Compound essence, compound essence nanocapsule as well as preparation method and application of compound essence nanocapsule
By screening and combining the monomer of lavender essential oil and combining it with nanocapsule technology, compound flavor nanocapsules with good antibacterial properties and high thermal stability were prepared, which solved the problems of poor aroma and insufficient antibacterial effect of lavender essential oil, and achieved the dual improvement of aroma long-lasting and antibacterial properties.
Patent Information
- Application Number
- CN202411837597.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-13
- Publication Date
- 2025-04-01
AI Technical Summary
The aroma substances of lavender essential oil are easy to evaporate and deteriorate, and have poor thermal stability, resulting in poor permanence of aroma and difficult to store and transport, which limits its application. Meanwhile, lavender nanocapsules alone may not achieve the required antibacterial effect.
The composition and content of fragrance monomers in essential oils were determined by gas chromatography mass spectrometry, and the fragrance monomers with the best antibacterial properties were screened out, and compounded with the essential oils to prepare compound fragrances. Complex flavors, OSA starch and maltodextrin were used as wall materials and prepared into nanocapsules by self-assembly.
The prepared compound flavor and compound flavor nano capsules have pleasant odor, good antibacterial properties, and have high thermal stability, effectively extend the fragrance retention period of aromatic textiles and improve product durability.
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Figure CN119736121A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of microcapsules, and in particular to a compound flavor, a compound flavor nanocapsule, and a preparation method and application thereof. Background Art
[0002] Lavender (Lavandula angustifolia Mill) is a plant of the genus Lavandula in the family Lamiaceae, genus Perilla, with a strong aromatic smell and a sweet floral aroma. Lavender essential oil is a precious plant extract obtained by distillation from the flower spikes of certain lavender varieties. It is a light yellow clear oily liquid that exudes a sweet, herbal, slightly floral and charming smell. It has multiple pharmacological effects and biological activities such as antibacterial, anti-inflammatory, anti-fatigue, sedative, improving insomnia, and promoting wound healing. However, the aroma substances of lavender essential oil are volatile, easy to deteriorate, and have poor thermal stability, which leads to poor persistence of the aroma of lavender essential oil and difficulty in storage and transportation, limiting its application.
[0003] With the improvement of people's living standards and the change of consumption concepts, traditional cotton fabrics can no longer meet people's daily needs. The development of high-quality, multifunctional and intelligent high-end textile consumer products has become an important way for the textile industry to adapt to the trend of consumption upgrading. Among them, antibacterial textiles have been favored by more and more people. Textiles are an important medium for bacterial reproduction and transmission. Antibacterial textiles can not only effectively inhibit the reproduction and growth of pathogens on textiles, but also block the spread of bacteria, achieving antibacterial and deodorizing functions.
[0004] Therefore, microencapsulation technology can be used to encapsulate essential oils in the cavity of nanocapsules, and bind them to fabric fibers through adsorption, electrostatic interaction, hydrogen bonding, ionic bonding, etc., which can give the fabric a fragrant smell and various functions. However, lavender nanocapsules alone may not achieve the required antibacterial effect.
[0005] Chinese patent CN113863004A discloses a mosquito repellent and antibacterial plant Chinese medicine essential oil composition and a method for preparing a mosquito repellent and antibacterial functional cotton knitted fabric. The plant Chinese medicine essential oil composition is used as a core material and a melamine resin is used as a wall material to prepare a microcapsule. The raw materials include 30-40% citronella essential oil, 25-35% lavender essential oil, 20-30% artemisia essential oil and 10-15% eucalyptus essential oil. The cotton knitted fabric prepared by using the Chinese medicine essential oil composition has an inhibition rate of ≥96.1% on Staphylococcus aureus, an inhibition rate of ≥93.2% on Escherichia coli, and an inhibition rate of ≥85.6% on Candida albicans, and has good antibacterial properties. However, the Chinese medicine essential oil composition may have a strong Chinese herbal medicine smell, which is not easily accepted by the public, limiting its application. Summary of the invention
[0006] The purpose of the present invention is to provide a compound flavor, a compound flavor nanocapsule and a preparation method and application thereof. The prepared compound flavor nanocapsule has a pleasant smell and good antibacterial property, and has high thermal stability.
[0007] The purpose of the present invention can be achieved by the following technical solutions:
[0008] In one aspect, the present invention provides a method for preparing a compound flavor, comprising the following steps:
[0009] S1: Determine the components and contents of fragrance monomers in essential oils by gas chromatography-mass spectrometry, thereby screening out the top five fragrance monomers in essential oils;
[0010] S2: Determine the antibacterial properties of the fragrance monomers screened out in step S1 through molecular docking and antibacterial experiments, thereby screening out the fragrance monomers with the best antibacterial properties in the essential oil;
[0011] S3: Compounding the fragrance monomers screened out in step S2 with essential oils in proportion, determining the optimal compounding ratio through sensory evaluation, and preparing a compound essence.
[0012] Preferably, in step S1, the detection conditions of the gas chromatography in the gas chromatography-mass spectrometry instrument include:
[0013] Chromatographic column: HP-INNOWAX polar column, specification: 60m×0.25mm×0.25μm;
[0014] DB-5 non-polar column, specifications: 60m×0.25mm×0.25μm;
[0015] Carrier gas: helium, carrier gas flow rate: 0.6~1.4mL / min;
[0016] Heating conditions: programmed heating, starting at 50-70°C, maintained for 4-8 min, then heated to 110-130°C at a rate of 3-7°C / min, then heated to 220-260°C at a rate of 2-4°C / min and maintained for 15-25 min;
[0017] Split ratio: (5~10):1.
[0018] Further preferably, in step S1, the detection conditions of the gas chromatography in the gas chromatography-mass spectrometry instrument include:
[0019] Chromatographic column: HP-INNOWAX polar column, specification: 60m×0.25mm×0.25μm;
[0020] DB-5 non-polar column, specifications: 60m×0.25mm×0.25μm;
[0021] Carrier gas: helium, carrier gas flow rate: 1mL / min;
[0022] Heating conditions: programmed heating, starting at 60°C, maintained for 6 min, then heated to 120°C at a rate of 5°C / min, then heated to 240°C at a rate of 3°C / min and maintained for 20 min;
[0023] Split ratio: 10:1.
[0024] Preferably, in step S1, the detection conditions of the mass spectrometer in the gas chromatography-mass spectrometry instrument include:
[0025] Ionization method: EI;
[0026] Ionization energy: 50-80eV;
[0027] Solvent delay time: 1-7min;
[0028] Ion source temperature: 190-260°C;
[0029] Quadrupole temperature: 120-170℃;
[0030] Transmission line temperature: 240-320°C;
[0031] Scan mode: SCAN;
[0032] Scanning ion range (m / z): 20-450.
[0033] Preferably, in step S1, the internal standard method is used to determine the fragrance monomer components and contents in the essential oil by gas chromatography-mass spectrometry, and the internal standard is 2-octanol.
[0034] Preferably, in step S2, the molecular docking refers to docking the fragrance monomer screened in step S1 with AcrIIA14 protein, and judging the antibacterial effect by the size of the binding energy.
[0035] Further preferably, a binding energy value less than -4.25 kcal / mol indicates a certain binding activity between the two, less than -5.0 kcal / mol indicates a good binding activity, and less than -7.0 kcal / mol indicates a strong binding activity. The higher the binding activity, the better the antibacterial effect.
[0036] Preferably, in step S2, the antibacterial experiment is an inhibition zone experiment, using Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 as test strains, and the fragrance monomer screened in step S1 is subjected to an inhibition zone experiment, and the antibacterial effect is judged by the size of the inhibition zone.
[0037] Preferably, based on the molecular docking experiment, the fragrance monomers with a binding energy less than -6.5 kcal / mol are screened out, and then the fragrance monomers with the largest antibacterial zone are screened out from them. The obtained fragrance monomers are the fragrance monomers with the best antibacterial properties in the essential oil.
[0038] Preferably, in step S3, the sensory evaluation refers to determining the optimal compounding ratio through the sensory olfactory scoring of the sensory panel and the test analysis results of the GFace facial expression detection system. When the sensory score of the floral fragrance in the sensory olfactory scoring is higher than 7 points, and the proportion of pleasure and relaxation in the test analysis results of the GFace facial expression detection system is above 85%, then the compounding ratio is the optimal compounding ratio.
[0039] Preferably, in step S3, the optimal compounding ratio of the fragrance monomer to the essential oil is 1:(2-20).
[0040] Preferably, in step S3, the fragrance monomers include linalool, linalyl acetate, and trans-caryophyllene, and the essential oils include lavender essential oil, thyme essential oil, jasmine essential oil, rose essential oil, and violet essential oil.
[0041] Further preferably, the fragrance monomer is linalool, the essential oil is lavender essential oil, and the compound essential oil is obtained by compounding linalool and lavender essential oil.
[0042] Further preferably, the fragrance monomer is linalyl acetate, the essential oil is jasmine essential oil, and the compound essential oil is obtained by compounding linalyl acetate and jasmine essential oil.
[0043] Further preferably, the fragrance monomer is trans-caryophyllene, the essential oil is rose essential oil, and the compound essential oil is obtained by compounding trans-caryophyllene and rose essential oil.
[0044] In a second aspect, the present invention further provides a compound flavor, which is prepared by the above-mentioned method for preparing the compound flavor.
[0045] In a third aspect, the present invention further provides a compound flavor nanocapsule, wherein the nanocapsule comprises the following components in percentage by mass: 15-30% core material, 25-45% wall material, and the remainder water, wherein the core material is the compound flavor mentioned above, and the wall material is OSA starch / maltodextrin.
[0046] In the present invention, the OSA starch is octenyl succinic anhydride (OSA) modified starch.
[0047] In a fourth aspect, the present invention further provides a method for preparing the above-mentioned composite flavor nanocapsules, comprising the following steps:
[0048] S1: dissolving OSA starch and maltodextrin in water, stirring and mixing to obtain a wall material solution;
[0049] S2: The core material and the wall material solution are stirred and mixed, and homogenized and emulsified under a high-speed shearing machine to prepare nanocapsules.
[0050] Preferably, in step S1, the mass ratio of OSA starch to maltodextrin is 2:(1-7), the stirring rate is 300-1200 r / min, the stirring temperature is 40-75° C., and the stirring time is 30-180 min.
[0051] More preferably, the DE value of the maltodextrin is 4-17.
[0052] Preferably, in step S2, the shear rate of the high-speed shearing machine is 10000-22000 r / min, the temperature is 15-40° C., and the time is 10-50 min.
[0053] In a fifth aspect, the present invention also provides an application of the above-mentioned compound fragrance nanocapsule in the field of antibacterial textiles.
[0054] The present invention improves the antibacterial property on the basis of pleasant fragrance by introducing antibacterial fragrance monomers and compounding with essential oils. The compound fragrance nanocapsules are further prepared by microencapsulation technology, which can not only solve the shortcomings of high volatility, poor thermal stability and short fragrance retention time of fragrance, but also effectively prolong the fragrance retention period of aromatic textiles, improve product durability, and solve many problems that cannot be overcome by traditional technologies and processes.
[0055] The invention selects lavender essential oil with aromatic smell to compound with the fragrance monomer, realizes the antibacterial function and maintains the pleasant smell, and has broad application prospects.
[0056] Compared with the prior art, the present invention has the following beneficial effects:
[0057] (1) The present invention first determines the fragrance monomers used for compound flavors through GC / MS (gas chromatography-mass spectrometry analysis method), molecular docking and antibacterial experiments, determines the compounding ratio of the compound flavors through sensory evaluation, and then prepares a compound flavor nanocapsule by a self-assembly method using the compound flavor as the core material and OSA starch and maltodextrin as the wall material. The prepared compound flavor and compound flavor nanocapsule have a pleasant smell, good antibacterial performance, and high thermal stability.
[0058] (2) The present invention optimizes the compound essence obtained by optimally compounding the selected effective antibacterial fragrance monomers with essential oils, thereby achieving a higher antibacterial effect and better sensory evaluation, having an obvious floral fragrance and making people happy.
[0059] (3) The preparation method of the present invention has mild conditions, a relatively simple and easy-to-control process, and innovatively introduces compound flavors as core materials. The prepared nanocapsules have high thermal and mechanical stability and are green and safe.
[0060] (4) Compared with existing flavors, the composite flavor nanocapsules of the present invention have aroma substances that are not easy to volatilize, not easy to deteriorate, and have good thermal stability. The aroma of essential oils is long-lasting and easy to store and transport.
[0061] (5) The composite fragrance nanocapsules prepared by the present invention can be used to improve the antibacterial property of scented textiles and can release fragrance for a long time. BRIEF DESCRIPTION OF THE DRAWINGS
[0062] Figure 1 This is a graph showing the results of the inhibition zone test of five flavor monomers in Example 1 of the present invention using Escherichia coli ATCC 25922 as the test bacteria;
[0063] Figure 2 This is a graph showing the results of the inhibition zone test of five flavor monomers in Example 1 of the present invention using Staphylococcus aureus ATCC 29213 as the test bacteria;
[0064] Figure 3 It is a sensory evaluation radar chart obtained according to different ratios of linalool and lavender essential oil in Examples 1, 2 and 3 of the present invention;
[0065] Figure 4 It is the olfactory sensory analysis diagram obtained by the GFace facial expression detection system according to different ratios of linalool and lavender essential oil in Examples 1, 2, and 3 of the present invention;
[0066] Figure 5 This is a scanning electron microscope image of the composite lavender essence nanocapsules in Example 4 of the present invention;
[0067] Figure 6 This is a particle size distribution diagram of the composite lavender essence nanocapsules in Example 4 of the present invention;
[0068] Figure 7 Thermogravimetric analysis diagrams of Example 4, Example 2 and Comparative Example 1 of the present invention;
[0069] Figure 8 This is a comparison chart of the inhibition zones of Example 2 of the present invention and Comparative Example 2 using Escherichia coli ATCC 25922 as the test bacteria;
[0070] Fig. 9 The figure is a comparison chart of the inhibition zones of Example 2 of the present invention and Comparative Example 2 using Staphylococcus aureus ATCC 29213 as the test strain. DETAILED DESCRIPTION
[0071] The present invention is described in detail below in conjunction with the accompanying drawings and specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and specific operation process, but the protection scope of the present invention is not limited to the following embodiments.
[0072] The OSA starch used in the following examples and comparative examples was purchased from Shanghai Yuanye Biotechnology Co., Ltd., the maltodextrin used was purchased from Shanghai Mairui Biochemical Technology Co., Ltd., and the GFace facial expression detection system used was purchased from Yingfu Instruments. The remaining reagents, methods, instruments and equipment used in the present invention are conventional reagents, methods, instruments and equipment in the art, and the remaining reagents and materials used are commercially available.
[0073] Example 1
[0074] A lavender compound essence, wherein the compounding ratio of the flavor monomer and the lavender essential oil is determined by the following specific steps:
[0075] (1) GC / MS analysis of lavender essential oil was performed with 2-octanol as internal standard, wherein the detection conditions of gas chromatography were as follows: heating conditions: programmed heating: 60°C as initial temperature, maintained for 6 min, then heated to 120°C at a rate of 5°C / min, then heated to 240°C at a rate of 3°C / min and maintained for 20 min, with a split ratio of 10:1. The detection conditions of mass spectrometry were as follows: ionization mode: EI; ionization energy: 70 eV; solvent delay time: 3 min; ion source temperature: 230°C; quadrupole temperature: 150°C; transmission line temperature: 280°C; scanning mode: SCAN; scanning ion range (m / z): 30-400. The detection results are shown in Table 1. The top five fragrance monomers were selected according to their contents, namely linalool, linalyl acetate, isoborneol acetate, L-β-pinene, and trans-caryophyllene.
[0076] Table 1 GC / MS analysis results
[0077]
[0078]
[0079] (2) The five selected flavor monomers were docked with AcrIIA14 protein respectively. First, the receptor protein AcrIIA14 protein was retrieved from the pdb database. The receptor protein was modified by dehydration, ligand removal, hydrogenation, charge balance, etc., and then the receptor protein was molecularly docked with the five flavor monomers. The results are shown in Table 2. The docking results were analyzed and the binding activity of the five flavor monomers with the protein was judged according to the size of the binding energy.
[0080] Table 2 Molecular docking results
[0081]
[0082]
[0083] It can be seen that linalyl acetate has the best binding activity, followed by linalool.
[0084] Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 were used as test bacteria, and the selected fragrance monomers were subjected to an inhibition zone experiment. The specific process is as follows:
[0085] 1. Culture medium preparation
[0086] LB liquid culture medium - use a measuring cylinder to measure 100mL of distilled water and pour it into a 250mL reagent bottle. Use an analytical electronic balance to weigh 2.5g of LB broth culture medium and add it to mix well. Sterilize it in a high-temperature and high-pressure steam sterilizer at 121℃ for 15min and set aside. LB solid culture medium - use a measuring cylinder to measure 100mL of distilled water and pour it into a 250mL reagent bottle. Use an analytical electronic balance to weigh 2.5g of LB broth culture medium and 1.5g of agar powder. Add the above weighed reagents and mix well. Sterilize it in a high-temperature and high-pressure steam sterilizer at 121℃ for 15min. When the culture medium cools to about 40-50℃, use an electric pipette to take 15mL of the culture medium and pour it into a disposable sterile plate.
[0087] 2. Preparation of Bacterial Suspension
[0088] Take three 12mL bacterial culture tubes, add 3mL LB liquid medium to each, pick single colonies from the solid culture medium of Staphylococcus aureus and Escherichia coli and add them to the liquid culture medium, and use the other tube as a blank control. Place in a constant temperature shaker (37°C, 200rpm) and shake culture overnight (15h).
[0089] 3. Filter and sterilize the samples.
[0090] 4. Inhibition zone test
[0091] Dilute the E. coli and Staphylococcus aureus solutions to 106 CFU / mL with sterile PBS solution, then apply 100 μL evenly on the LB solid medium. Punch holes with a 10 mm hole puncher, and add 100 μL of sample solution to each hole. Place the culture dish in a constant temperature incubator at 37°C for 24 hours. After the culture is completed, take out the sample, take a picture, and measure and record the size of the inhibition zone.
[0092] Figure 1 and 2The antibacterial zone test data of the five fragrance monomers in Example 1 of the present invention are shown in Figures AF and AF, respectively, represent the samples linalool, linalyl acetate, levorotatory-β-pinene, isoborneol acetate, trans-caryophyllene and the blank control. Escherichia coli ATCC 25922 was used as the test strain. The test results are shown in Figure AF. Figure 1 As shown in the figure, a small amount of E. coli colonies were found growing on the edge of plate A, indicating a significant antibacterial effect on E. coli. The inhibition zone of plate B was about 4 mm, and the other three samples had no obvious antibacterial effect. Staphylococcus aureus ATCC 29213 was used as the test strain, and the test results were as follows: Figure 2 As shown, no Staphylococcus aureus colonies were found on plates A and C, and a small amount of Staphylococcus aureus colonies grew on the upper edge of plate D, indicating a significant antibacterial effect on Staphylococcus aureus. The inhibition zone of plate B was about 10 mm, and sample E had no obvious antibacterial effect. Linalool and linalyl acetate had an inhibitory effect on both bacteria.
[0093] According to the results of molecular docking and antibacterial experiments, it was judged that the molecular docking binding activities of linalool and linalyl acetate were both less than -6.5 kcal / mol, and the binding activities were good. Judging from the size of the inhibition zone, the antibacterial activity of linalool was significantly greater than that of linalyl acetate. Finally, it was determined that linalool was the fragrance monomer used for compounding with lavender essential oil.
[0094] (3) Linalool and lavender essential oil were mixed in a volume ratio of 1:6. Six students were asked to conduct GFace facial expression detection system testing and sensory evaluation. The sensory evaluation scoring criteria are shown in Table 3.
[0095] Table 3 Sensory evaluation of compound flavors
[0096]
[0097] Embodiment 2:
[0098] A compounded lavender essence, wherein the compounding ratio of the fragrance monomer to the lavender essential oil is determined in a manner substantially the same as that of Example 1, except that in step (3), linalool and the lavender essential oil are compounded in a ratio of 1:10.
[0099] (1) GC / MS analysis of lavender essential oil was performed with 2-octanol as internal standard, wherein the detection conditions of gas chromatography were as follows: heating conditions: programmed heating: 60°C as initial temperature, maintained for 6 min, then heated to 120°C at a rate of 5°C / min, then heated to 240°C at a rate of 3°C / min and maintained for 20 min, with a split ratio of 10:1. The detection conditions of mass spectrometry were as follows: ionization mode: EI; ionization energy: 70 eV; solvent delay time: 3 min; ion source temperature: 230°C; quadrupole temperature: 150°C; transfer line temperature: 280°C; scanning mode: SCAN; scanning ion range (m / z): 30-400. The top five fragrance monomers were selected according to their contents, namely linalool, linalyl acetate, isoborneol acetate, L-β-pinene, and trans-caryophyllene.
[0100] (2) The five selected fragrance monomers were docked with AcrIIA14 protein respectively, and Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 were used as test strains, and the selected fragrance monomers were subjected to an inhibition zone experiment. Finally, it was determined that linalool was the fragrance monomer used for compounding with lavender essential oil.
[0101] (3) Linalool and lavender essential oil were mixed in a volume ratio of 1:10, and six students were asked to conduct the GFace facial expression detection system test and sensory evaluation.
[0102] Embodiment 3:
[0103] A compounded lavender essence, wherein the compounding ratio of the fragrance monomer to the lavender essential oil is determined in a manner substantially the same as that of Example 1, except that in step (3), linalool and the lavender essential oil are compounded in a ratio of 1:13.
[0104] (1) GC / MS analysis of lavender essential oil was performed with 2-octanol as internal standard, wherein the detection conditions of gas chromatography were as follows: heating conditions: programmed heating: 60°C as initial temperature, maintained for 6 min, then heated to 120°C at a rate of 5°C / min, then heated to 240°C at a rate of 3°C / min and maintained for 20 min, with a split ratio of 10:1. The detection conditions of mass spectrometry were as follows: ionization mode: EI; ionization energy: 70 eV; solvent delay time: 3 min; ion source temperature: 230°C; quadrupole temperature: 150°C; transfer line temperature: 280°C; scanning mode: SCAN; scanning ion range (m / z): 30-400. The top five fragrance monomers were selected according to their contents, namely linalool, linalyl acetate, isoborneol acetate, L-β-pinene, and trans-caryophyllene.
[0105] (2) The five selected fragrance monomers were docked with AcrIIA14 protein respectively, and Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 were used as test strains, and the selected fragrance monomers were subjected to an inhibition zone experiment. Finally, it was determined that linalool was the fragrance monomer used for compounding with lavender essential oil.
[0106] (3) Linalool and lavender essential oil were mixed in a volume ratio of 1:13, and six students were asked to conduct the GFace facial expression detection system test and sensory evaluation.
[0107] Figure 3 It is a sensory evaluation radar chart obtained according to different ratios of linalool and lavender essential oil in Examples 1, 2 and 3 of the present invention, as shown in Figure 3 As shown, when the ratio of linalool to lavender essential oil is 1:10, the floral fragrance is rich and smells the most harmonious and comfortable.
[0108] Figure 4 It is the olfactory sensory analysis diagram obtained by the GFace facial expression detection system according to different ratios of linalool and lavender essential oil in Examples 1, 2, and 3 of the present invention, as shown in FIG. Figure 4 As shown in the figure, when the compounding ratio of linalool: lavender essential oil is 1:10, the probability of smelling pleasure in the GFace facial expression detection system is the highest, and the probability of disappointment, sadness, etc. is very low or 0. Therefore, the compounding ratio of 1:10 is the best compounding ratio of lavender compound essence.
[0109] Example 4
[0110] A composite lavender essence nanocapsule comprises the following components in percentage by mass: 23.3% of OSA starch, 11.7% of maltodextrin, 20% of composite lavender essence, and the balance is water.
[0111] A method for preparing composite lavender essence nanocapsules, the specific steps are as follows:
[0112] (1) GC / MS analysis of lavender essential oil was performed with 2-octanol as internal standard, wherein the detection conditions of gas chromatography were as follows: heating conditions: programmed heating: 60°C as initial temperature, maintained for 6 min, then heated to 120°C at a rate of 5°C / min, then heated to 240°C at a rate of 3°C / min and maintained for 20 min, with a split ratio of 10:1. The detection conditions of mass spectrometry were as follows: ionization mode: EI; ionization energy: 70 eV; solvent delay time: 3 min; ion source temperature: 230°C; quadrupole temperature: 150°C; transfer line temperature: 280°C; scanning mode: SCAN; scanning ion range (m / z): 30-400. The top five fragrance monomers were selected according to their contents, namely linalool, linalyl acetate, isoborneol acetate, L-β-pinene, and trans-caryophyllene.
[0113] (2) The five selected fragrance monomers were docked with AcrIIA14 protein respectively, and Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 were used as test strains, and the selected fragrance monomers were subjected to an inhibition zone experiment. Finally, it was determined that linalool was the fragrance monomer used for compounding with lavender essential oil.
[0114] (3) Based on the test results of Examples 1-3, linalool and lavender essential oil were compounded according to an optimal compounding ratio of 1:10.
[0115] (4) According to the above mass ratio, maltodextrin and OSA starch were weighed, added into a beaker filled with deionized water, placed in a water bath at a temperature of 60° C., and stirred at a rate of 650 r / min until the maltodextrin and OSA starch were completely dissolved to obtain a wall material solution.
[0116] (5) The wall material solution was taken out of the water bath and placed at room temperature. Then 20 g of the essence prepared above was weighed and slowly added to the wall material solution at a stirring rate of 650 r / min, and the mixture was stirred and mixed evenly. Finally, shear emulsification was performed at a rate of 10,000 r / min for 20 min.
[0117] Figure 5 This is a scanning electron microscope image of the composite lavender essence nanocapsule in Example 4 of the present invention. Figure 5 As shown, the nanocapsules are uniform spherical structures.
[0118] Figure 6 This is the particle size distribution diagram of the composite lavender essence nanocapsules in Example 4 of the present invention, as shown in Figure 6 As shown, the average particle size of the nanocapsules is 163 nm.
[0119] Comparative Example 1:
[0120] A blank capsule and a preparation method thereof.
[0121] (1) According to the mass ratio of Example 4, maltodextrin and OSA starch were weighed, added into a beaker filled with deionized water, placed in a water bath at a temperature of 60° C., and stirred at a rate of 650 r / min until the maltodextrin and OSA starch were completely dissolved to obtain a wall material solution.
[0122] (2) The wall material solution was taken out of the water bath and placed at room temperature, and shear emulsified at a rate of 10,000 r / min for 20 min.
[0123] Comparative Example 2
[0124] Lavender essential oil
[0125] Figure 7 The thermogravimetric analysis diagrams of Example 4, Example 2, and Comparative Example 1 of the present invention are shown in FIG. Figure 7 As shown in the figure, the compound lavender essence starts to lose weight at 60.4℃, and the maximum weight loss occurs at about 149.2℃, and the essence is almost completely volatilized. The empty capsule, that is, only OSA starch and maltodextrin wall material, starts to lose weight at 56.5℃ in the first stage, and the maximum weight loss occurs at about 200.1℃; the weight loss in the second stage starts at 222.6℃, and the maximum weight loss occurs at about 275℃. In this stage, a large amount of thermal decomposition of the polymer occurs, and the weight loss reaches 63.41%. The weight loss rate slows down when the temperature is greater than 290℃. The compound lavender essence nanocapsules, i.e., containing OSA starch, maltodextrin and compound lavender essence, began to lose weight at about 54.1°C in the first stage, and the maximum weight loss point occurred at about 212.2°C. The mass loss in this stage was mainly caused by the volatilization of essential oil and water not embedded on the surface of the capsule. The second stage of weight loss, i.e., rapid weight loss, began at about 220.6°C, which was about 160°C higher than that of pure lavender essential oil, confirming the protective effect of the microcapsules on the core material. The maximum weight loss point was around 284.1°C, and the weight loss rate slowed down after the temperature was greater than 302°C.
[0126] Figure 8 and Fig. 9 The figure is a comparison diagram of the inhibition zones of Example 2 of the present invention and Comparative Example 2. As shown in the figure, A is compounded lavender essence, and B is lavender essential oil, which proves that the antibacterial ability of the compounded lavender essence is stronger than that of lavender essential oil.
[0127] Example 5
[0128] (1) Preparation of composite lavender essence nanocapsules according to Example 4
[0129] (2) Testing the antibacterial rate of composite lavender essence nanocapsules by plate coating method
[0130] 1. Culture medium preparation
[0131] LB liquid culture medium - use a measuring cylinder to measure 100mL of distilled water and pour it into a 250mL reagent bottle. Use an analytical electronic balance to weigh 2.5g of LB broth culture medium and add it to mix well. Sterilize it in a high-temperature and high-pressure steam sterilizer at 121℃ for 15min and set aside. LB solid culture medium - use a measuring cylinder to measure 100mL of distilled water and pour it into a 250mL reagent bottle. Use an analytical electronic balance to weigh 2.5g of LB broth culture medium and 1.5g of agar powder. Add the above weighed reagents and mix well. Sterilize it in a high-temperature and high-pressure steam sterilizer at 121℃ for 15min. When the culture medium cools to about 40-50℃, use an electric pipette to take 15mL of the culture medium and pour it into a disposable sterile plate.
[0132] 2. Preparation of Bacterial Suspension
[0133] Take three 12mL bacterial culture tubes, add 3mL LB liquid medium to each, pick single colonies from the solid culture medium of Staphylococcus aureus and Escherichia coli and add them to the liquid culture medium, and use the other tube as a blank control. Place in a constant temperature shaker (37℃, 200rpm) and shake culture overnight (15h).
[0134] 3. Place the sample in a high temperature and high pressure steam sterilizer and sterilize at 121℃ for 20 minutes.
[0135] 4. Co-culture + plate spread count test
[0136] Dilute the bacterial solution to 106 CFU / mL with sterile PBS, mix the sterilized sample with the diluted bacterial solution at a ratio of 1:1, and the control group is a group without sample. Place in a 37°C constant temperature incubator and shake for 24 hours. After the culture is completed, dilute the bacterial solution 10 times in a row with sterile PBS solution, take 100 μL of the dilution and evenly spread it on the LB solid culture medium. Place in a 37°C constant temperature incubator and culture for 18 hours, take out and take pictures and record the number of colonies. The results are shown in Table 4.
[0137] Table 4 Antibacterial rate results
[0138]
[0139] In summary, the nanocapsules prepared by the present invention are green and safe, and compared with the uncompounded lavender essential oil nanocapsules, have better antibacterial properties, can be used for the antibacterial and fragrance of functional cotton fabrics, and have broad application prospects.
[0140] The above description of the embodiments is to facilitate the understanding and use of the invention by those skilled in the art. It is obvious that those skilled in the art can easily make various modifications to these embodiments and apply the general principles described herein to other embodiments without creative work. Therefore, the present invention is not limited to the above embodiments, and improvements and modifications made by those skilled in the art based on the disclosure of the present invention without departing from the scope of the present invention should be within the scope of protection of the present invention.
Claims
1. A method for preparing a compound flavor, characterized in that: The following steps are involved: S1: Determine the components and contents of fragrance monomers in essential oils by gas chromatography-mass spectrometry, thereby screening out the top five fragrance monomers in essential oils; S2: Determine the antibacterial properties of the fragrance monomers screened out in step S1 through molecular docking and antibacterial experiments, thereby screening out the fragrance monomers with the best antibacterial properties in the essential oil; S3: Compounding the fragrance monomers screened out in step S2 with essential oils in proportion, determining the optimal compounding ratio through sensory evaluation, and preparing a compound essence.
2. The method for preparing a compound flavor according to claim 1, characterized in that: In step S1, The detection conditions of the gas chromatography in the gas chromatography-mass spectrometry instrument include: Chromatographic column: HP-INNOWAX polar column, specification: 60m×0.25mm×0.25μm; DB-5 non-polar column, specifications: 60m×0.25mm×0.25μm; Carrier gas: helium, carrier gas flow rate: 0.6~1.4mL / min; Heating conditions: programmed heating, starting at 50-70°C, maintained for 4-8 min, then heated to 110-130°C at a rate of 3-7°C / min, then heated to 220-260°C at a rate of 2-4°C / min and maintained for 15-25 min; Split ratio: (5-10): 1; The detection conditions of the mass spectrometer in the gas chromatography-mass spectrometry instrument include: Ionization method: EI; Ionization energy: 50-80eV; Solvent delay time: 1-7min; Ion source temperature: 190-260°C; Quadrupole temperature: 120-170℃; Transmission line temperature: 240-320°C; Scan mode: SCAN; Scanning ion range (m / z): 20-450; The internal standard method was used to determine the fragrance monomer components and contents in the essential oil by gas chromatography-mass spectrometry, wherein the internal standard was 2-octanol.
3. The method for preparing a compound flavor according to claim 1, characterized in that: In step S2, The molecular docking refers to docking the fragrance monomer screened in step S1 with the AcrIIA14 protein, and judging the antibacterial effect by the size of the binding energy; The antibacterial experiment is an inhibition zone experiment, using Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 29213 as test bacteria, and performing an inhibition zone experiment on the fragrance monomer screened in step S1, and judging the antibacterial effect by the size of the inhibition zone; Based on molecular docking experiments, fragrance monomers with binding energy less than -6.5 kcal / mol were screened out, and then the fragrance monomers with the largest antibacterial zone were screened out from them. The obtained fragrance monomers are the fragrance monomers with the best antibacterial properties in essential oils.
4. The method for preparing a compound flavor according to claim 1, characterized in that: In step S3, the sensory evaluation refers to determining the optimal compounding ratio through the sensory olfactory scoring of the sensory panel and the test analysis results of the GFace facial expression detection system. When the sensory score of the floral fragrance in the sensory olfactory scoring is higher than 7 points, and the proportion of pleasure and relaxation in the test analysis results of the GFace facial expression detection system is above 85%, then the compounding ratio is the optimal compounding ratio.
5. The method for preparing a compound flavor according to claim 1, characterized in that: In step S3, the optimal compounding volume ratio of the fragrance monomer to the essential oil is 1:(2-20); The fragrance monomers include one or more of linalool, linalyl acetate, and trans-caryophyllene, and the essential oils include one or more of lavender essential oil, thyme essential oil, jasmine essential oil, rose essential oil, and violet essential oil.
6. A compound flavor, characterized in that: The compound flavor is prepared by the preparation method of the compound flavor as described in any one of claims 1 to 5.
7. A composite flavor nanocapsule, characterized in that: The nanocapsule comprises the following components in percentage by mass: 15-30% of core material, 25-45% of wall material, and the remainder of water. The core material is the compound flavor as claimed in claim 6, and the wall material is OSA starch / maltodextrin.
8. A method for preparing the composite flavor nanocapsule according to claim 7, characterized in that: The following steps are involved: S1: dissolving OSA starch and maltodextrin in water, stirring and mixing evenly to prepare a wall material solution; S2: The core material and the wall material solution are stirred and mixed, and homogenized and emulsified under a high-speed shearing machine to prepare nanocapsules.
9. The method for preparing composite flavor nanocapsules according to claim 8, characterized in that: In step S1, the mass ratio of OSA starch to maltodextrin is 2:(1-7), the stirring rate is 300-1200 r / min, the stirring temperature is 40-75° C., and the stirring time is 30-180 min; In step S2, the shear rate of the high-speed shearing machine is 10000-22000 r / min, the temperature is 15-40° C., and the time is 10-50 min.
10. Use of the compound fragrance nanocapsule according to claim 7 in the field of antibacterial textiles.
Citation Information
Patent Citations
Mosquito-repellent and antibacterial plant traditional Chinese medicine essential oil composition and preparation method of mosquito-repellent and antibacterial functional cotton knitted fabric
CN113863004A