High-loading-capacity nanoscale microcapsule essence emulsion based on dextrin, raw material composition of high-loading-capacity nanoscale microcapsule essence emulsion, and preparation method and application of high-loading-capacity nanoscale microcapsule essence emulsion

Abstract

The invention discloses a dextrin-based high-load nanoscale microcapsule essence emulsion, and a raw material composition, a preparation method and application thereof. The dextrin-based high-load nanoscale microcapsule essence emulsion is prepared from the following components in percentage by mass: 10.0-57.0 wt% of liquid essence, 10.0-57.0 wt% of dextrin, 10.0-57.0 wt% of dextrin, 10.0-57.0 wt% of water, 0.1-0.5 wt 1.0 wt% to 35.0 wt% of dextrin; 1.0 wt% to 10.0 wt% of an emulsifier; and the balance of deionized water. The non-toxic and cheap dextrin is used as a wall material, so that the dosage of auxiliary materials is reduced, the cost is saved, the essence loading capacity of the emulsion is improved, the defect of low essence loading capacity of the emulsion is overcome, the dosage of the essence is reduced, and the flowability and the stability are high; meanwhile, the preparation process is simple, large-scale production and further use are facilitated, the essence loading capacity of the obtained essence microcapsule emulsion can reach 57.0%, and the microcapsule embedding rate is 95% or above.

Description

Technical Field

[0001] The present invention belongs to the technical field of essence nano-capsules, and particularly relates to a nano-scale micro-capsule essence emulsion based on dextrin, its raw material composition, its preparation method and its application. Background Art

[0002] With the development of nano- and micron technologies, the research on nano- and micron micro-capsules has been increasing. The emulsion method is a new type of dispersed emulsion that uses nano-solid particles to replace traditional organic surfactants (such as emulsifiers, thickeners, deflocculants, etc.) to stabilize the emulsion system. By using polymer materials to form a dense protective film, the steric hindrance between the active ingredient and air is increased, so that the active ingredient is isolated from the external environment, the stability is enhanced, and the storage period is extended. In addition, it also has functions such as controlled release.

[0003] In the prior art, the widely used aromatic nano-capsules use the special cavity structure of β-cyclodextrin to encapsulate the essence. Although the method is simple, there are also problems such as irregular structure, low loading capacity, and uneven particle size distribution. Summary of the Invention

[0004] In order to solve the deficiencies of the prior art, the purpose of the present invention is to provide a nano-scale micro-capsule essence emulsion based on dextrin, its raw material composition, its preparation method and its application. The nano-scale micro-capsule essence emulsion prepared by the method of the present invention using dextrin as the wall material can solve the problems of low loading capacity and complicated post-treatment in the prior art.

[0005] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0006] On the one hand, the present invention provides a raw material composition of a nano-scale micro-capsule essence emulsion based on dextrin, which consists of the following components in mass percentages:

[0007] Liquid essence 10.0wt% - 57.0wt%; dextrin 1.0wt% - 35.0wt%; emulsifier 1.0wt% - 10.0wt%; the balance is deionized water.

[0008] In the present invention, dextrin is also known as white dextrin and corn dextrin.

[0009] In some embodiments, the liquid essence is a water-insoluble liquid essence.

[0010] In some embodiments, the liquid essence is orange essence.

[0011] In some embodiments, the emulsifier is Tween-80.

[0012] On the other hand, the present invention provides a method for preparing a dextrin-based high-loading nano-scale microcapsule fragrance emulsion, which at least includes:

[0013] (1) Add dextrin to deionized water, heat it at a constant temperature of 50-70 °C, and stir until the dextrin is fully swollen to obtain an aqueous phase. Cool the aqueous phase to room temperature and set it aside.

[0014] (2) Add liquid fragrance to the aqueous phase and stir to mix to obtain an oil-water mixed phase.

[0015] (3) Add an emulsifier to the oil-water mixed phase and stir to mix to obtain a high-loading nano-scale microcapsule fragrance emulsion.

[0016] The present invention uses dextrin as the wall material and liquid fragrance as the core material, and adopts the emulsion method to prepare a fragrance nano-emulsion with dextrin as the capsule wall. Among them, the aqueous phase is dextrin and deionized water, the oil phase is liquid fragrance, and a certain proportion of emulsifier is added after the aqueous phase and the oil phase are mixed. After stirring and reacting, the fragrance can be coated in it to form a nano-emulsion.

[0017] In step (1), the stirring speed is 200-1000 rpm;

[0018] In step (2), the stirring speed is 200-1000 rpm;

[0019] In step (2), the mixing temperature is 20-40 °C;

[0020] In step (3), the stirring speed is 200-1000 rpm.

[0021] During / after the stirring and mixing in step (3), a shearing operation is further included; preferably, the shearing time is 1-10 min; the shearing speed is 10000 rpm.

[0022] In the present application, during / after the aqueous phase, the oil phase and the emulsifier are mixed and stirred and reacted, high-speed shearing can be further carried out to form a nano-emulsion with a smaller particle size.

[0023] In the third aspect of the present invention, there is also provided a dextrin-based high-loading nano-scale microcapsule fragrance emulsion, which is prepared by the above-mentioned method for preparing a dextrin-based high-loading nano-scale microcapsule fragrance emulsion.

[0024] In the fourth aspect of the present invention, there is also provided an application of the above-mentioned dextrin-based high-loading nano-scale microcapsule fragrance emulsion in the fields of food, daily chemicals and printing and packaging.

[0025] The positive and progressive effects of the present invention are as follows:

[0026] (1) In the present invention, dextrin is first dispersed in the aqueous phase to form a dextrin aqueous solution, and then the essence is dispersed in the dextrin aqueous solution (aqueous phase) that is incompatible with it in the form of tiny droplets to form an oil-in-water emulsion. Then, an emulsifier is introduced. Under the action of the emulsifier, the surface tension at the oil / water interface is reduced, forming a thermodynamically stable emulsion. The essence emulsion prepared by this method is novel, and a stable emulsion with a high loading amount can be obtained, reducing the proportion of wall materials, etc. Moreover, the wall material is non-toxic, inexpensive, and readily available. The prepared nanoemulsion has a relatively regular spherical shape and a relatively uniform particle size.

[0027] (2) In the present invention, dextrin, which is non-toxic and inexpensive, is used as the wall material. This not only reduces the dosage of excipients, saves costs, but also increases the ability of the emulsion to load essence, breaks through the defect of low fragrance loading capacity of the emulsion, reduces the essence dosage, and has good fluidity and high stability. At the same time, the preparation process of the present invention is simple, facilitating large-scale production and further use. The essence loading amount of the obtained essence microcapsule emulsion can reach 57.0%, and the microcapsule embedding rate is above 95%. Description of the Drawings

[0028] Figure 1 is the particle size distribution diagram of the microcapsule emulsion prepared in Example 1 of the present invention;

[0029] Figure 2 is the thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 1 of the present invention;

[0030] Figure 3 is the scanning electron microscope diagram of the microcapsule emulsion prepared in Example 1 of the present invention;

[0031] Figure 4 is the particle size distribution diagram of the microcapsule emulsion prepared in Example 2 of the present invention;

[0032] Figure 5 is the thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 2 of the present invention;

[0033] Figure 6 is the scanning electron microscope diagram of the microcapsule emulsion prepared in Example 2 of the present invention;

[0034] Figure 7 is the particle size distribution diagram of the microcapsule emulsion prepared in Example 3 of the present invention;

[0035] Figure 8 is the thermogravimetric analysis diagram of the microcapsule emulsion prepared in Example 3 of the present invention;

[0036] Figure 9 is the scanning electron microscope diagram of the microcapsule emulsion prepared in Example 3 of the present invention. Detailed Embodiments

[0037] The present invention will be specifically described below in conjunction with embodiments. The technical solutions of the present invention are clearly and completely described to facilitate the understanding of those skilled in the art. The described embodiments are only a part of the embodiments of the present invention, rather than all of them. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the scope of protection of the present invention. At the same time, for the raw materials not specifically described below, they are all commercially available products; the process steps or preparation methods not specifically mentioned are all process steps or preparation methods known to those skilled in the art.

[0038] The reagents or materials used in each embodiment of the present invention are as follows: Orange essence was purchased from Shanghai Yikesaiting Flavor Co., Ltd.; dextrin and Tween-80 were purchased from Shanghai Titan Technology Co., Ltd.

[0039]

Performance Test

[0040] The application performance of the products prepared in the examples and comparative examples was tested. The test methods are as follows:

[0041] I. Particle size distribution diagram: Tested with a nano particle size and Zeta potential analyzer (DLS) model Zetasizer Nano ZS90 produced by Malvern Company, UK.

[0042] II. Thermogravimetric analysis diagram: Tested with a thermogravimetric analyzer (TG) model TGA / DSC3+ produced by Mettler Toledo Company, Switzerland.

[0043] III. SEM diagram: Tested with a scanning electron microscope (SEM) model GeminiSEM 300 produced by ZEISS Company, Germany.

[0044] IV. Determination of encapsulation efficiency: Evaluate the encapsulation efficiency and performance of the microcapsules through the comprehensive application of thermogravimetric analysis and scanning electron microscopy images.

[0045] V. Loading capacity test: Thermogravimetric analysis method.

[0046] VI. Emulsion stability test: Centrifuged with a Feige TDL-4 desktop low-speed centrifuge at a normal temperature test condition of 2000 rpm / 30 min, and observe the condition of the emulsion.

[0047] Example 1

[0048] A nano-scale microcapsule essence emulsion with a high loading capacity based on dextrin is prepared from the following raw materials in mass percentages:

[0049] Raw material Mass percentage Orange essence 57.0wt% Dextrin 15.2wt% Tween - 80 5.0wt% Deionized water 22.8wt%

[0050] The specific preparation steps are as follows:

[0051] (1) Preparation of the aqueous phase: Weigh 2.28 g of deionized water, place 1.52 g of dextrin powder into the deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder, thus obtaining the aqueous phase;

[0052] (2) Preparation of the water-oil mixed phase: Cool the aqueous phase to 25 °C, add 5.7 g of orange essence, place it on an electric stirrer, maintain at 25 °C and stir at 300 rpm to make it homogeneous;

[0053] (3) Preparation of the nanoemulsion: Add 0.5 g of Tween-80 to the water-oil mixed phase in (2), stir electrically for 2 hr to form a uniform emulsion, which is the nano-level orange microcapsule essence emulsion.

[0054] From Figure 1 , Figure 2 and Figure 3 it can be seen that the nano-level microcapsule essence emulsion was successfully prepared in this example. The average particle size (D(50.nm)) is 317 nm, and it has a high loading capacity (57.0%), and the microcapsule embedding rate is above 95%.

[0055] The test results of the emulsion stability show that by centrifugation, it was observed that no water and oil separated out, so it was judged that the emulsion prepared by this method has good stability in the later stage.

[0056] Example 2

[0057] A nano-level microcapsule essence emulsion based on dextrin is prepared from raw materials with the following mass percentages:

[0058]

[0059]

[0060] The specific preparation steps are as follows:

[0061] (1) Preparation of the aqueous phase: Weigh 4.95 g of deionized water, place 3.30 g of dextrin powder into the deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder, thus obtaining the aqueous phase;

[0062] (2) Preparation of the water-oil mixed phase: Cool the aqueous phase to 25 °C, add 1.0 g of orange essence, place it on an electric stirrer, maintain at 25 °C and stir at 300 rpm to make it homogeneous;

[0063] (3) Preparation of nanoemulsion: Add 0.75 g of Tween-80 to the (2) water-oil mixed phase, stir electrically for 2 hr to form a uniform emulsion, which is the nano-level orange microcapsule essence emulsion.

[0064] From Figure 4 , Figure 5 and Figure 6 It can be seen that this example successfully prepared a nano-level microcapsule essence emulsion with an average particle size (D(50.nm)) of 385 nm and a relatively high loading capacity (10.0%), and the microcapsule embedding rate was above 95%.

[0065] The test results of the emulsion stability showed that no water and oil were separated out by centrifugation, so it was judged that the emulsion prepared by this method had good stability in the later stage.

[0066] Example 3

[0067] A nano-level microcapsule essence emulsion based on dextrin is prepared from raw materials with the following mass percentages:

[0068] Raw material Mass percentage Orange essence 33.6wt% Dextrin 24.56wt% Tween - 80 5.0wt% Deionized water 36.84wt%

[0069] The specific steps of its preparation method are as follows:

[0070] (1) Preparation of the aqueous phase: Weigh 3.684 g of deionized water, place 2.456 g of dextrin powder in deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder to obtain the aqueous phase;

[0071] (2) Preparation of the water-oil mixed phase: Cool the aqueous phase to 25 °C, add 3.36 g of orange essence, place it on an electric stirrer, keep it at 25 °C and stir at 300 rpm to make it homogeneous;

[0072] (3) Preparation of nanoemulsion: Add 0.5 g of Tween-80 to the (2) water-oil mixed phase, stir electrically for 2 hr to form a uniform emulsion, which is the nano-level orange microcapsule essence emulsion.

[0073] From Figure 7 , Figure 8 and Figure 9 It can be seen that this example successfully prepared a nano-level microcapsule essence emulsion with an average particle size (D(50.nm)) of 321 nm and a relatively high loading capacity (33.6%), and the microcapsule embedding rate was above 95%.

[0074] The test results of the emulsion stability showed that no water and oil were separated out by centrifugation, so it was judged that the emulsion prepared by this method had good stability in the later stage.

[0075] Comparative Example 1

[0076] A high-load nano-scale microcapsule essence emulsion is prepared from raw materials with the following mass percentages:

[0077] Raw material Mass percentage Orange essence 57.0wt% Dextrin 15.2wt% Tween - 20 5.0wt% Deionized water 22.8wt%

[0078] The specific steps of its preparation method are as follows:

[0079] (1) Preparation of the aqueous phase: Weigh 2.28 g of deionized water, place 1.52 g of dextrin powder into the deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder, thus obtaining the aqueous phase;

[0080] (2) Preparation of the water-oil mixed phase: Cool the aqueous phase to 25 °C, add 5.7 g of orange essence, place it on an electric stirrer, maintain at 25 °C and stir at 300 rpm to make it homogeneous;

[0081] (3) Preparation of the nano-emulsion: Add 0.5 g of Tween-20 to the water-oil mixed phase in (2), stir electrically for 2 h to form a uniform emulsion, which is the nano-scale orange microcapsule essence emulsion.

[0082] The test results of the emulsion stability show that: after the reaction ended, it was found that a small amount of oil floated on the surface, indicating that under these conditions, all these essences could not be completely emulsified into the emulsion.

[0083] Comparative Example 2

[0084] A high-load nano-scale microcapsule essence emulsion is prepared from raw materials with the following mass percentages:

[0085] Raw material Mass percentage Orange essence 57.0wt% β - Cyclodextrin 15.2wt% Tween - 80 5.0wt% Deionized water 22.8wt%

[0086] The specific steps of its preparation method are as follows:

[0087] (1) Preparation of the aqueous phase: Weigh 2.28 g of deionized water, place 1.52 g of β-cyclodextrin powder into the deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder, thus obtaining the aqueous phase;

[0088] (2) Preparation of the water-oil mixed phase: Cool the aqueous phase to 25 °C, add 5.7 g of orange essence, place it on an electric stirrer, maintain at 25 °C and stir at 300 rpm to make it homogeneous;

[0089] (3) Preparation of the nano-emulsion: Add 0.5 g of Tween-80 to the water-oil mixed phase in (2), stir electrically for 2 h to form a uniform emulsion, which is the nano-scale orange microcapsule essence emulsion.

[0090] The test results of emulsion stability showed that: after the reaction ended, a small amount of oil was found floating on the surface, and it was not a uniform emulsion, indicating that under these conditions, all these flavors could not be emulsified into an emulsion.

[0091] Comparative Example 3

[0092] A nano - scale microcapsule flavor emulsion with a high loading amount is prepared from raw materials with the following mass percentages:

[0093] Raw material Mass percentage Orange essence 57.0wt% Hydroxypropyl - β - cyclodextrin 15.2wt% Tween - 80 5.0wt% Deionized water 22.8wt%

[0094] The specific steps of its preparation method are as follows:

[0095] (1) Preparation of the aqueous phase: Weigh 2.28 g of deionized water, place 1.52 g of hydroxypropyl - β - cyclodextrin powder in the deionized water, heat it to 50 °C under the action of an electric stirrer, and stir at 300 rpm for 10 min to completely dissolve the dextrin powder, thus obtaining the aqueous phase;

[0096] (2) Preparation of the water - oil mixed phase: Cool the aqueous phase to 25 °C, add 5.7 g of orange flavor, place it on an electric stirrer, keep it at 25 °C and stir at 300 rpm to make it homogeneous;

[0097] (3) Preparation of the nano - emulsion: Add 0.5 g of Tween - 80 to the water - oil mixed phase in (2), stir electrically for 2 hr to form a uniform emulsion, which is the nano - scale orange microcapsule flavor emulsion.

[0098] The test results of emulsion stability showed that: after the reaction ended, after standing for a while, obvious oil - water stratification occurred, indicating that under these conditions, all these flavors could not be emulsified into an emulsion.

[0099] It can be seen from the comparison of Examples 1 - 3 and Comparative Examples 1 - 3 that dextrin embedding flavors has a certain selectivity. Due to the differences in flavors, it means that the types and amounts of spices in the flavors are different, and the functional groups involved are also different. And the interaction of dextrin with different functional groups is also different, thus resulting in different final emulsion stabilities.

[0100] The microcapsule flavor emulsion prepared by the method of the present invention not only reduces the dosage of auxiliary materials, saves costs, but also increases the ability of the emulsion to load flavors, breaks through the defect of low flavor - loading capacity of the emulsion, reduces the dosage of flavors, and has good stability.

[0101] The above are only the preferred embodiments of the present invention, and do not impose any formal or substantial limitations on the present invention. It should be noted that for those of ordinary skill in the art of this technology, without departing from the premise of the present invention, several improvements and supplements can still be made, and these improvements and supplements should also be regarded as within the protection scope of the present invention. Any equivalent changes in the form of slight modifications, decorations, and evolutions that can be made by those skilled in the art using the technical content disclosed above without departing from the spirit and scope of the present invention are equivalent embodiments of the present invention; at the same time, any equivalent changes, modifications, and evolutions made to the above embodiments based on the substantial technology of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A raw material composition of a high-load nano-scale microcapsule flavor emulsion based on dextrin, characterized in that: The composition comprises the following components in percentage by weight: Liquid flavor 10.0wt%-57.0wt%; dextrin 1.0wt%-35.0wt%; emulsifier 1.0wt%-10.0wt%; the balance is deionized water.

2. The raw material composition of the high-load nano-scale microcapsule flavor emulsion based on dextrin according to claim 1, characterized in that: The liquid essence is a liquid essence that is insoluble in water.

3. The raw material composition of the high-load nano-scale microcapsule flavor emulsion based on dextrin according to claim 2, characterized in that: The liquid flavor is orange flavor.

4. The raw material composition of the high-load nano-scale microcapsule flavor emulsion based on dextrin according to claim 1, characterized in that: The emulsifier is Tween-80.

5. A method for preparing a high-load nano-scale microcapsule flavor emulsion based on dextrin, characterized in that: The raw materials of the dextrin-based high-load nano-scale microcapsule flavor emulsion include the raw material composition of the dextrin-based high-load nano-scale microcapsule flavor emulsion according to any one of claims 1 to 4, and the method includes the following steps: (1) adding dextrin to deionized water, heating at a constant temperature of 50 to 70° C., stirring until the dextrin is fully dissolved 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 high-load nano-scale microcapsule essence emulsion.

6. The method for preparing the high-load nano-scale microcapsule flavor emulsion based on dextrin 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; In step (2), the stirring speed is 200 to 1000 rpm; In step (2), the mixing temperature is 20 to 40° C.; In step (3), the stirring speed is 200 to 1000 rpm; During / after the stirring and mixing in step (3), a shearing operation is also included.

7. The method for preparing the high-load nano-scale microcapsule flavor emulsion based on dextrin according to claim 6, characterized in that: The shearing time is 1 to 10 minutes; And / or, the shearing speed is 10000 rpm.

8. A high-load nano-scale microcapsule flavor emulsion based on dextrin, characterized in that: The invention is prepared by the method for preparing the high-load nano-scale microcapsule flavor emulsion based on dextrin as claimed in any one of claims 5 to 7.

9. Application of the dextrin-based high-load nano-microcapsule flavor emulsion according to claim 8 in the fields of food, daily chemicals and printing and packaging.

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