CN111992153A - High-loading-capacity high-thermal-stability menthol microcapsule and preparation method thereof - Google Patents
High-loading-capacity high-thermal-stability menthol microcapsule and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-load high-thermostability menthol microcapsule and a preparation method thereof, wherein the preparation method of the high-load high-thermostability menthol microcapsule comprises the steps of preparing a water phase by using octenyl succinate esterified starch; preparing an oil phase from lipids and menthol; pouring the oil phase into the water phase, homogenizing under high pressure; cooling and spray drying. The cooling rate is 0.5-1.5 ℃/min. The preparation method of the menthol capsule provided by the invention has the advantages of low cost, green, safe and simple process, and can adopt an optimal cooling mode according to production conditions, obviously reduce the volatility of menthol, isolate external components, release the menthol in a controlled mode, and achieve the effects of protecting core materials, slowly releasing, keeping cool and improving thermal stability.
Description
Technical Field
The invention belongs to the technical field of microcapsules, and particularly relates to a high-capacity high-thermal-stability menthol microcapsule and a preparation method thereof.
Background
The volatile active compounds, wherein the flavors and fragrances occupy a large category, have wide application in the cosmetic, food and pharmaceutical industries. However, volatile actives are unstable, sensitive to light, heat, oxygen and moisture, and due to their volatile nature, are easily lost during processing and use, are not conducive to transportation and storage, and limit the practical use of volatile compounds. In order to solve these problems, active materials can be encapsulated in microcapsules by microencapsulation technology, which has the effects of changing the existing state of the materials, protecting sensitive components, reducing volatility, controlling release, prolonging storage time, and the like. With these unique advantages, microcapsule technology has attracted much attention.
The spray drying method is the most widely adopted method in the preparation method of the essence and flavor microcapsule, and has the characteristics of simple operation, low cost, easy continuous production, high drying speed, good product dispersibility and solubility and the like. The conventional spray drying process steps can be described simply as: uniformly dispersing the core material in the wall material solution to prepare a solution, an emulsion or a suspension, sending the test solution into spray drying equipment, atomizing the test solution into liquid drops by airflow, uniformly dispersing the liquid drops in hot airflow to quickly evaporate the solvent for dissolving the wall material, and solidifying the wall material to form the microcapsule. There are three main classes of wall materials commonly used for spray drying: carbohydrates, hydrocolloids, proteins.
The Solid Lipid Nanoparticle (SLN) is an emulsion type coating carrier, and the SLN is a dispersion formed by coating an active substance in a lipid core and dispersing the active substance in a surfactant aqueous solution by taking one or more high-melting solid lipids as the carrier.
Menthol, also known as menthol, is the main component of essential oils of peppermint and is an important flavor. Menthol has a fresh mint fragrance, can stimulate cold receptors on the skin without causing actual temperature change, has the effects of local itching relieving, pain relieving, cooling and slight local anesthesia, and is widely applied to the production of foods, medicines, toothpaste, oral hygiene products, cosmetics, cigarettes and the like. In the food industry, menthol can be used as an aromatizer for foods such as beverages, cakes, candies, chewing gums and the like to improve the flavor of the foods. It can be used as irritant in medicine, and has effects in refreshing and relieving itching; it can be used for treating headache, and inflammation of nose, pharynx, and larynx by oral administration. Can be used in toothpaste and oral hygiene products for deodorizing and refreshing. In the cosmetic industry, the product can be used as a freshener, a penetration enhancer or an essence and added into products of various formulations.
However, menthol is poor in stability, volatile (especially, volatile loss is more serious under high temperature conditions), poor in water solubility (0.4mg/L), irritating to the skin and eyes, and affecting the use effect, and is a problem in being safely and effectively applied to cosmetic formulations. The volatility of the menthol can be reduced through microcapsule embedding, external components are isolated, and the menthol is released in a controlled manner, so that the effects of protecting a core material, slowly releasing, durably cooling and improving the thermal stability are achieved.
The essence and flavor microcapsule prepared by the spray drying method mostly adopts polymer wall materials, such as modified starch, Arabic gum, polyvinyl alcohol and the like, but the problems of low loading capacity, high surface oil content, poor thermal stability and the like generally exist.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made in view of the above-mentioned technical drawbacks.
Therefore, as one aspect of the present invention, the present invention overcomes the disadvantages of the prior art and provides a high-loading high-thermal stability menthol microcapsule and a preparation method thereof.
In order to solve the technical problems, the invention provides the following technical scheme: a method for preparing high-load high-thermostability menthol microcapsules comprises preparing an aqueous phase from starch octenyl succinate; preparing an oil phase from lipids and menthol; pouring the oil phase into the water phase, homogenizing under high pressure; cooling and spray drying.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the cooling rate is 0.5-1.5 ℃/min.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: and cooling, namely cooling the nano emulsion subjected to high-pressure homogenization to room temperature for more than 30 min.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the cooling medium used for cooling comprises one or more of air, water, ice, a sodium chloride solution, a potassium chloride solution, oil, liquid nitrogen, a coolant and a refrigerant.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the lipid comprises shea butter and wax, wherein the wax comprises one or more of candelilla wax, beeswax, carnauba wax, microcrystalline wax, and ozokerite; the hydrolyzed starch octenyl succinate starch comprises one or more of Capsul, Purity Gum Ultra, HI-CAP 100.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the mass ratio of the shea butter, the wax and the menthol is (1-7): (0-12): (3-15).
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the homogenizing time is 0.5-3 min, and the rotating speed is 8000-15000 rpm/min; the high pressure homogenization, which is a homogenization pressure of 800bar, is performed in 5 rounds of cycles.
As a preferred scheme of the preparation method of the high-loading high-thermal-stability menthol microcapsule, the preparation method comprises the following steps: the feeding amount of the spray drying is 20ml/min, the air inlet temperature is 180 ℃, and the air outlet temperature is 80 ℃.
As another aspect of the present invention, the present invention provides a high-load high-thermostability menthol microcapsule characterized in that: the menthol loading is more than or equal to 30 percent.
As a preferred embodiment of the high-loading high-thermal-stability menthol microcapsule of the present invention, wherein: the microcapsule can be stably stored for more than 180 days.
The invention has the beneficial effects that:
the preparation method of the menthol capsule provided by the invention has the advantages of low cost, green process, safety and simplicity. The octenyl succinic acid esterified starch is an excellent food-grade material, has good emulsifying property and film forming property, and is an ideal wall material.
According to the invention, the menthol is wrapped in the composite wall material microcapsule formed by lipid and modified starch, so that the volatility of the menthol is obviously reduced, external components are isolated, the menthol is released in a controlled manner, and the effects of protecting core materials, slowly releasing, keeping cool and improving thermal stability are achieved. The storage time is prolonged by long-acting inhibition of the crystallization of the menthol, and the application range is expanded. By regulating the occurrence state of menthol in the microcapsule, menthol microcapsules characterized by high loading (> 30%), low surface menthol (< 1%) are obtained. The lipid-modified starch composite wall material microcapsule has excellent thermal stability, the menthol released at the high temperature of 100 ℃ is less than 7 percent, and the thermal stability is obviously enhanced compared with the modified starch wall material microcapsule. XRD analysis shows that the microencapsulated menthol is in an amorphous state and still keeps the amorphous state after being hermetically stored for 180 days at room temperature, and the microcapsule after being stored for 180 days has almost no menthol leakage and still keeps excellent thermal stability.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a schematic diagram of the implementation of four cooling modes;
FIG. 2 is a graph showing the results of cooling the emulsion with liquid nitrogen;
FIG. 3 is a graph of the results of several hours after cooling the emulsion with liquid nitrogen and ice;
FIG. 4 is a graph of the results of the emulsion after cooling on ice for 3 days;
FIG. 5 is an XRD survey of the spray drying of the emulsion under different cooling conditions to form microcapsules;
FIG. 6 is a graph representing SLN in the emulsion before spray drying under the natural cooling condition of the emulsion. SLN (formed by shea butter, candelilla wax and menthol) appearance (a-c) and particle size distribution diagram (d) in the emulsion; (a) SEM picture; (b) a TEM image; (c) CLSM panel, red is nile red stained SLN; (d) the particle size distribution of SLN;
FIG. 7 is a diagram showing the appearance of microcapsules (a) and (b) formed by spray drying after the emulsion is naturally cooled; cross-sectional views (c), (d) of the microcapsules cut open;
FIG. 8 is a TEM image (a, b) and a CLSM image (c) of a green dyed starch HI-CAP 100, (d) of a red dyed SLN, (e) yellow is the overlap of the green and red channels after the emulsion has cooled down naturally and is spray dried to form microcapsules;
FIG. 9 is an SEM image of each serial number of menthol microcapsule in the example, and the left and right images are the images of each serial number under different multiples;
FIG. 10 shows the results of the thermal stability test of menthol microcapsules of each number in examples;
figure 11 is an XRD examination of menthol microcapsules prepared with different waxes and different waxes from example 3.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Surface menthol content test:
accurately weighing a certain mass m1(about 3G) of menthol microcapsules, 80mL of absolute ethanol was added, the mixture was stirred gently at room temperature for 1min with magnetic stirring, and the mixture was poured into a G3 sand-core funnel (m was weighed in advance)2) Filtering, washing with small amount of anhydrous ethanol for 3 times, air drying the sand core funnel and the filter residue in a fume hood overnight, volatilizing ethanol, and weighing3. The calculation formula of the surface menthol content is as follows:
surface menthol content ═ m1+m2-m3)/(m1X capacity)
Menthol loading test:
accurately weighing and accurately weighing a certain mass m4(about 3g) menthol microcapsules placed on petri dish m5Adding 80g of deionized water and 20g of ethanol, and drying in an oven at 100 ℃ to obtain the menthol with weight loss. Repeatedly adding deionized water and ethanol (mass ratio of 4:1), drying in oven at 100 deg.C until constant weight m6。
Menthol loading ═ m6﹣m5)/m4
In the embodiment, the core material is a composite lipid and essence or a medicament, such as shea butter, candelilla wax and menthol, the wall material comprises octenyl succinic acid esterified starch or silica and the like, and the core-wall ratio is the mass ratio of the core material to the wall material.
The theoretical loading of microcapsules refers to the mass fraction of menthol to total solids in the formulation, excluding water. Menthol is lost during the preparation process, so it is of interest to measure the actual loading. The influence of the preparation method on the retention rate of menthol can be analyzed from the comparison between the theoretical loading capacity and the actual loading capacity, and if the difference between the theoretical loading capacity and the actual loading capacity is not large, the loss of the menthol in the preparation process is small, and the retention rate is high.
Example 1:
water phase by weight: dissolving 19.2 parts of octenyl succinate starch (HI-CAP 100) in 64 parts of water, stirring for 1 hour at 90 ℃ in a constant-temperature water bath, and gelatinizing the starch to form a transparent solution; oil phase: 1.2 parts of shea butter, 3.6 parts of candelilla wax and 12 parts of menthol are stirred for 1 hour in a constant-temperature water bath at 80 ℃ until the materials are completely melted and fully mixed. Pouring the oil phase into the water phase, homogenizing for 1min with a homogenizer at a rotation speed of 10000rpm/min to obtain pre-emulsion. Homogenizing the pre-emulsion under high pressure, homogenizing under 800bar, circulating for 5 rounds to obtain hot nanoemulsion, and cooling the hot nanoemulsion. And feeding the cooled emulsion into a peristaltic pump for drying. The adopted spray drying process parameters are that the feeding amount is 20ml/min, the air inlet temperature of spray drying is 180 ℃, and the air outlet temperature is 80 ℃.
In cooling, the following cooling method is adopted in the present embodiment:
1. natural cooling
The high pressure homogenized nanoemulsion (about 200g) is at about 70-80 deg.C, and is cooled to room temperature 20-30 deg.C by standing for half an hour to 1 hour
The emulsion is naturally cooled and then spray-dried to obtain beige microcapsule powder with good fluidity and the average grain diameter of 8.12 mu m. Tests show that the menthol loading capacity is 33.33%, the encapsulation rate is 99.3%, the thermal stability is excellent, the menthol is continuously placed at 60 ℃, 80 ℃ and 100 ℃ for 12 hours, and the loss of the menthol is only 6.7%; after 12h at 100 ℃, menthol loss was 9.6%.
2. Tap water cooling
Running water is filled into the outer pipe of the spherical condenser pipe, hot nano emulsion (about 200g) is slowly poured into the inner pipe, the emulsion slowly flows down along the wall of the inner pipe, and is received by a clean beaker, and the temperature can be reduced to room temperature once after cooling.
3. Pouring tap water into the outer pipe of the spherical condenser pipe, putting the spherical condenser pipe into a refrigerator to be frozen into ice blocks, slowly pouring hot nano emulsion (about 200g) into the inner pipe, slowly flowing the emulsion down along the inner pipe wall, carrying the emulsion by using a clean beaker, and cooling once, wherein the temperature of the emulsion is lower than the room temperature finally.
After the ice blocks are cooled, the emulsion is unstable, a large amount of solid is separated out, and the spray drying is not facilitated.
4. The prepared thermal nanoemulsion (about 200g) was placed in a reaction kettle and put into liquid nitrogen for cooling for 15 min.
After the liquid nitrogen is cooled, the emulsion is excessively cooled and solidified, and after the emulsion is gradually recovered to the room temperature, a large amount of solid is separated out, so that the emulsion cannot be spray-dried. Samples that were overcooled with liquid nitrogen could not be spray dried, so freeze drying was chosen and menthol crystallized.
TABLE 1 product Condition after different cooling regimes
The preparation method takes octenyl succinic acid esterified starch as an emulsifier to emulsify an oil phase, forms thermal nano emulsion through high-pressure homogenization, has the preparation temperature of 80-90 ℃, the oil phase is in a molten oil drop state, and the thermal nano emulsion is cooled before spray drying to ensure that solid oil is cooled down to form Solid Lipid Nanoparticles (SLN), so the influence of the cooling speed is explored, and the cooling speed is as follows: natural cooling < tap water bath cooling < ice water bath cooling < liquid nitrogen cooling. The loading of the microcapsules prepared by natural cooling and tap water bath cooling is still high above 33.3%, while the emulsion is thickened and difficult to spray-dry due to overcooled ice water bath cooling and liquid nitrogen cooling, the ice water bath cooling can carry out spray-drying only marginally, but the loading of the microcapsules is only 16.31%, and the liquid nitrogen cooled emulsion cannot carry out spray-drying. The microcapsules prepared by using ice water bath or liquid nitrogen quenching have poor thermal stability. The industrial production according to the technical content of the application may need artificial cooling means. Through this application, discovery refrigerated speed has apparent influence to microcapsule preparation, and when small batch production, because the emulsion volume is few, cooling speed is fast relatively, consequently select natural cooling or water bath cooling mode can, if for industrialization mass production, consider whole cooling effect, propose increasing auxiliary cooling's means, like stirring, blast air etc. do benefit to even, quick cooling, stabilize the cooling effect of batch product, satisfy the demand that enlarges production.
The liquid nitrogen-and ice-cooled emulsion in fig. 3 was left for several hours to become a suspension of octenyl succinated starch, lipids (shea butter, candelilla wax), menthol and water. Starch is used as emulsifier, and emulsifies oil phase (lipid + menthol), and after cooling, the solid oil is solidified to form Solid Lipid Nanoparticles (SLN), namely suspension. The liquid nitrogen cooled emulsion, because the temperature was too low, solidified and the surface was like a popsicle surface with a "film" (fig. 2). The ice-cooled emulsion did not solidify completely, but formed a thin film on the surface (fig. 3), which should be formed by the starch; the lower layer is a suspension, and most of the solid is separated out.
Example 2:
dissolving water-phase octenyl succinate starch (HI-CAP 100) in water by weight, stirring for 1h in a constant-temperature water bath at 90 ℃, and gelatinizing the starch to form a transparent solution; heating oil-phase menthol in water bath at 80 deg.C to completely melt. Pouring the oil phase into the water phase, homogenizing for 1min with a homogenizer at a rotation speed of 10000rpm/min to obtain pre-emulsion. Homogenizing the pre-emulsion under high pressure, homogenizing under 800bar, circulating for 5 rounds to obtain hot nanometer emulsion, and naturally cooling to room temperature. And (3) feeding the emulsion cooled to room temperature into a peristaltic pump for spray drying, wherein the feeding amount is 20ml/min, the air inlet temperature of the spray drying is 180 ℃, the air outlet temperature is 80 ℃, and white microcapsule powder with good fluidity and the average particle size of 3.25-6.23 mu m is obtained.
TABLE 1 menthol microcapsule formulations and results
The morphology of the spray-dried particles depends on various factors such as drying kinetics and liquid phase composition. At the beginning of the drying process, the atomized droplet surface begins to dry, forming a shell, and then bubble nucleation occurs, with bubbles growing, expanding, and bursting through the surface until most of the internal moisture evaporates. Since the drying conditions were constant for all 4 formulations, the different morphology of the dried particles was only affected by their composition. The film forming property of the wall material, the interaction between the wall material and the active substance (menthol) and other factors can influence the morphology of the solid particles. As can be seen in FIG. 9, the microcapsules are spherical, with depressions, wrinkles, irregularities in the surface, and varying sizes. This is a typical feature of low load capsules, which gradually become filled and less wrinkled as the menthol load increases, but the microcapsules under formula 13 were found to break. No. 10-13 microcapsule is not added with lipid, menthol is coated by single octenyl succinic acid esterified starch, and the proportion of the menthol in the No. 10-13 microcapsule formula is as follows: the starches are, 1:9, 2:8, 3:7, 4:6 respectively, and it can be seen that as the menthol loading increases, i.e. the oil: the proportion of the emulsifier is increased, the emulsifying effect is reduced, the emulsion is unstable, and the emulsion is partially broken in the spray drying process, so that the No. 13 microcapsule is broken.
Example 3
Water phase by weight: dissolving 19.2 parts of octenyl succinated starch (HI-CAP 100) in 64 parts of water, and stirring for 1 hour in a constant temperature water bath at 90 ℃; oil phase: 1.2 parts of shea butter, 3.6 parts of wax (see Table 3) and 12 parts of menthol were stirred in a thermostatic water bath at 80 ℃ for 1 hour until they were completely melted and fully miscible. Pouring the oil phase into the water phase, homogenizing for 1min with a homogenizer at a rotation speed of 10000rpm/min to obtain pre-emulsion. Homogenizing the pre-emulsion under high pressure, homogenizing under 800bar, circulating for 5 rounds to obtain hot nanometer emulsion, and naturally cooling to room temperature. And (3) feeding the emulsion cooled to room temperature into a peristaltic pump for spray drying, wherein the feeding amount is 20ml/min, the air inlet temperature of the spray drying is 180 ℃, and the air outlet temperature is 80 ℃, so that the off-white microcapsule powder is obtained, and the fluidity is good.
TABLE 3 menthol microcapsule formulations and results
Example 4:
water phase by weight: dissolving 10 parts of octenyl succinate starch (HI-CAP 100) and 5 parts of Tween-20 (or Tween-60 or Tween-80) in 75 parts of water, and stirring for 1h in a constant-temperature water bath at 90 ℃; oil phase: 0.6 part of shea butter, 1.8 parts of candelilla wax and 7.6 parts of menthol are stirred for 1 hour in a water bath with constant temperature of 80 ℃ until the materials are completely melted and fully mixed. Pouring the oil phase into the water phase, homogenizing for 1min with a homogenizer at a rotation speed of 10000rpm/min to obtain pre-emulsion. Homogenizing the pre-emulsion under high pressure, homogenizing under 800bar, circulating for 5 rounds to obtain hot nanometer emulsion, and naturally cooling to room temperature. And (3) feeding the emulsion cooled to room temperature into a peristaltic pump for spray drying, wherein the feeding amount is 20ml/min, the air inlet temperature of the spray drying is 180 ℃, and the air outlet temperature is 80 ℃, so that the off-white microcapsule powder is obtained. In the spray drying process, the obvious findings include strong smell, much loss, poor atomization effect and serious wall sticking of the powder. As can be seen from Table 4, the compounded Tween-20/Tween-60/Tween-80 has poor effect, a great amount of menthol is lost in the process of preparing the microcapsule, and the difference between the actual loading capacity and the theoretical value is large, probably because the Tween-20/Tween-60/Tween-80 and octenyl succinic acid esterified starch in the formula have competitive adsorption, the emulsification effect is poor, and the effect of finally forming the microcapsule by spray drying is influenced.
TABLE 4 formulation of menthol microcapsules and results
| Serial number | 23 | 30 | 31 | 32 |
| Shea butter | 1.2 | 0.6 | 0.6 | 0.6 |
| Candelilla wax | 3.6 | 1.8 | 1.8 | 1.8 |
| |
12 | 7.6 | 7.6 | 7.6 |
| HI-CIP100 | 19.2 | 10 | 10 | 10 |
| Tween-60 | 5 | |||
| Tween-80 | 5 | |||
| Tween-20 | 5 | |||
| Water (W) | 64 | 75 | 75 | 75 |
| Theoretical capacity/% | 33.33 | 30.4 | 30.4 | 30.4 |
| Actual loading/% | 32.76 | 7.29 | 6.07 | 9.48 |
| SLN average particle diameter/nm | 274 | 160.4 | 96.7 | 132.3 |
| Mean particle diameter/nm of the powder dissolved in water | 716.3 | 2129 | 350 | 160 |
In order to investigate whether the addition of a surfactant can improve the emulsifying effect and reduce the SLN particle size, it was attempted to formulate a surfactant in octenyl succinate starch. Several tween surfactants were tried in this example and the microcapsules were found to perform poorly when formulated with octenyl succinate starch. The reason for the poor effect may be that the starch (large molecule) and the surfactant (small molecule) are adsorbed competitively, so that one of them is exfoliated and cannot be adsorbed on the oil-water interface. Under the conditions of the embodiment, the starch and the surfactant do not generate synergistic interaction, and the synergistic interaction can be realized by screening the types of the surfactants and determining the optimal ratio of the macromolecules and the micromolecules.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of a high-capacity high-thermal-stability menthol microcapsule is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
preparing an aqueous phase from starch esterified with octenyl succinate;
preparing an oil phase from lipids and menthol;
pouring the oil phase into the water phase, homogenizing under high pressure;
cooling and spray drying.
2. A process for the preparation of high load high thermal stability menthol microcapsules according to claim 1, characterized in that: the cooling rate is 0.5-1.5 ℃/min.
3. A process for the preparation of high load high thermal stability menthol microcapsules according to claim 1, characterized in that: and cooling, namely cooling the nano emulsion subjected to high-pressure homogenization to room temperature for more than 30 min.
4. A process for the preparation of high load high thermal stability menthol microcapsules according to claim 1, characterized in that: the cooling medium used for cooling comprises one or more of air, water, ice, a sodium chloride solution, a potassium chloride solution, oil, liquid nitrogen, a coolant and a refrigerant.
5. A process for the preparation of high load high thermal stability menthol microcapsules according to any one of claims 1 to 4, characterized in that: the lipid comprises shea butter and wax, wherein the wax comprises one or more of candelilla wax, beeswax, carnauba wax, microcrystalline wax, and ozokerite; the hydrolyzed starch octenyl succinate starch comprises one or more of Capsul, Purity Gum Ultra, HI-CAP 100.
6. A process for the preparation of high load high thermal stability menthol microcapsules according to claim 5, characterized in that: the mass ratio of the shea butter, the wax and the menthol is (1-7): (0-12): (3-15).
7. A high load high thermal stability menthol microcapsule according to any one of claims 1 to 4 and 6 and its preparation method, characterized in that: the homogenizing time is 0.5-3 min, and the rotating speed is 8000-15000 rpm/min; the high pressure homogenization, which is a homogenization pressure of 800bar, is performed in 5 rounds of cycles.
8. A process for the preparation of high load high thermal stability menthol microcapsules according to any one of claims 1 to 5 or 7, characterized in that: the feeding amount of the spray drying is 20ml/min, the air inlet temperature is 180 ℃, and the air outlet temperature is 80 ℃.
9. A high load high thermal stability menthol microcapsule according to any one of claims 1 to 8, characterized in that: the menthol loading is more than or equal to 30 percent.
10. A high load high thermal stability menthol microcapsule according to claim 9, characterized in that: the microcapsule can be stably stored for more than 180 days.
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| CN111992153B (en) | 2022-10-18 |
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