CN118788258B - Lasting fragrance-retaining essence microcapsule and preparation method and application thereof - Google Patents
Lasting fragrance-retaining essence microcapsule and preparation method and application thereof Download PDFInfo
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- 230000002045 lasting effect Effects 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000000341 volatile oil Substances 0.000 claims abstract description 70
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 48
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- 238000000034 method Methods 0.000 claims abstract description 29
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- 239000004115 Sodium Silicate Substances 0.000 claims description 16
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 16
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 16
- 240000006891 Artemisia vulgaris Species 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
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- 229940006186 sodium polystyrene sulfonate Drugs 0.000 claims description 8
- 239000001110 calcium chloride Substances 0.000 claims description 7
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 7
- 239000010634 clove oil Substances 0.000 claims description 7
- 239000000171 lavandula angustifolia l. flower oil Substances 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 241000233855 Orchidaceae Species 0.000 claims description 6
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- 159000000007 calcium salts Chemical class 0.000 claims description 4
- 239000002537 cosmetic Substances 0.000 claims description 3
- 239000010653 helichrysum oil Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 239000010668 rosemary oil Substances 0.000 claims description 3
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- 239000001138 artemisia absinthium Substances 0.000 description 14
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 14
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a lasting fragrance-retaining essence microcapsule, and a preparation method and application thereof, and belongs to the technical field of essences. Coating the first essence in calcium carbonate particles, then coating the calcium carbonate particles in silk fibroin/silicon oxide hybrid capsules, dissolving calcium carbonate in the silk fibroin/silicon oxide hybrid capsules by using hydrochloric acid solution, coating the second essential oil in Arabic gum and gelatin wall materials by adopting a double-curd method to prepare second essential oil microcapsules, and coating the second essential oil microcapsules and the silk fibroin/silicon oxide hybrid capsules together in crosslinked products of sodium alginate and calcium to prepare the lasting fragrance type essence microcapsules. The essence is microencapsulated and then is changed into solid powder from liquid state, which is beneficial to storage, transportation and use, secondly, the quick volatilization of the essential oil is inhibited, the fragrance retention time is prolonged, the application range is enlarged, thirdly, the sensitive ingredients in the essence are protected, a plurality of components in the essence are sensitive to light, heat, acid and the like, and the reaction between the essence and the outside can be reduced after the microencapsulation.
Description
Technical Field
The invention relates to the technical field of essence, in particular to a lasting fragrance-retaining essence microcapsule, and a preparation method and application thereof.
Background
The essence is widely used in the fields of textile, food, cosmetics and the like due to the unique fragrance, however, most essences have high volatility and poor stability and are limited in practical application. The problems can be overcome by microencapsulating the essence, the volatilization rate of the essence can be effectively reduced by coating the essence with the polymer film, the oxidation deterioration and loss of the essence under the external condition are prevented, and the stability of the essence is improved.
The perfume microencapsulation method mainly comprises an in-situ polymerization method, a complex coacervation method, an interfacial polymerization method and the like. The in-situ polymerization method mainly uses melamine resin and urea resin, and has the advantages of simple encapsulation process, compact microcapsule shell and good thermal stability. The complex coacervation method mainly uses gelatin, chitosan, acacia, sodium alginate and the like as wall material monomers, and the monomer raw materials are low in cost and environment-friendly, but glutaraldehyde and the like are needed to be used for solidification, and the prepared microcapsule has poor thermal stability, low embedding rate and poor durability. Formaldehyde or glutaraldehyde and the like can cause the residue of irritant substances, and has toxic and side effects on eyes, respiration, nerves, endocrine and the like. The polyurethane and polyurea shell microcapsule prepared by the interfacial polymerization method can radically and effectively avoid the problem of free formaldehyde in the microcapsule, and has the advantages of simple encapsulation process, low reaction temperature and high coating rate.
Disclosure of Invention
In order to solve the problem that two kinds of essential oils can be loaded simultaneously and the loading amounts of the two kinds of essential oils are different, different essential oils are coated by adopting different methods, the invention provides a lasting fragrance-retaining essence microcapsule, a preparation method and application thereof, and different essential oils are embedded by different methods, so that different release rates of the different essential oils can be realized, and the levels of front fragrance and rear fragrance are presented.
The technical scheme of the invention is realized as follows:
The invention provides a preparation method of a lasting fragrance type essence microcapsule, which comprises the steps of coating a first essence in calcium carbonate particles, then coating the calcium carbonate particles in a silk fibroin/silicon oxide hybrid capsule, dissolving calcium carbonate in the silk fibroin/silicon oxide hybrid capsule by using a hydrochloric acid solution, coating second essential oil in Arabic gum and gelatin wall materials by adopting a double-curd method to prepare a second essential oil microcapsule, and coating the second essential oil microcapsule and the silk fibroin/silicon oxide hybrid capsule in a crosslinked product of sodium alginate and calcium to prepare the lasting fragrance type essence microcapsule.
As a further improvement of the invention, the method comprises the following steps:
S1, preparing calcium carbonate particles coated with a first essence, namely adding the first essence and sodium polystyrene sulfonate into water, adding calcium salt, stirring and mixing uniformly, dripping sodium carbonate solution, stirring and reacting, standing, centrifuging, washing and drying to obtain the calcium carbonate particles coated with the first essence;
S2, preparing a silk fibroin/silicon oxide hybrid capsule, namely dissolving silk fibroin peptide in PBS solution, adding calcium carbonate particles coated with first essence, stirring and uniformly mixing to prepare suspension, dissolving sodium silicate in water, regulating pH value to prepare sodium silicate solution, adding the prepared sodium silicate solution into the suspension, stirring and reacting, centrifuging, washing, drying, adding into hydrochloric acid solution, reacting, centrifuging, washing, and drying to prepare the silk fibroin/silicon oxide hybrid capsule;
S3, preparing a second essential oil microcapsule, namely adding Arabic gum and gelatin into water, stirring and mixing uniformly, adding the second essential oil, shearing, heating, adjusting the pH value of the solution to be a first pH value, stirring and reacting, cooling, adjusting the pH value of the solution to be a second pH value, adding a curing agent, curing, and freeze-drying to prepare the second essential oil microcapsule;
S4, preparing the lasting fragrance type essence microcapsule, namely dissolving sodium alginate in water, adding the silk fibroin/silicon oxide hybrid capsule, the second essential oil microcapsule and the emulsifying agent, uniformly mixing, then dropwise adding the mixture into fish oil, emulsifying, dropwise adding a calcium chloride solution, solidifying at normal temperature, centrifuging, washing and drying to prepare the lasting fragrance type essence microcapsule.
As a further improvement of the invention, the calcium salt in the step S1 is calcium chloride, the mass ratio of the first essence to the sodium polystyrene sulfonate to the calcium chloride to the 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.
As a further improvement of the present invention, the first essence is at least one selected from the group consisting of rose oil, tree orchid oil, white orchid oil, ylang oil, helichrysum oil, lavender oil, sclareum oil, clove oil and rosemary oil.
As a further improvement of the invention, in the step S2, the pH value of the PBS solution is 7-7.2, the pH value is adjusted to 7.5-8, the mass ratio of the silk fibroin peptide to the calcium carbonate particles coated with the first essence to the sodium silicate is 2-3:4-6:7-9, the stirring reaction time is 15-30min, and the concentration of the hydrochloric acid solution is 0.1-0.3mol/L.
As a further improvement of the invention, in the step S3, the mass ratio of the Arabic gum, the gelatin, the second essential oil and the curing agent is 10-12:10-12:4-7:0.5-1, the shearing rotating speed is 7000-8000r/min, the time is 10-20min, the heating temperature is 35-45 ℃, the cooling temperature is 10-15 ℃, 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.
As a further improvement of the present invention, the second essential oil is mugwort essential oil.
As a further improvement of the invention, in the step S4, the mass ratio of the sodium alginate to the silk fibroin/silicon oxide hybrid capsule to the second essential oil microcapsule to the emulsifier is 9-11:3-5:6-8:0.5-1, the emulsifier is at least one selected from tween-20, tween-40, tween-60, tween-80 and tween-85, and the normal temperature curing time is 20-40min.
The invention further protects the lasting fragrance-retaining essence microcapsule prepared by the preparation method.
The invention further protects the application of the lasting fragrance type essence microcapsule in cosmetics and textiles.
The invention has the following beneficial effects:
The essence can change the physical state of the essence after microencapsulation, and is changed into solid powder from liquid state after microencapsulation, thereby being beneficial to storage, transportation and use, inhibiting the quick volatilization of essential oil, improving the fragrance retention time, expanding the application range of the essential oil, protecting the sensitive components in the essence, having a plurality of components sensitive to light, heat, acid and the like, and reducing the reaction of the essence with the outside after microencapsulation.
In the invention, the first essential oil such as rose oil, tree orchid oil, white orchid oil, ylang oil, helichrysum oil, lavender oil, sclareum oil, clove oil and rosemary oil can generate strong fragrance by adopting a small amount of volatilization. The first essential oil can be used for regulating the fragrance.
The aroma of the second essential oil mugwort essential oil is not as intense as the first essential oil, but the second essential oil is required to be used as the post-adjusting aroma, and a large amount of mugwort essential oil is required to be loaded. The invention can realize different release rates of different essential oils by embedding different essential oils through different methods, thereby presenting the layers of front fragrance and rear fragrance.
In order to solve the problem that two kinds of essential oil can be loaded simultaneously and the loading amounts of the two kinds of essential oil are different, different methods are adopted to coat different essential oils. The silk fibroin/silicon oxide hybrid capsule is prepared by adopting a bionic method, and can load less first essential oil. The bio-siliconizing process is performed by induction of bio-macromolecules. Because the bionic siliconizing process can be carried out under a milder condition, the structure controllability and the carrier material biocompatibility are good.
Under the condition of no polyelectrolyte additive, caCO 3 precipitated from supersaturated solution containing Ca 2+ and CO 3 2- is often in calcite crystal form, the edges and corners are clear, the formation of subsequent microcapsules is not facilitated, the size of the obtained crystal particles can be reduced by adding a small amount of sodium polystyrene sulfonate, the crystal particles are spherical, the prepared calcium carbonate template has electronegativity, and can be better loaded in silk fibroin/silicon oxide hybrid capsule wall materials.
The invention adopts a double-curd method to load the second essential oil, and achieves the aims of reducing the concentration of the solvent and separating phases by enabling the polymer wall materials with opposite electric potentials to generate electrostatic action. Because the microsphere particles prepared by the double-curd method are larger, more essential oil can be loaded, and the requirements of the invention are met.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Silk fibroin peptide, content >99%, white powder, purchased from wuhan Hua Xiangke biotechnology limited.
Example 1
The embodiment provides a preparation method of a lasting fragrance type essence microcapsule, which comprises the following steps:
S1, preparing calcium carbonate particles coated with clove oil, namely adding 3g of clove oil and 0.1g of sodium polystyrene sulfonate into 200mL of water, adding 10g of calcium chloride, stirring and mixing for 10min, dropwise adding 200mL of solution containing 10g of sodium carbonate, stirring and reacting for 30S, standing for 20min, centrifuging, washing and drying to prepare the calcium carbonate particles coated with the clove oil;
S2, preparing a silk fibroin/silicon oxide hybrid capsule, namely dissolving 2g of silk fibroin peptide in 200mL of PBS solution with the pH value of 7, adding 4g of calcium carbonate particles coated with clove oil, stirring and mixing for 10min to prepare a suspension, dissolving 7g of sodium silicate in 200mL of water, adjusting the pH value to 7.5 to prepare a sodium silicate solution, adding the sodium silicate solution into the suspension, stirring and reacting for 15min, centrifuging, washing, drying, adding 200mL of 0.1mol/L dilute hydrochloric acid solution, reacting for 30min, centrifuging, washing, and drying to prepare the silk fibroin/silicon oxide hybrid capsule;
S3, preparing an wormwood essential oil microcapsule, namely adding 10g of Arabic gum and 10g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 4g of wormwood essential oil, shearing for 10min at 7000r/min, heating to 35 ℃, adjusting the pH value of the solution to 3.5, stirring and reacting for 10min, cooling to 10 ℃, adjusting the pH value of the solution to 5.5, adding 0.5g of glutamine transaminase, solidifying for 2h, and freeze-drying to obtain the wormwood essential oil microcapsule;
S4, preparing the fragrance-retaining essence microcapsule, namely dissolving 9g of sodium alginate in 500mL of water, adding 3g of silk fibroin/silicon oxide hybrid capsule, 6g of wormwood essential oil microcapsule and 0.5g of tween-40, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 20min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Example 2
The embodiment provides a preparation method of a lasting fragrance type essence microcapsule, which comprises the following steps:
S1, preparing calcium carbonate particles coated with lavender oil, namely adding 4g of lavender oil and 0.2g of sodium polystyrene sulfonate into 200mL of water, adding 12g of calcium chloride, stirring and mixing for 10min, dropwise adding 200mL of solution containing 11g of sodium carbonate, stirring and reacting for 60S, standing for 30min, centrifuging, washing and drying to prepare the calcium carbonate particles coated with lavender oil;
S2, preparing a silk fibroin/silicon oxide hybrid capsule, namely dissolving 3g of silk fibroin peptide into 200mL of PBS solution with the pH value of 7.2, adding 6g of calcium carbonate particles coated with lavender oil, stirring and mixing for 10min to prepare a suspension, dissolving 9g of sodium silicate into 200mL of water, adjusting the pH value to 8 to prepare a sodium silicate solution, adding into the suspension, stirring and reacting for 30min, centrifuging, washing, drying, adding into 200mL of 0.3mol/L dilute hydrochloric acid solution, reacting for 50min, centrifuging, washing, and drying to prepare the silk fibroin/silicon oxide hybrid capsule;
S3, preparing an wormwood essential oil microcapsule, namely adding 12g of Arabic gum and 12g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 7g of wormwood essential oil, shearing for 20min at 8000r/min, heating to 45 ℃, adjusting the pH value of the solution to 4.5, stirring and reacting for 20min, cooling to 15 ℃, adjusting the pH value of the solution to 6.5, adding 1g of glutamine transaminase, solidifying for 4h, and freeze-drying to obtain the wormwood essential oil microcapsule;
s4, preparing the fragrance-retaining essence microcapsule, namely dissolving 11g of sodium alginate in 500mL of water, adding 5g of silk fibroin/silicon oxide hybrid capsule, 8g of wormwood essential oil microcapsule and 1g of tween-40, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 40min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Example 3
The embodiment provides a preparation method of a lasting fragrance type essence microcapsule, which comprises the following steps:
S1, preparing calcium carbonate particles coated with rose oil, namely adding 3.5g of rose oil and 0.15g of sodium polystyrene sulfonate into 200mL of water, adding 11g of calcium chloride, stirring and mixing for 10min, dropwise adding 200mL of solution containing 10.5g of sodium carbonate, stirring and reacting for 45S, standing for 25min, centrifuging, washing and drying to prepare the calcium carbonate particles coated with the rose oil;
S2, preparing a silk fibroin/silicon oxide hybrid capsule, namely dissolving 2.5g of silk fibroin peptide into 200mL of PBS solution with the pH value of 7.1, adding 5g of calcium carbonate particles coated with rose oil, stirring and mixing for 10min to prepare a suspension, dissolving 8g of sodium silicate into 200mL of water, adjusting the pH value to 7.7 to prepare a sodium silicate solution, adding the sodium silicate solution into the suspension, stirring and reacting for 20min, centrifuging, washing, drying, adding 200mL of 0.2mol/L dilute hydrochloric acid solution, reacting for 40min, centrifuging, washing, and drying to prepare the silk fibroin/silicon oxide hybrid capsule;
S3, preparing an mugwort essential oil microcapsule, namely adding 11g of Arabic gum and 11g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 5.5g of mugwort essential oil, shearing for 15min at 7500r/min, heating to 40 ℃, adjusting the pH value of the solution to 4, stirring and reacting for 15min, cooling to 12 ℃, adjusting the pH value of the solution to 6, adding 0.7g of glutamine transaminase, solidifying for 3h, and freeze-drying to obtain the mugwort essential oil microcapsule;
S4, preparing the fragrance-retaining essence microcapsule, namely dissolving 10g of sodium alginate in 500mL of water, adding 4g of silk fibroin/silicon oxide hybrid capsule, 7g of wormwood essential oil microcapsule and 0.7g of tween-85, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 30min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Comparative example 1
The difference compared with example 3 is that the double curd method is used to coat the rose oil.
The method comprises the following steps:
S1, preparing rose oil microcapsules, namely adding 11g of Arabic gum and 11g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 5.5g of rose oil, shearing for 15min at 7500r/min, heating to 40 ℃, adjusting the pH value of the solution to 4, stirring and reacting for 15min, cooling to 12 ℃, adjusting the pH value of the solution to 6, adding 0.7g of glutamine transaminase, solidifying for 3h, and freeze-drying to prepare the rose oil microcapsules;
s2, preparing an mugwort essential oil microcapsule, namely adding 11g of Arabic gum and 11g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 5.5g of mugwort essential oil, shearing for 15min at 7500r/min, heating to 40 ℃, adjusting the pH value of the solution to 4, stirring and reacting for 15min, cooling to 12 ℃, adjusting the pH value of the solution to 6, adding 0.7g of glutamine transaminase, solidifying for 3h, and freeze-drying to obtain the mugwort essential oil microcapsule;
S3, preparing the fragrance-retaining essence microcapsule, namely dissolving 10g of sodium alginate in 500mL of water, adding 4g of rose oil microcapsule, 7g of wormwood essential oil microcapsule and 0.7g of tween-85, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 30min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Comparative example 2
Compared with example 3, the difference is that the rose oil and the wormwood essential oil are directly coated in sodium alginate.
The method comprises the following steps:
The preparation method of the fragrance-retaining essence microcapsule comprises the steps of dissolving 10g of sodium alginate in 500mL of water, adding 4g of rose oil, 7g of mugwort essential oil and 0.7g of tween-85, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 30min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Comparative example 3
Compared with example 3, the difference is that the complex curd method is adopted to coat the rose oil, and the wormwood essential oil is directly coated in the sodium alginate.
The method comprises the following steps:
S1, preparing rose oil microcapsules, namely adding 11g of Arabic gum and 11g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 5.5g of rose oil, shearing for 15min at 7500r/min, heating to 40 ℃, adjusting the pH value of the solution to 4, stirring and reacting for 15min, cooling to 12 ℃, adjusting the pH value of the solution to 6, adding 0.7g of glutamine transaminase, solidifying for 3h, and freeze-drying to prepare the rose oil microcapsules;
S2, preparing the fragrance-retaining essence microcapsule, namely dissolving 10g of sodium alginate in 500mL of water, adding 4g of rose oil microcapsule, 7g of wormwood essential oil and 0.7g of tween-85, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 30min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Comparative example 4
Compared with example 3, the difference is that the mugwort essential oil is coated by the double curd method, and the rose oil is directly coated in sodium alginate.
The method comprises the following steps:
S1, preparing an mugwort essential oil microcapsule, namely adding 11g of Arabic gum and 11g of gelatin into 1000mL of water, stirring and mixing uniformly, adding 5.5g of mugwort essential oil, shearing for 15min at 7500r/min, heating to 40 ℃, adjusting the pH value of the solution to 4, stirring and reacting for 15min, cooling to 12 ℃, adjusting the pH value of the solution to 6, adding 0.7g of glutamine transaminase, solidifying for 3h, and freeze-drying to obtain the mugwort essential oil microcapsule;
S2, preparing the fragrance-retaining essence microcapsule, namely dissolving 10g of sodium alginate in 500mL of water, adding 4g of rose oil, 7g of wormwood essential oil microcapsule and 0.7g of tween-85, dropwise adding into 1L of fish oil, emulsifying for 15min at 5000r/min, dropwise adding 10mL of 3wt% calcium chloride solution, solidifying for 30min at normal temperature, centrifuging, washing and drying to obtain the fragrance-retaining essence microcapsule.
Test example 1 determination of the embedding Rate
Pouring 1g (2 positions after the decimal point) of the persistent fragrance type essence microcapsules prepared in the examples 1-3 or the comparative examples 1-4 (mass m 1) into a culture dish, placing the microcapsules in an electrothermal blowing drying oven, drying the microcapsules to constant weight at 80 ℃, taking out the microcapsules again to obtain the mass m 2, taking out the microcapsules with the mass m 0 as the empty evaporation dish, and calculating the embedding rate (E) according to the formula (1):
E=1-[(m1-m2)-β(m1-m0)]/[1-α(m1-m0)]×100%(1)
wherein alpha represents the mass fraction of core essence or sesame oil in the sample microcapsule emulsion, and beta represents the mass fraction of volatile components except essence or sesame oil in the sample microcapsule emulsion.
The results are shown in Table 1.
TABLE 1
As shown in the table above, the lasting fragrance type essence microcapsules prepared in the examples 1-3 have higher embedding rate.
Test example 2 sustained release Performance test
The sustained release performance test was performed on the fragrance-lasting essence microcapsules prepared in examples 1 to 3 and comparative examples 1 to 4 of the present invention.
(1) Sensory characterization
5 Persons sensitive to the fragrance are selected to evaluate the fragrance intensity of the sample, and the average value is taken as a final evaluation result. The evaluation result was 5-grade, and the flavor intensity was classified into 1-5-grade (grade 1, very light flavor, grade 2, light flavor, grade 3, medium flavor, grade 4, heavy flavor, grade 5, heavy flavor). The evaluation period was 120 days. The results are shown in Table 2.
TABLE 2
As can be seen from the above table, the lasting fragrance-retaining essence microcapsules prepared in examples 1-3 of the present invention can still maintain good fragrance release over a longer period.
Constant temperature weightlessness test microcapsules are placed in an environment of 120 ℃ for a certain period of time, and the microcapsules are taken out and weighed at intervals. The slow release performance of the essence microcapsules is characterized by the mass loss rate before and after the microcapsule treatment. The evaluation period was 12h.
The calculation formula is shown as formula (2).
Mass loss rate (%) = (M 1-M2）/M1 (2)
Wherein M 1 is the mass of the aromatic microcapsule before treatment, g, and M 2 is the mass of the aromatic microcapsule after treatment, g.
The results are shown in Table 3.
TABLE 3 Table 3
As shown in the table above, the lasting fragrance type essence microcapsules prepared in the embodiments 1-3 have good heat-resistant stability and good slow release effect.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (9)
1. The preparation method of the lasting fragrance type essence microcapsule is characterized by comprising the following steps of:
S1, preparing calcium carbonate particles coated with a first essence, namely adding the first essence and sodium polystyrene sulfonate into water, adding calcium salt, stirring and mixing uniformly, dripping sodium carbonate solution, stirring and reacting, standing, centrifuging, washing and drying to obtain the calcium carbonate particles coated with the first essence;
S2, preparing a silk fibroin/silicon oxide hybrid capsule, namely dissolving silk fibroin peptide in PBS solution, adding calcium carbonate particles coated with first essence, stirring and uniformly mixing to prepare suspension, dissolving sodium silicate in water, regulating pH value to prepare sodium silicate solution, adding the prepared sodium silicate solution into the suspension, stirring and reacting, centrifuging, washing, drying, adding into hydrochloric acid solution, reacting, centrifuging, washing, and drying to prepare the silk fibroin/silicon oxide hybrid capsule;
S3, preparing a second essential oil microcapsule, namely adding Arabic gum and gelatin into water, stirring and mixing uniformly, adding the second essential oil, shearing, heating, adjusting the pH value of the solution to be a first pH value, stirring and reacting, cooling, adjusting the pH value of the solution to be a second pH value, adding a curing agent, curing, and freeze-drying to prepare the second essential oil microcapsule;
S4, preparing the lasting fragrance type essence microcapsule, namely dissolving sodium alginate in water, adding the silk fibroin/silicon oxide hybrid capsule, the second essential oil microcapsule and the emulsifying agent, uniformly mixing, then dropwise adding the mixture into fish oil, emulsifying, dropwise adding a calcium chloride solution, solidifying at normal temperature, centrifuging, washing and drying to prepare the lasting fragrance type essence microcapsule.
2. The preparation method according to claim 1, wherein in the step S1, the calcium salt is calcium chloride, the mass ratio of the first essence to the sodium polystyrene sulfonate to the calcium chloride to the 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 method according to claim 1, wherein the first essence is at least one selected from the group consisting of rose oil, tree orchid oil, white orchid oil, ylang oil, helichrysum oil, lavender oil, sclareum oil, clove oil, and rosemary oil.
4. The preparation method according to claim 1, wherein in the step S2, the pH value of the PBS solution is 7-7.2, the pH value is adjusted to 7.5-8, the mass ratio of the silk fibroin peptide, the calcium carbonate particles coated with the first essence and the sodium silicate is (2-3): (4-6): (7-9), the stirring reaction time is 15-30min, and the concentration of the hydrochloric acid solution is 0.1-0.3mol/L.
5. The preparation method according to claim 1, wherein in the step S3, the mass ratio of the Arabic gum, the gelatin, the second essential oil and the curing agent is (10-12): 4-7): 0.5-1, the shearing rotation speed is 7000-8000r/min, the shearing time is 10-20min, the heating temperature is 35-45 ℃, the cooling temperature is 10-15 ℃, 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, wherein the second essential oil is mugwort essential oil.
7. The preparation method according to claim 1, wherein in the step S4, the mass ratio of the sodium alginate, the silk fibroin/silica hybrid capsule, the second essential oil microcapsule and the emulsifier is (9-11): 3-5): 6-8): 0.5-1, the emulsifier is at least one selected from tween-20, tween-40, tween-60, tween-80 and tween-85, and the curing time at normal temperature is 20-40min.
8. A long-lasting fragrance perfume microcapsule prepared by the preparation method according to any one of claims 1-7.
9. Use of the long-lasting fragrance type essence microcapsule according to claim 8 in cosmetics and textiles.
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