Nanoscale high-load essence microcapsule emulsion as well as raw material composition, preparation method and application thereof
The nano-level fragrance microcapsule emulsion is prepared by using β-cyclodextrin as the wall emulsion method, which solves the problems of irregular structure, low loading and high production cost of fragrance nanocapsules in the prior art, and achieves a high load, high stability and cost-effective fragrance microcapsule emulsion.
Patent Information
- Application Number
- CN202510248846.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-04
- Publication Date
- 2025-04-18
AI Technical Summary
The existing preparation methods for flavor nano microcapsules have problems such as irregular structure, low loading capacity, uneven particle size distribution and high production costs.
β-cyclodextrin is used as the wall material to prepare nano-scale high-load flavor microcapsule emulsions through the emulsion method to adjust the solubility and assembly behavior of β-cyclodextrin to form a dense membrane structure, and improve the load of flavor and the stability of the emulsion.
It has achieved a stable fragrance emulsion with a high load capacity, with a relatively uniform particle size, an embedding rate of up to 95%, and a low production cost, a simple process, which is convenient for large-scale production.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of flavor nanocapsules, and specifically relates to a nano-level high-load flavor microcapsule emulsion, a raw material composition thereof, and a preparation method and application thereof. Background Art
[0002] With the development of nano-micron technology, the research on nano-micron microcapsule emulsion is also increasing. The basic principle of emulsion preparation is to use surfactants to reduce the surface tension of liquids so that two immiscible liquids can form a stable emulsion. The use of polymer materials to form a dense protective film increases the steric hindrance between the active ingredients and the air, isolates the active ingredients from the external environment, enhances stability, and prolongs the storage period. In addition, it also has functions such as controlled release.
[0003] Among them, the most widely used methods for preparing flavor nano-microcapsules include β-cyclodextrin aromatic Pickering emulsion, silica aromatic nano-emulsion, calcium carbonate aromatic nano-emulsion, etc. The existing aromatic nano-capsules use the special cavity structure of β-cyclodextrin to encapsulate the flavor. Although the method is simple, it also has problems such as irregular structure, low loading capacity, and uneven particle size distribution.
[0004] In the prior art, the invention patent with Chinese patent number CN 111117769 A discloses a nano-scale Pickering emulsion flavor and a preparation method thereof. The raw materials of the nano-scale Pickering emulsion flavor are composed of 5.0-10.0wt% of flavor, 3.0-4.0wt% of β-cyclodextrin, 4-6wt% of sodium caseinate, 0.8-1wt% of emulsifier (Tween-20), and 79.0-87.2wt% of deionized water. The loading amount of the flavor is up to 10.0wt%, and sodium caseinate and Tween-20 are used as emulsifiers at the same time. The loading amount of the emulsion flavor prepared by the method is low, and the production cost is high. Summary of the invention
[0005] In order to solve the deficiencies of the prior art, the purpose of the present invention is to provide a nano-scale high-load flavor microcapsule emulsion, a raw material composition, a preparation method and an application thereof. The method of the present invention uses β-cyclodextrin as a wall material to prepare a nano-scale flavor microcapsule emulsion, which has a high loading capacity and can be used directly or mixed with food / ink coatings, etc., with simple post-processing and low production cost.
[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows:
[0007] In one aspect, the present invention provides a raw material composition of a nano-scale high-load flavor microcapsule emulsion, comprising the following components in percentage by mass:
[0008] Liquid flavor 10.0wt%-47.6wt%; beta-cyclodextrin 1.0wt%-32.0wt%; emulsifier 1.0wt%-10.0wt%; the balance is deionized water.
[0009] In some embodiments, the liquid flavor is an oily liquid flavor.
[0010] In some embodiments, the liquid flavor is apple flavor or cherry flavor.
[0011] In some embodiments, the emulsifier is Tween-20.
[0012] In another aspect, the present invention provides a method for preparing a nano-scale high-load flavor microcapsule emulsion, which at least comprises:
[0013] (1) adding β-cyclodextrin to deionized water, heating at a constant temperature of 50 to 70° C., stirring until the β-cyclodextrin is fully swollen to obtain an aqueous phase, and cooling the aqueous phase to room temperature for later use;
[0014] (2) adding liquid essence into the water phase, stirring and mixing, to obtain an oil-water mixed phase;
[0015] (3) adding an emulsifier into the oil-water mixed phase, stirring and mixing, and preparing a nano-scale high-load flavor microcapsule emulsion.
[0016] The present invention uses β-cyclodextrin as the wall material and liquid essence as the core material, and adopts an emulsion method to prepare a nano-essence emulsion with β-cyclodextrin as the capsule wall. The water phase is β-cyclodextrin and deionized water, the oil phase is the liquid essence, and a certain proportion of emulsifier is added after the water phase and the oil phase are mixed. After stirring and reacting, the essence can be coated therein to form a nano-essence emulsion.
[0017] In step (1), the stirring speed is 200 to 1000 rpm / min;
[0018] In step (2), the stirring speed is 200 to 1000 rpm / min;
[0019] In step (2), the mixing temperature is 20 to 40° C.;
[0020] In step (3), the stirring speed is 200 to 1000 rpm / min.
[0021] During / after the stirring and mixing in step (3), a shearing operation is also included; preferably, the shearing time is 1 to 10 minutes; and the shearing speed is 10000 rpm / min.
[0022] In the present invention, when the emulsifier is added to the oil-water mixed phase and during / after the stirring reaction, the stirring reaction time can be shortened by high-speed shearing to form a nano flavor emulsion with a smaller particle size.
[0023] The third aspect of the present invention further provides a nano-scale high-load flavor microcapsule emulsion, which is prepared by the above-mentioned preparation method of the nano-scale high-load flavor microcapsule emulsion.
[0024] The fourth aspect of the present invention also provides an application of the above-mentioned nano-scale high-load flavor microcapsule emulsion in the fields of food, daily chemicals and printing and packaging.
[0025] The positive and progressive effects of the present invention are:
[0026] (1) In the present invention, since the solubility of β-cyclodextrin in water at room temperature is only 1.85%, the solubility increases rapidly after heating. In addition, due to the hydrophobic cavity and hydrophilic shell of β-cyclodextrin, the β-cyclodextrin solution after heating and cooling is supersaturated, and the cyclodextrins self-assemble to form tiny crystals, which are amphiphilic. Therefore, these tiny crystals can be adsorbed on the oil-water interface, forming a dense film on the surface of the oil phase, and finally forming an oil-in-water emulsion. These tiny crystals show certain emulsifying activity and can replace traditional emulsifiers. The preparation of flavor emulsion by the method of the present invention is relatively novel, and a stable emulsion with a high load can be obtained, which reduces the proportion of wall materials, etc. The prepared nano flavor emulsion is in the shape of a regular sphere or sheet, and the particle size is relatively uniform.
[0027] (2) The present invention uses non-toxic and inexpensive β-cyclodextrin as the wall material, which not only reduces the amount of auxiliary materials used and saves costs, but also increases the ability of the emulsion to load flavors, overcomes the defect of low flavor loading of the emulsion, reduces the amount of flavor used, and has good fluidity and high stability. At the same time, the preparation process of the present invention is simple, which is convenient for large-scale production and further use. The flavor loading amount of the obtained flavor microcapsule emulsion can reach 47.6%, and the microcapsule embedding rate is above 95%. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 1 of the present invention;
[0029] Figure 2 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 1 of the present invention;
[0030] Figure 3 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 1 of the present invention;
[0031] Figure 4 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 2 of the present invention;
[0032] Figure 5is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 2 of the present invention;
[0033] Figure 6 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 2 of the present invention;
[0034] Figure 7 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 3 of the present invention;
[0035] Figure 8 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 3 of the present invention;
[0036] Fig. 9 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 3 of the present invention;
[0037] Fig.10 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 4 of the present invention;
[0038] Fig.11 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 4 of the present invention;
[0039] Fig.12 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 4 of the present invention;
[0040] Fig.13 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 5 of the present invention;
[0041] Fig.14 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 5 of the present invention;
[0042] Fig.15 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 5 of the present invention;
[0043] Fig.16 is a particle size distribution diagram of the microcapsule emulsion prepared in Example 6 of the present invention;
[0044] Fig.17 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 6 of the present invention;
[0045] Fig.18 is a scanning electron microscope image of the microcapsule emulsion prepared in Example 6 of the present invention;
[0046] Fig.19 is a particle size distribution diagram of the microcapsule emulsion prepared in Comparative Example 1 of the present invention;
[0047] Fig. 20 is a thermogravimetric analysis diagram of the microcapsule emulsion prepared in Comparative Example 2 of the present invention;
[0048] Fig.21 It is a scanning electron microscope image of the microcapsule emulsion prepared in Comparative Example 3 of the present invention. DETAILED DESCRIPTION
[0049] The present invention is described in detail below in conjunction with the embodiments, and the technical scheme of the present invention is clearly and completely described to facilitate the understanding of the present invention by those skilled in the art. The described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present invention. At the same time, the raw materials mentioned below that are not described in detail are all commercially available products; the process steps or preparation methods not mentioned in detail are process steps or preparation methods known to those skilled in the art.
[0050] The reagents or materials used in the embodiments of the present invention are as follows: apple flavor and cherry flavor were purchased from Shanghai Exceptin Spice Co., Ltd.; β-cyclodextrin, Tween-20 and sodium caseinate were purchased from Shanghai Titan Technology Co., Ltd.
[0051]
Performance test
[0052] The application performance test of the products prepared in the examples and comparative examples was carried out, and the test method was as follows:
[0053] 1. Particle size diagram: The test was conducted using a nanoparticle size and Zeta potential analyzer (DLS) of model ZetasizerNano ZS90 produced by Malvern, UK.
[0054] 2. Thermogravimetric analysis: The test was conducted using a thermogravimetric analyzer (TG) model TGA / DSC3+ produced by Swiss Mettler Toledo.
[0055] 3. SEM image: The test was conducted using a scanning electron microscope (SEM) of model GeminiSEM 300 produced by ZEISS of Germany.
[0056] 4. Determination of embedding rate: The embedding rate and performance of microcapsules were evaluated through the comprehensive application of thermogravimetric analysis and scanning electron microscopy images.
[0057] 5. Loading capacity test: thermogravimetric analysis.
[0058] 6. Emulsion stability test: Use Feige TDL-4 desktop low-speed centrifuge for centrifugation, test at room temperature at 2000rpm / 30min, and observe the condition of the emulsion.
[0059] Example 1
[0060] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0061] Liquid Fragrance 47.6wt% β-Cyclodextrin 16.0wt% Emulsifier 4.4wt% Deionized water 32.0wt%
[0062] The specific steps of its preparation method are as follows:
[0063] (1) Preparation of the aqueous phase: Weigh 3.2 g of deionized water, place 1.6 g of β-cyclodextrin powder in the deionized water, heat to 50° C. under the action of an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0064] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g of apple essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0065] (3) Preparation of nanoemulsion: 0.44 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0066] from Figure 1 , Figure 2 and Figure 3 It can be seen that the example successfully prepared a nano-scale microcapsule flavor emulsion with an average particle size (D(50.nm)) of 177nm, a relatively high loading amount (47.6%), and a microcapsule embedding rate of more than 95%.
[0067] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0068] Example 2
[0069] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0070] Liquid Fragrance 10.0wt% β-Cyclodextrin 28.5wt% Emulsifier 4.4wt% Deionized water 57.1wt%
[0071] The specific steps of its preparation method are as follows:
[0072] (1) Preparation of the aqueous phase: Weigh 5.71 g of deionized water, place 2.85 g of β-cyclodextrin powder in the deionized water, heat to 50° C. under the action of an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0073] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 1.0 g of apple essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0074] (3) Preparation of nanoemulsion: 0.44 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0075] from Figure 4 , Figure 5 and Figure 6 It can be seen that the embodiment successfully prepared nano-scale flavor microcapsule emulsion with an average particle size (D(50.nm)) of 139nm, a relatively high loading amount (10.0%), and a microcapsule embedding rate of more than 95%.
[0076] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0077] Example 3
[0078] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0079] Liquid Fragrance 28.8wt% β-Cyclodextrin 22.3wt% Emulsifier 4.4wt% Deionized water 44.5wt%
[0080] The specific steps of its preparation method are as follows:
[0081] (1) Preparation of the aqueous phase: Weigh 4.45 g of deionized water, place 2.23 g of β-cyclodextrin powder in the deionized water, heat to 50° C. with an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0082] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 2.88 g of apple essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0083] (3) Preparation of nanoemulsion: 0.44 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0084] from Figure 7 , Figure 8 and Fig. 9 It can be seen that the embodiment successfully prepared nano-scale flavor microcapsule emulsion with an average particle size (D(50.nm)) of 426nm, a relatively high loading amount (28.8%), and a microcapsule embedding rate of more than 95%.
[0085] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0086] Example 4
[0087] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0088] Liquid Fragrance 47.6wt% β-Cyclodextrin 15.9wt% Emulsifier 4.8wt% Deionized water 31.7wt%
[0089] The specific steps of its preparation method are as follows:
[0090] (1) Preparation of the aqueous phase: Weigh 3.17 g of deionized water, place 1.59 g of β-cyclodextrin powder in the deionized water, heat to 50° C. with an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0091] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g cherry essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0092] (3) Preparation of nanoemulsion: 0.48 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, namely, the nano-scale cherry microcapsule essence emulsion.
[0093] from Fig.10 , Fig.11 and Fig.12 It can be seen that the example successfully prepared a nano-scale microcapsule flavor emulsion with an average particle size (D(50.nm)) of 156nm, a relatively high loading amount (47.6%), and a microcapsule embedding rate of more than 95%.
[0094] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0095] Example 5
[0096] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0097] Liquid Fragrance 10.0wt% β-Cyclodextrin 31.0wt% Emulsifier 7.0wt% Deionized water 52.0wt%
[0098] The specific steps of its preparation method are as follows:
[0099] (1) Preparation of the aqueous phase: Weigh 5.2 g of deionized water, place 3.1 g of β-cyclodextrin powder in the deionized water, heat to 50° C. under the action of an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0100] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 1.0 g cherry essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0101] (3) Preparation of nanoemulsion: 0.7 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, namely, the nano-scale cherry microcapsule essence emulsion.
[0102] from Fig.13 , Fig.14 and Fig.15 It can be seen that the embodiment successfully prepared a nano-scale microcapsule flavor emulsion with an average particle size (D(50.nm)) of 412nm, a relatively high loading amount (10.0%), and a microcapsule embedding rate of more than 95%.
[0103] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0104] Example 6
[0105] A nano-scale high-load flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0106] Liquid Fragrance 28.8wt% β-Cyclodextrin 22.0wt% Emulsifier 5.2wt% Deionized water 44.0wt%
[0107] The specific steps of its preparation method are as follows:
[0108] (1) Preparation of the aqueous phase: Weigh 4.4 g of deionized water, place 2.2 g of β-cyclodextrin powder in the deionized water, heat to 50° C. under the action of an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0109] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 2.88 g cherry essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0110] (3) Preparation of nanoemulsion: 0.52 g of Tween-20 was added to the water-oil two-phase mixture and stirred for 2 hours to form an O / W type uniform emulsion, which is the nano-scale cherry microcapsule essence emulsion.
[0111] from Fig.16 , Fig.17 and Fig.18 It can be seen that the embodiment successfully prepared a nano-scale microcapsule flavor emulsion with an average particle size (D(50.nm)) of 583nm, a relatively high loading amount (28.8%), and a microcapsule embedding rate of more than 95%.
[0112] The results of the emulsion stability test showed that no water and oil were observed to be precipitated through centrifugation, which indicated that the emulsion prepared by this method had good late stability.
[0113] Comparative Example 1
[0114] A flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0115] Apple flavor 47.6wt% β-Cyclodextrin 15.9wt% Sodium Caseinate 4.0wt% Tween-20 0.8wt% Deionized water 31.7wt%
[0116] The specific steps of its preparation method are as follows:
[0117] 1) Preparation of the aqueous phase: Weigh 3.17 g of deionized water, place 1.59 g of β-cyclodextrin powder in the deionized water, heat to 50° C. under the action of an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to obtain the aqueous phase;
[0118] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g of apple essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0119] (3) Preparation of nanoemulsion: 0.4 g sodium caseinate and 0.08 g Tween-20 were added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0120] from Fig.19 , Fig. 20 and Fig.21 It can be seen that the comparative example successfully prepared a nano-scale microcapsule flavor emulsion with an average particle size (D(50.nm)) of 278nm, a relatively high loading capacity (47.6%), and a microcapsule embedding rate of more than 95%.
[0121] The emulsion stability test results show that no water and oil precipitation was observed by centrifugation, and it is judged that the emulsion prepared by this method has good late stability. Compared with Example 1, the microcapsule flavor emulsion prepared by this preparation method has good late stability, and the comparative example is that the double emulsifier works together, but the raw material cost of sodium caseinate is higher than Tween-20, and because of the additional component, the production process is slightly complicated. Comprehensively considering the actual production process and application, the emulsion has good late stability, and Example 1 is more cost-effective than Comparative Example 1.
[0122] Comparative Example 2
[0123] A flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0124] Cherry flavor 47.6wt% β-Cyclodextrin 15.9wt% Sodium Caseinate 4.0wt% Tween-20 0.8wt% Deionized water 31.7wt%
[0125] The specific steps of its preparation method are as follows:
[0126] (1) Preparation of the aqueous phase: Weigh 3.17 g of deionized water, place 1.59 g of β-cyclodextrin powder in the deionized water, heat to 50° C. with an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0127] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g cherry essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0128] (3) Preparation of nanoemulsion: 0.4 g sodium caseinate and 0.08 g Tween-20 were added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0129] The results of the emulsion stability test showed that water precipitation was observed through centrifugation, which indicated that the late stability of the emulsion prepared by this method was poor.
[0130] Comparative Example 3
[0131] A flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0132] Cherry flavor 47.6wt% Hydroxypropyl-β-cyclodextrin 15.9wt% Tween-20 4.8wt% Deionized water 31.7wt%
[0133] The specific steps of its preparation method are as follows:
[0134] (1) Preparation of the aqueous phase: Weigh 3.17 g of deionized water, place 1.59 g of β-cyclodextrin powder in the deionized water, heat to 50° C. with an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0135] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g of apple essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0136] (3) Preparation of nanoemulsion: 0.48 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0137] The results of the emulsion stability test showed that water precipitation was observed through centrifugation, which indicated that the late stability of the emulsion prepared by this method was poor.
[0138] Comparative Example 4
[0139] A flavor microcapsule emulsion is prepared from the following raw materials in percentage by mass:
[0140] Cherry flavor 47.6wt% Hydroxypropyl-β-cyclodextrin 15.9wt% Tween-20 4.8wt% Deionized water 31.7wt%
[0141] The specific steps of its preparation method are as follows:
[0142] (1) Preparation of the aqueous phase: Weigh 3.17 g of deionized water, place 1.59 g of β-cyclodextrin powder in the deionized water, heat to 50° C. with an electric stirrer, and stir at 300 rpm / min for 30 min to completely dissolve the β-cyclodextrin powder to prepare the aqueous phase;
[0143] (2) Preparation of water-oil mixed phase: Cool the water phase to 25°C, add 4.76 g cherry essence, place on an electric stirrer to maintain 25°C and stir at 300 rpm / min to make it homogeneous;
[0144] (3) Preparation of nanoemulsion: 0.48 g of Tween-20 was added to the water-oil mixed phase (2), and stirred electrically for 2 hours to form an O / W type uniform emulsion, which is the nano-scale apple microcapsule essence emulsion.
[0145] The results of the emulsion stability test showed that water precipitation was observed through centrifugation, which indicated that the late stability of the emulsion prepared by this method was poor.
[0146] By comparing Examples 1 to 6 with Comparative Examples 1 to 4, it can be seen that β-cyclodextrin has a certain degree of selectivity in embedding flavors. The difference in flavors means that the types and amounts of spices in the flavors are also different, and the functional groups involved are also different. The interaction of the cavity of β-cyclodextrin with different functional groups is also different, which leads to the difference in the final emulsion stability.
[0147] The microcapsule flavor emulsion prepared by the preparation method of the present invention not only reduces the amount of auxiliary materials used, saves costs, but also increases the ability of the emulsion to load flavors, overcomes the defect of low emulsion flavor loading, reduces the amount of flavors used, and the emulsion of the present invention has good stability.
[0148] The above is only a preferred embodiment of the present invention, and is not any formal or substantial limitation of the present invention. It should be pointed out that ordinary technicians in this technical field can make several improvements and supplements without departing from the present invention, and these improvements and supplements should also be regarded as the protection scope of the present invention. Any technician familiar with this profession, without departing from the spirit and scope of the present invention, can make some changes, modifications and equivalent changes made by using the technical content disclosed above, which are equivalent embodiments of the present invention; at the same time, any changes, modifications and evolutions of any equivalent changes made to the above embodiments based on the essential technology of the present invention are still within the scope of the technical solution of the present invention.
Claims
1. A raw material composition of a nano-scale high-load flavor microcapsule emulsion, characterized in that: The composition comprises the following components in percentage by weight: Liquid flavor 10.0wt%-47.6wt%; beta-cyclodextrin 1.0wt%-32.0wt%; emulsifier 1.0wt%-10.0wt%; the balance is deionized water.
2. The raw material composition of the nano-scale high-load flavor microcapsule emulsion according to claim 1, characterized in that: The liquid flavor is an oily liquid flavor.
3. The raw material composition of the nano-scale high-loaded flavor microcapsule emulsion according to claim 2, characterized in that: The liquid flavor is apple flavor or cherry flavor.
4. The raw material composition of the nano-scale high-loaded flavor microcapsule emulsion according to claim 1, characterized in that: The emulsifier is Tween-20.
5. A method for preparing a nano-scale high-load flavor microcapsule emulsion, characterized in that: The raw materials of the nano-scale high-load flavor microcapsule emulsion include the raw material composition of the nano-scale high-load flavor microcapsule emulsion as claimed in any one of claims 1 to 4, and the method includes the following steps: (1) adding β-cyclodextrin to deionized water, heating at a constant temperature of 50 to 70° C., stirring until the β-cyclodextrin is fully swollen to obtain an aqueous phase, and cooling the aqueous phase to room temperature for later use; (2) adding liquid essence into the water phase, stirring and mixing, to obtain an oil-water mixed phase; (3) adding an emulsifier into the oil-water mixed phase, stirring and mixing, and preparing a nano-scale high-load flavor microcapsule emulsion.
6. The method for preparing the nano-scale high-load flavor microcapsule emulsion according to claim 5, characterized in that: The preparation method satisfies at least one of the following conditions: In step (1), the stirring speed is 200 to 1000 rpm / min; In step (2), the stirring speed is 200 to 1000 rpm / min; In step (2), the mixing temperature is 20 to 40° C.; In step (3), the stirring speed is 200 to 1000 rpm / min; During / after the stirring and mixing in step (3), a shearing operation is also included.
7. The method for preparing the nano-scale high-load flavor microcapsule emulsion according to claim 6, characterized in that: The shearing time is 1 to 10 minutes; And / or, the shearing speed is 10000 rpm / min.
8. A nano-scale high-load flavor microcapsule emulsion, characterized in that: The invention is prepared by the method for preparing the nano-scale high-load flavor microcapsule emulsion as claimed in any one of claims 5 to 7.
9. Application of the nano-scale high-load flavor microcapsule emulsion according to claim 8 in the fields of food, daily chemicals and printing and packaging.
Citation Information
Patent Citations
Nanoscale Pickering emulsion essence and preparation method thereof
CN111117769A