperature of the homogenization treatment is 45-55 ℃, and the speed of the homogenization treatment is 8000-10000 rpm; the homogenizing treatment adopts a homogenizer, the homogenizing time is too short, the mixing is insufficient, the efficiency is too low if the mixing is too long, no practical significance is realized, and if the homogenization is carried out under an exposure condition, the homogenization is more likely to cause the homogenization materials to be oxidized; in the homogenizing process, the homogenizing rod can generate heat to heat the homogenized substance to a certain extent, if the homogenizing temperature is too low, the temperature difference between the inside and the outside is too large, the homogenization is not facilitated, and if the homogenizing temperature is too high, the volatilization of the essential oil is accelerated on one hand, and on the other hand, the components are damaged; meanwhile, if the speed is too high in the homogenizing process, excessive shearing can be caused to the wall material, and the formation of microcapsules is not facilitated.
Preferably, in the third step, the dehydration solvent is isopropanol which has good water solubility and good solubility for plant essential oil, and the uncoated essential oil on the surface of the microcapsule is removed; the temperature of the dehydration solvent is 0-4 ℃, and the extruded microcapsule can be rapidly hardened at the temperature to be in a glass state, so that the microcapsule structure forming is facilitated.
Preferably, in the third step, nitrogen is specifically introduced into the isolated air; on the basis of the original extrusion equipment, nitrogen is introduced into the extrusion equipment, so that the equipment has no oxygen in the operation process, and the situation that the surface of the microcapsule is blackened due to the oxidation of the uncoated essential oil is avoided.
Preferably, in the third step, the extrusion is specifically performed by using a double-rod screw extrusion device; through two pole screw extrusion equipment, extrude in 0 ~ 4 ℃ dehydration solvent isopropanol, when the extrusion fluid contacts microthermal isopropanol through the pore membrane, the wall material just dehydrates the sclerosis and cladding thereupon on the surface of essential oil, makes the coarse product of slight filament, and the product after to the extrusion again, filtration treatment separates out the coarse product from dehydration solvent, obtains the preliminary product of glass state's essential oil microcapsule.
Preferably, in step three, the filtering treatment specifically refers to: filtering by adopting a micro-pore filtering membrane with the pore diameter of 0.6-0.8 mu m; residual water and isopropanol can be effectively filtered out by filtration treatment to be isolated from the glass state, and the process is carried out in a closed container to ensure that the process is isolated from oxygen.
Preferably, in the fourth step, the constant temperature is 45-55 ℃, and the constant temperature drying equipment is an electrothermal blowing drying oven;
preferably, the preparation method further comprises the steps of grinding the lemon grass essential oil microcapsules obtained in the step four, filling the ground lemon grass essential oil microcapsules into a brown wide-mouth frosted bottle, coating sealing grease on the bottle mouth to prevent air from entering, storing the bottle at 15-20 ℃ in a dark place, and prolonging the service life of the microcapsules without adding preservatives and antioxidants.
Compared with the prior art, the invention has the advantages that:
1. the material selected by the invention is food-grade starch which is natural, safe and good in affinity;
2. the production process completely isolates oxygen, so that an antioxidant does not need to be added in the formula;
3. compared with other production methods, the operation temperature is lower, and the loss of flavor substances is effectively reduced;
4. after elution, the residual oil on the surface of the product is less and the stability is strong; the yield of the essential oil microcapsule product is improved, and particularly, the effective loading capacity (oil content) can be obviously improved and can reach more than 10 percent;
5. the product has a complete structure, small particle size, uniform distribution and small surface pore area, can effectively slow down the volatilization of the core material and the entrance of external oxygen in the storage period, prolongs the shelf life and increases the market value;
6. can be continuously produced, thereby being more suitable for industrial requirements.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
fig. 1 is an SEM scanning electron microscope image of No. 2 lemongrass essential oil microcapsule product.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment relates to a lemongrass essential oil microcapsule and a preparation method thereof, which are carried out according to the following steps:
1. determining the type of an emulsifier suitable for the lemongrass essential oil, wherein the emulsifier is used by compounding monoglyceride and sucrose ester, and the weight parts of the emulsifier in the lemongrass essential oil microcapsule are 0.278 and 2.847 respectively; the weight percentages of the emulsifier and the emulsifier are respectively 26.8 percent and 73.2 percent, and the HLB value, namely the water-oil balance value of the emulsifying system is 12;
2. preparing a saturated aqueous solution of a wall material, uniformly stirring at a low speed of 150rpm, slowly adding an emulsifier, and after the emulsifier is completely added, adding the lemon grass essential oil in a corresponding weight part at a speed of 60 drops per minute under a stirring state to form a mixed system, wherein the mixed system comprises the following components in parts by weight: 12.5 parts of lemon grass essential oil, 50 parts of wall material (HI-CAP100 modified starch) and 3.125 parts of emulsifier;
uniformly stirring the mixed system at the constant temperature of 3.45 ℃ at the speed of 150rpm, and homogenizing until a uniform emulsion is formed; homogenizing at 45 deg.C for 4min at 10000 rpm;
4. extruding the uniform emulsion into a dehydration solvent at 0-4 ℃ by using double-rod spiral extrusion equipment under the condition of air isolation, and removing contained water to obtain a dehydration product; filtering the dehydrated product by adopting a micro-pore filtering membrane with the pore diameter of 0.6-0.8 mu m, filtering, and removing a dehydrating solvent to obtain a glassy essential oil microcapsule primary product;
and drying the essential oil microcapsule primary product at the constant temperature of 5.45 ℃ until the essential oil microcapsule primary product is solid, thus obtaining the lemongrass essential oil microcapsule. Grinding the mixture, putting the mixture into a brown wide-mouth frosted bottle, coating sealing grease on the bottle mouth to prevent air from entering, and storing the bottle at 15-20 ℃ in a dark place.
Example 2
The embodiment relates to a lemongrass essential oil microcapsule and a preparation method thereof, which are carried out according to the following steps:
1. determining the type of an emulsifier suitable for the lemongrass essential oil, wherein the emulsifier is used by compounding monoglyceride and sucrose ester, and the weight parts of the emulsifier in the lemongrass essential oil microcapsule are 0.278 and 2.847 respectively; the weight percentages of the emulsifier and the emulsifier are respectively 26.8 percent and 73.2 percent, and the HLB value, namely the water-oil balance value of the emulsifying system is 12;
2. preparing a saturated aqueous solution of wall materials, uniformly stirring at a low speed of 150rpm, slowly adding an emulsifier, and after the emulsifier is completely added, adding the lemon grass essential oil in a corresponding weight part at a speed of 60 drops per minute under a stirring state) to form a mixed system, wherein the mixed system comprises the following components in parts by weight: 12.5 parts of lemon grass essential oil, 100 parts of wall material and 3.125 parts of emulsifier;
stirring the mixed system uniformly at the constant temperature of 3.50 ℃ at the speed of 150rpm, and homogenizing until a uniform emulsion is formed; homogenizing at 50 deg.C for 5min and 8000 rpm;
4. extruding the uniform emulsion into a dehydration solvent at 0-4 ℃ by using double-rod spiral extrusion equipment under the condition of air isolation, and removing contained water to obtain a dehydration product; filtering the dehydrated product by adopting a micro-pore filtering membrane with the pore diameter of 0.6-0.8 mu m, filtering, and removing a dehydrating solvent to obtain a glassy essential oil microcapsule primary product;
and drying the essential oil microcapsule primary product at the constant temperature of 5.50 ℃ until the essential oil microcapsule primary product is solid, thus obtaining the lemongrass essential oil microcapsule. Grinding the mixture, putting the mixture into a brown wide-mouth frosted bottle, coating sealing grease on the bottle mouth to prevent air from entering, and storing the bottle at 15-20 ℃ in a dark place.
Example 3
The embodiment relates to a lemongrass essential oil microcapsule and a preparation method thereof, which are carried out according to the following steps:
1. determining the type of an emulsifier suitable for the lemongrass essential oil, wherein the emulsifier is used by compounding monoglyceride and sucrose ester, and the weight parts of the emulsifier in the lemongrass essential oil microcapsule are 0.278 and 2.847 respectively; the weight percentages of the emulsifier and the emulsifier are respectively 26.8 percent and 73.2 percent, and the HLB value, namely the water-oil balance value of the emulsifying system is 12;
2. preparing a saturated aqueous solution of wall materials, uniformly stirring at a low speed of 150rpm, slowly adding an emulsifier, and after the emulsifier is completely added, adding the lemon grass essential oil in a corresponding weight part at a speed of 60 drops per minute under a stirring state) to form a mixed system, wherein the mixed system comprises the following components in parts by weight: 100 parts of lemongrass essential oil, 50 parts of wall material and 3.125 parts of emulsifier;
stirring the mixed system uniformly at the constant temperature of 3.55 ℃ at the speed of 150rpm, and homogenizing the mixed system until a uniform emulsion is formed; homogenizing at 55 deg.C for 6min and 9000 rpm;
4, extruding the uniform emulsion into a dehydration solvent at 0-4 ℃ by using double-rod spiral extrusion equipment under the condition of air isolation, and removing contained water to obtain a dehydration product; filtering the dehydrated product by adopting a micro-pore filtering membrane with the pore diameter of 0.6-0.8 mu m, filtering, and removing a dehydrating solvent to obtain a glassy essential oil microcapsule primary product;
and drying the essential oil microcapsule primary product at the constant temperature of 5.55 ℃ until the essential oil microcapsule primary product is solid, thus obtaining the lemongrass essential oil microcapsule. Grinding the mixture, putting the mixture into a brown wide-mouth frosted bottle, coating sealing grease on the bottle mouth to prevent air from entering, and storing the bottle at 15-20 ℃ in a dark place.
The operation can realize the invention within the following parameter condition ranges: the lemon grass essential oil microcapsule comprises 12.5-100 parts by weight of lemon grass essential oil, 50-100 parts by weight of wall materials and 3.125-35 parts by weight of emulsifying agents; the weight parts of monoglyceride and sucrose ester in the lemon grass essential oil microcapsule are 0.278-3.115 and 2.847-31.885 respectively; the HLB value of the emulsification system, namely the water-oil balance value, is 12-14; the stirring speed is 150-200 rpm; the adding speed of the lemongrass essential oil is 60-80 drops/min; the operation temperature is 45-55 ℃, and the homogenization temperature is 45-55 ℃.
Performance testing
The production conditions and properties of the products obtained in examples 1 to 3 were summarized and the results of the tests (oil content and yield measurements were determined according to conventional methods in the art) are shown in table 1 below:
TABLE 1
| Examples | Numbering | Temperature (. degree.C.) | Time (min) | Rotational speed (rpm) | Core to wall ratio | Oil content (%) | Yield (%) |
| 1 | 1 | 45 | 4 | 10000 | 1:4 | 12.11 | 65.28 |
| 2 | 2 | 50 | 5 | 8000 | 1:8 | 12.68 | 69.72 |
| 3 | 3 | 55 | 6 | 9000 | 2:1 | 11.93 | 69.33 |
As can be seen from the results in Table 1, the essential oil content of all the 3 examples is above 10%, the yield is above 60%, wherein the process index of the No. 2 lemongrass essential oil microcapsule product is best (corresponding to the process conditions of 50 ℃, 5min, 8000rpm, and a core-wall ratio of 1:8), and both the oil content and the yield are highest. Particularly, by the process, the oil content of the lemongrass essential oil microcapsule is improved by nearly one time compared with the prior similar products. The average particle size is 200nm, the particle size is small and the distribution is uniform. Through an accelerated test, based on a step constant temperature Arrhenius model, the fact that 10% of the essential oil is decomposed at the room temperature of 25 ℃ is deduced, and the required time is about 116 days. The product has better stability and longer life expectancy than similar products.
The scanning electron microscope image of the lemongrass essential oil microcapsule is shown in figure 1, and as can be seen from figure 1, the product of the No. 2 lemongrass essential oil microcapsule has a complete structure and small surface pore area, can effectively slow down the volatilization of core materials and the entrance of external oxygen in the storage period, prolongs the shelf life, and increases the market value.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (7)
1. The preparation method of the lemongrass essential oil microcapsule is characterized by comprising the following components in parts by weight: 12.5-100 parts of lemon grass essential oil, 50-100 parts of wall materials and 3.125-35 parts of emulsifier; wherein the wall material is modified starch with the type of HI-CAP 100; the emulsifier is compounded by monoglyceride and sucrose ester, and the weight parts of the monoglyceride and the sucrose ester in the lemon grass essential oil microcapsule are 0.278-3.115 parts and 2.847-31.885 parts respectively; the water-oil balance value of the emulsifier is 12-14; the core-wall ratio of the lemongrass essential oil microcapsules is 1: 8-2: 1, and the weight of the emulsifier is 20-35% of that of the lemongrass essential oil;
the preparation method comprises the following steps:
step one, preparing a saturated aqueous solution of a wall material, uniformly stirring at 150-200 rpm, adding an emulsifier, and after the emulsifier is completely added, adding the lemon grass essential oil in a corresponding weight part at a speed of 60-80 drops/min under a stirring state to form a mixed system;
step two, uniformly stirring the mixed system at constant temperature and under the condition of 150-200 rpm, and homogenizing until a uniform emulsion is formed; the time of the homogenization treatment is 4-6 min, the temperature of the homogenization treatment is 45-55 ℃, and the speed of the homogenization treatment is 8000-10000 rpm;
extruding the emulsion into a dehydration solvent at 0-4 ℃ under the condition of air isolation, and removing contained water to obtain a dehydration product; filtering the dehydration product, and removing the dehydrating agent to obtain a glassy essential oil microcapsule primary product; the dehydration solvent is isopropanol;
and step four, drying the essential oil microcapsule primary product at constant temperature until the essential oil microcapsule primary product is solid, and obtaining the lemongrass essential oil microcapsule.
2. The method for preparing lemongrass essential oil microcapsules according to claim 1, wherein in the first step, the emulsifier is added at a speed of 10 g/min.
3. The preparation method of the lemongrass essential oil microcapsule as claimed in claim 1, wherein in the second and fourth steps, the constant temperature is 45-55 ℃.
4. The method for preparing lemongrass essential oil microcapsules according to claim 1, wherein in the third step, nitrogen is introduced into the isolated air.
5. The preparation method of lemongrass essential oil microcapsules according to claim 1, wherein in the third step, the extrusion is performed by a double-rod screw extrusion device.
6. The preparation method of lemongrass essential oil microcapsules according to claim 1, wherein in the third step, the filtration treatment specifically comprises: filtering by adopting a micro-pore filtering membrane with the pore diameter of 0.6-0.8 mu m.
7. The preparation method of the lemongrass essential oil microcapsules according to claim 1, wherein the preparation method further comprises the steps of grinding the lemongrass essential oil microcapsules obtained in the step four, filling the grinded bottle with a brown wide-mouth frosted bottle, coating sealing grease on the mouth of the brown wide-mouth frosted bottle, and storing the bottle at 15-20 ℃ in a dark condition.
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Effective date of registration: 20200720 Address after: Room 2248, building 2, No. 1599, Fengpu Avenue, Fengxian District, Shanghai, 201499 Patentee after: Shanghai bosikon Environmental Protection Technology Development Co., Ltd Address before: 200240 Dongchuan Road, Shanghai, No. 800, No. Patentee before: SHANGHAI JIAO TONG University |
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