A kind of long-lasting fragrance essence microcapsule and its preparation method and application

The prepared fragrance microcapsules achieved the hierarchy of the front and back fragrances by coating different essential oils, combined with calcium carbonate, silk fibroin/silica hybrid capsules, and the compound curd method, and solved the poisoning of traditional methods The problem of curing agent improves the stability and safety of the fragrance.

CN118788258BActive Publication Date: 2024-12-17COFFEE BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411282753.6
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-09-13
Publication Date
2024-12-17
Estimated Expiration
2044-09-13

AI Technical Summary

Technical Problem

The existing fragrance microencapsulation methods are difficult to load two essential oils at the same time and the load volumes are different, making it difficult to achieve the hierarchical effects of the front and rear fragrances. The curing agents used in traditional methods such as glutaraldehyde have toxic side effects.

Method used

Different essential oils are coated by different methods. The first flavor is coated with calcium carbonate particles and then wrapped in silk fibroin/silica hybrid capsules. The second essential oil is coated with gum acacia and gelatin wall materials by the recurd method. and combine it with calcium alginate cross-linked product to prepare long-lasting fragrance microcapsules.

Benefits of technology

The release rates of different essential oils are achieved, thus presenting the layered effects of the pre-scent and post-scent fragrance, while avoiding the residue of toxic curing agents, improving the stability and safety of the fragrance.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention proposes a long-lasting fragrance type flavor microcapsule and its preparation method and application, which belongs to the field of flavor technology. The first flavor is coated in calcium carbonate particles, and then coated in silk fibroin / silicon oxide hybrid capsules, and then the calcium carbonate in the silk fibroin / silicon oxide hybrid capsules is dissolved with hydrochloric acid solution, and the second essential oil is coated in gum arabic and gelatin wall materials by a double coagulation method to obtain a second essential oil microcapsule, and the second essential oil microcapsule and the silk fibroin / silicon oxide hybrid capsule are coated together in a cross-linked product of sodium alginate and calcium to obtain a long-lasting fragrance type flavor microcapsule. After the essence of the present invention is microencapsulated, it changes from liquid to solid powder, which is conducive to storage, transportation and use; secondly, it inhibits the rapid volatilization of essential oils, increases the fragrance retention time, and expands its application range; thirdly, it protects sensitive components in the essence. Many components in the essence are sensitive to light, heat, acid, etc., and microencapsulation can reduce the reaction of the essence with the outside world.
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Description

Technical Field

[0001] The invention relates to the technical field of flavors, and in particular to a long-lasting fragrance-retaining flavor microcapsule and a preparation method and application thereof. Background Art

[0002] Fragrances are widely used in textiles, food, cosmetics and other fields due to their unique fragrance. However, most flavors are highly volatile and have poor stability, which limits their practical application. Microencapsulation of flavors can overcome these problems. Coating the flavors with polymer films can effectively reduce the volatility of the flavors, prevent the flavors from oxidizing, deteriorating and losing under external conditions, and improve the stability of the flavors.

[0003] The main methods for microencapsulation of flavors include in-situ polymerization, complex coacervation, interfacial polymerization, etc. The in-situ polymerization method is mainly based on melamine resin and urea-formaldehyde resin, and its advantages are simple encapsulation process, dense microcapsule shell and good thermal stability. The complex coacervation method mainly uses gelatin, chitosan, gum arabic, sodium alginate and other monomers as wall material monomers. These monomer raw materials are cheap and environmentally friendly, but they need to be cured with glutaraldehyde, etc., and the prepared microcapsules have poor thermal stability, low embedding rate and poor durability. Formaldehyde or glutaraldehyde will cause the residue of irritating substances, which have toxic side effects on the eyes, respiratory, nervous and endocrine systems. The polyurethane and polyurea shell microcapsules prepared by interfacial polymerization can effectively avoid the problem of free formaldehyde in microcapsules from the root, and have the advantages of simple encapsulation process, low reaction temperature and high coverage rate. Summary of the invention

[0004] In order to solve the problem of being able to load two essential oils at the same time with different loading amounts of the two essential oils, the present invention adopts different methods to encapsulate different essential oils, and proposes a long-lasting fragrance-retaining flavor microcapsule and a preparation method and application thereof. By encapsulating different essential oils by different methods, different release rates of different essential oils can be achieved, thereby presenting the layers of front fragrance and after fragrance.

[0005] The technical solution of the present invention is achieved in this way:

[0006] The invention provides a preparation method of a long-lasting fragrance essence microcapsule. The method comprises the following steps: coating a first essence in calcium carbonate particles, and then coating the first essence in a silk fibroin / silicon oxide hybrid capsule, dissolving the calcium carbonate in the silk fibroin / silicon oxide hybrid capsule with a hydrochloric acid solution, coating a second essential oil in a gum arabic and gelatin wall material by a double coagulation method to obtain a second essential oil microcapsule, and coating the second essential oil microcapsule and the silk fibroin / silicon oxide hybrid capsule together in a cross-linked product of sodium alginate and calcium to obtain a long-lasting fragrance essence microcapsule.

[0007] As a further improvement of the present invention, the following steps are included:

[0008] S1. Preparation of calcium carbonate particles coated with the first flavor: adding the first flavor and sodium polystyrene sulfonate to water, adding calcium salt, stirring and mixing, dropping sodium carbonate solution, stirring the reaction, standing, centrifuging, washing, and drying to obtain calcium carbonate particles coated with the first flavor;

[0009] S2. Preparation of silk fibroin / silicon oxide hybrid capsules: dissolving silk fibroin peptide in PBS solution, adding calcium carbonate particles coated with the first flavor, stirring and mixing evenly to obtain a suspension; dissolving sodium silicate in water, adjusting the pH value, and obtaining a sodium silicate solution; adding the obtained sodium silicate solution to the suspension, stirring for reaction, and then centrifuging, washing, drying, and then adding to a hydrochloric acid solution, reacting, centrifuging, washing, and drying to obtain a silk fibroin / silicon oxide hybrid capsule;

[0010] S3. Preparation of a second essential oil microcapsule: adding gum arabic and gelatin to water, stirring and mixing, adding a second essential oil, shearing, heating, adjusting the pH value of the solution to a first pH value, stirring the reaction, cooling, adjusting the pH value of the solution to a second pH value, adding a curing agent, curing, and freeze-drying to obtain a second essential oil microcapsule;

[0011] S4. Preparation of long-lasting fragrance microcapsules: dissolve sodium alginate in water, then add silk fibroin / silicon oxide hybrid capsules, second essential oil microcapsules and emulsifiers, mix well and drop into fish oil, emulsify, add calcium chloride solution, solidify at room temperature, centrifuge, wash, and dry to obtain long-lasting fragrance microcapsules.

[0012] As a further improvement of the present invention, the calcium salt in step S1 is calcium chloride, the mass ratio of the first flavor, sodium polystyrene sulfonate, calcium chloride and sodium carbonate is 3-4:0.1-0.2:10-12:10-11, the stirring reaction time is 30-60s, and the standing time is 20-30min.

[0013] As a further improvement of the present invention, the first fragrance is selected from at least one of rose oil, marigold oil, white jasmine oil, ylang-ylang oil, immortelle oil, lavender oil, clary sage oil, clove oil and rosemary oil.

[0014] As a further improvement of the present invention, the pH value of the PBS solution in step S2 is 7-7.2, the adjusted pH value is 7.5-8, the mass ratio of the silk fibroin peptide, the calcium carbonate particles coated with the first fragrance, and the sodium silicate is 2-3:4-6:7-9, the stirring reaction time is 15-30 min, and the concentration of the hydrochloric acid solution is 0.1-0.3 mol / L.

[0015] As a further improvement of the present invention, the mass ratio of gum arabic, gelatin, the second essential oil and the curing agent in step S3 is 10-12:10-12:4-7:0.5-1, the shearing speed is 7000-8000r / min, the time is 10-20min, the heating temperature is 35-45°C, the cooling temperature is 10-15°C, the curing time is 2-4h, the stirring reaction time is 10-20min, the first pH value is 3.5-4.5, the second pH value is 5.5-6.5, and the curing agent is glutamine transaminase.

[0016] As a further improvement of the present invention, the second essential oil is wormwood essential oil.

[0017] As a further improvement of the present invention, the mass ratio of the sodium alginate, the silk fibroin / silicon oxide hybrid capsule, the second essential oil microcapsule and the emulsifier in step S4 is 9-11:3-5:6-8:0.5-1, the emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80 and Tween-85, and the room temperature curing time is 20-40 min.

[0018] The present invention further protects a kind of long-lasting fragrance-retaining essence microcapsule prepared by the above-mentioned preparation method.

[0019] The present invention further protects the application of the above-mentioned long-lasting fragrance microcapsule in cosmetics and textiles.

[0020] The present invention has the following beneficial effects:

[0021] After the essence is microencapsulated, the physical state of the essence can be changed. After microencapsulation, the essence changes from liquid to solid powder, which is conducive to storage, transportation and use; secondly, it inhibits the rapid volatilization of essential oils, increases the fragrance retention time, and expands its application range; thirdly, it protects the sensitive ingredients in the essence. Many components in the essence are sensitive to light, heat, acid, etc. Microencapsulation can reduce the reaction of the essence with the outside world.

[0022] In the present invention, the first essential oil, such as natural essences such as rose oil, marigold oil, white jasmine oil, ylang-ylang oil, immortelle oil, lavender oil, clary sage oil, clove oil and rosemary oil, can produce a strong aroma by volatilizing a small amount. A small amount of the first essential oil can achieve the effect of adjusting the fragrance.

[0023] The aroma of the second essential oil, wormwood essential oil, is not as strong as the first essential oil, but the second essential oil needs to be used as the after-tune aroma, and a large amount of wormwood essential oil needs to be loaded. The ordinary addition ratio of the essential oil cannot meet the presentation of the front and back aromas. The present invention embeds different essential oils by different methods, and can achieve different release rates of different essential oils, thereby presenting the layers of the front and back aromas.

[0024] In order to solve the problem of being able to load two essential oils at the same time and the two essential oils have different loading amounts, the present invention uses different methods to coat different essential oils. The present invention adopts a biomimetic method to prepare a silk fibroin / silicon oxide hybrid capsule that can load a first essential oil with a smaller amount. The biosilicification process can only be carried out through the induction of biomacromolecules. Since the biomimetic silicification process can be carried out under relatively mild conditions, it has good structural controllability and carrier material biocompatibility.

[0025] In the absence of polyelectrolyte additives, the 2+ and CO3 2- The morphology of CaCO3 precipitated from the supersaturated solution is often calcite crystal type with sharp edges and corners, which is not conducive to the subsequent formation of microcapsules. Adding a small amount of sodium polystyrene sulfonate can reduce the size of the obtained crystal particles and make them spherical. The prepared calcium carbonate template has negative charge and can be better loaded in the silk fibroin / silicon oxide hybrid capsule wall material.

[0026] The present invention adopts the double coagulation method to load the second essential oil, and the polymer wall material with opposite potential generates electrostatic action to achieve the purpose of reducing solvent concentration and phase separation. Since the microsphere particles prepared by the double coagulation method are larger, more essential oil can be loaded, which meets the needs of the present invention. DETAILED DESCRIPTION

[0027] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0028] Silk fibroin peptide, content>99%, white powder, purchased from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.

[0029] Example 1

[0030] This embodiment provides a method for preparing a long-lasting fragrance microcapsule, comprising the following steps:

[0031] S1. Preparation of calcium carbonate particles coated with clove oil: 3 g of clove oil and 0.1 g of sodium polystyrene sulfonate were added to 200 mL of water, 10 g of calcium chloride was added, and the mixture was stirred for 10 min. 200 mL of a solution containing 10 g of sodium carbonate was added dropwise, and the mixture was stirred for 30 s. The mixture was allowed to stand for 20 min, centrifuged, washed, and dried to obtain calcium carbonate particles coated with clove oil;

[0032] S2. Preparation of silk fibroin / silicon oxide hybrid capsules: 2 g of silk fibroin peptide was dissolved in 200 mL of PBS solution with a pH value of 7, 4 g of calcium carbonate particles coated with clove oil were added, and the mixture was stirred for 10 min to obtain a suspension; 7 g of sodium silicate was dissolved in 200 mL of water, and the pH value was adjusted to 7.5 to obtain a sodium silicate solution; the solution was added to the suspension, stirred for reaction for 15 min, and then centrifuged, washed, dried, and added to 200 mL of 0.1 mol / L dilute hydrochloric acid solution, reacted for 30 min, centrifuged, washed, and dried to obtain silk fibroin / silicon oxide hybrid capsules;

[0033] S3. Preparation of wormwood essential oil microcapsules: 10 g of gum arabic and 10 g of gelatin were added to 1000 mL of water, stirred and mixed, 4 g of wormwood essential oil was added, sheared at 7000 r / min for 10 min, heated to 35 ° C, the pH value of the solution was adjusted to 3.5, stirred for 10 min, cooled to 10 ° C, the pH value of the solution was adjusted to 5.5, 0.5 g of glutamine transaminase was added, solidified for 2 h, and freeze-dried to obtain wormwood essential oil microcapsules;

[0034] S4. Preparation of long-lasting fragrance essence microcapsules: Dissolve 9g sodium alginate in 500mL water, add 3g silk fibroin / silicon oxide hybrid capsules, 6g mugwort essential oil microcapsules and 0.5g Tween-40, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, solidify at room temperature for 20min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0035] Example 2

[0036] This embodiment provides a method for preparing a long-lasting fragrance microcapsule, comprising the following steps:

[0037] S1. Preparation of calcium carbonate particles coated with lavender oil: 4 g of lavender oil and 0.2 g of sodium polystyrene sulfonate were added to 200 mL of water, 12 g of calcium chloride was added, and the mixture was stirred for 10 min. 200 mL of a solution containing 11 g of sodium carbonate was added dropwise, and the mixture was stirred for 60 s. The mixture was allowed to stand for 30 min, centrifuged, washed, and dried to obtain calcium carbonate particles coated with lavender oil;

[0038] S2. Preparation of silk fibroin / silicon oxide hybrid capsules: 3 g of silk fibroin peptide was dissolved in 200 mL of PBS solution with a pH value of 7.2, 6 g of calcium carbonate particles coated with lavender oil were added, and the mixture was stirred for 10 min to obtain a suspension; 9 g of sodium silicate was dissolved in 200 mL of water, and the pH value was adjusted to 8 to obtain a sodium silicate solution; the solution was added to the suspension, stirred for reaction for 30 min, and then centrifuged, washed, dried, and added to 200 mL of 0.3 mol / L dilute hydrochloric acid solution, reacted for 50 min, centrifuged, washed, and dried to obtain silk fibroin / silicon oxide hybrid capsules;

[0039] S3. Preparation of wormwood essential oil microcapsules: 12 g of gum arabic and 12 g of gelatin were added to 1000 mL of water, stirred and mixed, 7 g of wormwood essential oil was added, sheared at 8000 r / min for 20 min, heated to 45 ° C, the pH value of the solution was adjusted to 4.5, stirred and reacted for 20 min, cooled to 15 ° C, the pH value of the solution was adjusted to 6.5, 1 g of glutamine transaminase was added, solidified for 4 h, and freeze-dried to obtain wormwood essential oil microcapsules;

[0040] S4. Preparation of long-lasting fragrance essence microcapsules: Dissolve 11g sodium alginate in 500mL water, add 5g silk fibroin / silicon oxide hybrid capsules, 8g wormwood essential oil microcapsules and 1g Tween-40, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, cure at room temperature for 40min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0041] Example 3

[0042] This embodiment provides a method for preparing a long-lasting fragrance microcapsule, comprising the following steps:

[0043] S1. Preparation of rose oil-coated calcium carbonate particles: 3.5 g of rose oil and 0.15 g of sodium polystyrene sulfonate were added to 200 mL of water, 11 g of calcium chloride was added, and the mixture was stirred for 10 min. 200 mL of a sodium carbonate solution containing 10.5 g was added dropwise, and the mixture was stirred for 45 s. The mixture was allowed to stand for 25 min, centrifuged, washed, and dried to obtain rose oil-coated calcium carbonate particles.

[0044] S2. Preparation of silk fibroin / silicon oxide hybrid capsules: 2.5 g of silk fibroin peptide was dissolved in 200 mL of PBS solution with a pH value of 7.1, 5 g of calcium carbonate particles coated with rose oil were added, and the mixture was stirred for 10 min to obtain a suspension; 8 g of sodium silicate was dissolved in 200 mL of water, and the pH value was adjusted to 7.7 to obtain a sodium silicate solution; the solution was added to the suspension, stirred for reaction for 20 min, and then centrifuged, washed, dried, and added to 200 mL of 0.2 mol / L dilute hydrochloric acid solution, reacted for 40 min, centrifuged, washed, and dried to obtain silk fibroin / silicon oxide hybrid capsules;

[0045] S3. Preparation of wormwood essential oil microcapsules: 11 g of gum arabic and 11 g of gelatin were added to 1000 mL of water, stirred and mixed, 5.5 g of wormwood essential oil was added, sheared at 7500 r / min for 15 min, heated to 40 ° C, the pH value of the solution was adjusted to 4, stirred and reacted for 15 min, cooled to 12 ° C, the pH value of the solution was adjusted to 6, 0.7 g of glutamine transaminase was added, solidified for 3 h, and freeze-dried to obtain wormwood essential oil microcapsules;

[0046] S4. Preparation of long-lasting fragrance essence microcapsules: Dissolve 10g sodium alginate in 500mL water, add 4g silk fibroin / silicon oxide hybrid capsules, 7g wormwood essential oil microcapsules and 0.7g Tween-85, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, solidify at room temperature for 30min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0047] Comparative Example 1

[0048] Compared with Example 3, the difference lies in that the rose oil is coated by the double coagulation method.

[0049] The details are as follows:

[0050] S1. Preparation of rose oil microcapsules: 11 g of gum arabic and 11 g of gelatin were added to 1000 mL of water, stirred and mixed, 5.5 g of rose oil was added, sheared at 7500 r / min for 15 min, heated to 40°C, the pH value of the solution was adjusted to 4, stirred and reacted for 15 min, cooled to 12°C, the pH value of the solution was adjusted to 6, 0.7 g of glutamine transaminase was added, solidified for 3 h, and freeze-dried to obtain rose oil microcapsules;

[0051] S2. Preparation of wormwood essential oil microcapsules: 11 g of gum arabic and 11 g of gelatin were added to 1000 mL of water, stirred and mixed, 5.5 g of wormwood essential oil was added, sheared at 7500 r / min for 15 min, heated to 40 ° C, the pH value of the solution was adjusted to 4, stirred and reacted for 15 min, cooled to 12 ° C, the pH value of the solution was adjusted to 6, 0.7 g of glutamine transaminase was added, solidified for 3 h, and freeze-dried to obtain wormwood essential oil microcapsules;

[0052] S3. Preparation of long-lasting fragrance essence microcapsules: Dissolve 10g sodium alginate in 500mL water, add 4g rose oil microcapsules, 7g wormwood essential oil microcapsules and 0.7g Tween-85, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, solidify at room temperature for 30min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0053] Comparative Example 2

[0054] Compared with Example 3, the difference lies in that rose oil and wormwood essential oil are directly encapsulated in sodium alginate.

[0055] The details are as follows:

[0056] Preparation of long-lasting fragrance flavor microcapsules: 10g sodium alginate is dissolved in 500mL water, 4g rose oil, 7g wormwood essential oil and 0.7g Tween-85 are added, and the mixture is added dropwise to 1L fish oil. Emulsification is performed at 5000r / min for 15min, and 10mL 3wt% calcium chloride solution is added dropwise. The mixture is cured at room temperature for 30min, centrifuged, washed and dried to obtain long-lasting fragrance flavor microcapsules.

[0057] Comparative Example 3

[0058] Compared with Example 3, the difference lies in that the rose oil is coated by the double coagulation method, and the wormwood essential oil is directly coated in the sodium alginate.

[0059] The details are as follows:

[0060] S1. Preparation of rose oil microcapsules: 11 g of gum arabic and 11 g of gelatin were added to 1000 mL of water, stirred and mixed, 5.5 g of rose oil was added, sheared at 7500 r / min for 15 min, heated to 40°C, the pH value of the solution was adjusted to 4, stirred and reacted for 15 min, cooled to 12°C, the pH value of the solution was adjusted to 6, 0.7 g of glutamine transaminase was added, solidified for 3 h, and freeze-dried to obtain rose oil microcapsules;

[0061] S2. Preparation of long-lasting fragrance essence microcapsules: dissolve 10g sodium alginate in 500mL water, add 4g rose oil microcapsules, 7g wormwood essential oil and 0.7g Tween-85, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, solidify at room temperature for 30min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0062] Comparative Example 4

[0063] Compared with Example 3, the difference lies in that the mugwort essential oil is coated by the double coagulation method, and the rose oil is directly coated in the sodium alginate.

[0064] The details are as follows:

[0065] S1. Preparation of wormwood essential oil microcapsules: 11 g of gum arabic and 11 g of gelatin were added to 1000 mL of water, stirred and mixed, 5.5 g of wormwood essential oil was added, sheared at 7500 r / min for 15 min, heated to 40 ° C, the pH value of the solution was adjusted to 4, stirred and reacted for 15 min, cooled to 12 ° C, the pH value of the solution was adjusted to 6, 0.7 g of glutamine transaminase was added, solidified for 3 h, and freeze-dried to obtain wormwood essential oil microcapsules;

[0066] S2. Preparation of long-lasting fragrance essence microcapsules: Dissolve 10g sodium alginate in 500mL water, add 4g rose oil, 7g wormwood essential oil microcapsules and 0.7g Tween-85, add dropwise into 1L fish oil, emulsify at 5000r / min for 15min, add dropwise 10mL 3wt% calcium chloride solution, solidify at room temperature for 30min, centrifuge, wash and dry to obtain long-lasting fragrance essence microcapsules.

[0067] Test Example 1 Determination of embedding rate

[0068] Pour 1g (accurate to 2 decimal places) of the long-lasting fragrance microcapsules (mass: m 1) Place it in an electric hot air drying oven at 80°C and dry it to constant weight, then take it out and weigh it again. m 2. The mass of the empty evaporating dish is m 0, according to formula (1) to calculate the embedding rate ( E ):

[0069] E =1-[( m 1- m 2)- β ( m 1- m 0)] / [1- α ( m 1- m0)]×100%(1)

[0070] Where: α Represents the mass fraction of the core material essence or essential oil in the sample microcapsule emulsion; β Represents the mass fraction of volatile components other than essence or essential oil in the sample microcapsule emulsion.

[0071] The results are shown in Table 1.

[0072] Table 1

[0073]

[0074] It can be seen from the above table that the long-lasting fragrance microcapsules prepared in Examples 1-3 of the present invention have a higher embedding rate.

[0075] Test Example 2 Sustained Release Performance Test

[0076] The sustained-release performance of the long-lasting fragrance microcapsules prepared in Examples 1-3 of the present invention and Comparative Examples 1-4 was tested.

[0077] (1) Sensory representation

[0078] Five people who are sensitive to the fragrance intensity were selected to evaluate the fragrance intensity of the samples, and the average value was taken as the final evaluation result. The evaluation results were divided into 5 levels, and the fragrance intensity was divided into 1-5 levels (level 1, very light fragrance; level 2, light fragrance; level 3, medium fragrance; level 4, strong fragrance; level 5, very strong fragrance). The evaluation period was 120 days. The results are shown in Table 2.

[0079] Table 2

[0080]

[0081] It can be seen from the above table that the long-lasting fragrance-type essence microcapsules prepared in Examples 1-3 of the present invention can still maintain good fragrance release over a longer period.

[0082] The constant temperature weight loss test places the microcapsules in a 120℃ environment for a certain period of time, and takes out the microcapsules and weighs them at regular intervals. The mass loss rate before and after the microcapsule treatment is used to characterize the sustained release performance of the flavor microcapsules. The evaluation cycle is 12 hours.

[0083] The calculation formula is shown in formula (2).

[0084] Mass loss rate (%) = (M1-M2) / M1 (2)

[0085] Where: M1 is the mass of the aromatic microcapsules before treatment, g; M2 is the mass of the aromatic microcapsules after treatment, g.

[0086] The results are shown in Table 3.

[0087] Table 3

[0088]

[0089] It can be seen from the above table that the long-lasting fragrance-retaining essence microcapsules prepared in Examples 1-3 of the present invention have good heat resistance stability and good sustained-release effect.

[0090] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a long-lasting fragrance microcapsule, characterized in that: The following steps are involved: S1. Preparation of calcium carbonate particles coated with the first flavor: adding the first flavor and sodium polystyrene sulfonate to water, adding calcium salt, stirring and mixing, dropping sodium carbonate solution, stirring the reaction, standing, centrifuging, washing, and drying to obtain calcium carbonate particles coated with the first flavor; S2. Preparation of silk fibroin / silicon oxide hybrid capsules: dissolving silk fibroin peptide in PBS solution, adding calcium carbonate particles coated with the first flavor, stirring and mixing evenly to obtain a suspension; dissolving sodium silicate in water, adjusting the pH value, and obtaining a sodium silicate solution; adding the obtained sodium silicate solution to the suspension, stirring for reaction, and then centrifuging, washing, drying, and then adding to a hydrochloric acid solution, reacting, centrifuging, washing, and drying to obtain a silk fibroin / silicon oxide hybrid capsule; S3. Preparation of a second essential oil microcapsule: adding gum arabic and gelatin to water, stirring and mixing, adding a second essential oil, shearing, heating, adjusting the pH value of the solution to a first pH value, stirring the reaction, cooling, adjusting the pH value of the solution to a second pH value, adding a curing agent, curing, and freeze-drying to obtain a second essential oil microcapsule; S4. Preparation of long-lasting fragrance microcapsules: dissolve sodium alginate in water, then add silk fibroin / silicon oxide hybrid capsules, second essential oil microcapsules and emulsifiers, mix well and drop into fish oil, emulsify, add calcium chloride solution, solidify at room temperature, centrifuge, wash, and dry to obtain long-lasting fragrance microcapsules.

2. The preparation method according to claim 1, characterized in that In step S1, the calcium salt is calcium chloride, the mass ratio of the first flavor, sodium polystyrene sulfonate, calcium chloride and sodium carbonate is (3-4): (0.1-0.2): (10-12): (10-11), the stirring reaction time is 30-60s, and the standing time is 20-30min.

3. The preparation method according to claim 1, characterized in that: The first fragrance is selected from at least one of rose oil, marigold oil, white jasmine oil, ylang-ylang oil, immortelle oil, lavender oil, clary sage oil, clove oil and rosemary oil.

4. The preparation method according to claim 1, characterized in that The pH value of the PBS solution in step S2 is 7-7.2, the adjusted pH value is 7.5-8, the mass ratio of the silk fibroin peptide, the calcium carbonate particles coated with the first fragrance, and the sodium silicate is (2-3): (4-6): (7-9), the stirring reaction time is 15-30 min, and the concentration of the hydrochloric acid solution is 0.1-0.3 mol / L.

5. The preparation method according to claim 1, characterized in that The mass ratio of gum arabic, gelatin, the second essential oil and the curing agent in step S3 is (10-12): (10-12): (4-7): (0.5-1), the shearing speed is 7000-8000r / min, the shearing time is 10-20min, the heating temperature is 35-45°C, the cooling temperature is 10-15°C, the curing time is 2-4h, the stirring reaction time is 10-20min, the first pH value is 3.5-4.5, the second pH value is 5.5-6.5, and the curing agent is glutamine transaminase.

6. The preparation method according to claim 1, characterized in that: The second essential oil is wormwood essential oil.

7. The preparation method according to claim 1, characterized in that The mass ratio of the sodium alginate, the silk fibroin / silicon oxide hybrid capsule, the second essential oil microcapsule and the emulsifier in step S4 is (9-11): (3-5): (6-8): (0.5-1), the emulsifier is selected from at least one of Tween-20, Tween-40, Tween-60, Tween-80 and Tween-85, and the room temperature curing time is 20-40 min.

8. A long-lasting fragrance microcapsule obtained by the preparation method according to any one of claims 1 to 7.

9. Use of the long-lasting fragrance microcapsule according to claim 8 in cosmetics and textiles.