O1 / W / O2 type double emulsion as well as preparation method and application thereof

Abstract

The invention relates to an O1 / W / O2 type double emulsion as well as a preparation method and application thereof. The O1 / W / O2 type double emulsion comprises an inner-layer oil phase O1, a middle-layer water phase W and an outer-layer oil phase O2, the inner-layer oil phase O1 comprises essence and a first solvent; the middle layer water phase W comprises a water-soluble emulsifier and water; the outer-layer oil phase O2 comprises an oil-soluble emulsifier and a second solvent; the water-soluble emulsifier comprises a combination of flaxseed gum, whey protein isolate and Tween 80. The emulsion provided by the invention has the advantages of simple, cheap and easily available raw materials, simple preparation method and low cost; the obtained emulsion improves the stability of the essence, the essence loading rate is high, the essence has good fragrance loading and holding performance, and controlled release of the loaded essence can be achieved through temperature change.

Description

Technical Field

[0001] The invention relates to the technical field of emulsions, and in particular to an O1 / W / O2 double emulsion and a preparation method and application thereof. Background Art

[0002] The flavor itself has a unique aromatic smell and anti-inflammatory and antibacterial effects. It is often used as an additive and has been widely used in the fields of food, medicine, cosmetics, textiles and paper. Among them, mint flavor, one of the most widely used spices in the world, is widely used in food, medicine, cosmetics and other industries due to its fresh mint aroma and antipruritic and analgesic, antibacterial and anti-inflammatory, penetration-promoting, cooling and mild local anesthesia. However, the volatility of the flavor makes it easy to deteriorate during storage and use, so it is urgent to improve the stability of the flavor and realize the controlled release of the flavor. The current solution strategy is mainly to develop a suitable carrier (i.e., a flavor-carrying material) for loading the flavor, thereby inhibiting the volatilization of the flavor and improving the stability of the flavor. The existing flavor-carrying materials mainly include porous adsorption materials, microcapsules and emulsions, but most of the materials still have limitations such as complex preparation process, low flavor loading rate, insufficient stability and high cost to varying degrees. The preparation method of the emulsion is relatively simple and low-cost. Most of the flavor-carrying emulsions reported so far are single emulsions.

[0003] CN118599157A discloses a preparation and application of a konjac gum / hydroxypropyl methylcellulose double-layer film loaded with thyme essential oil Pickering emulsion, and the preparation method includes: preparing TEMPO oxidized chitin nanocrystals; dissolving TEMPO oxidized chitin nanocrystals in water to obtain a nanocrystal suspension; mixing thyme essential oil with a nanocrystal suspension to obtain a Pickering emulsion; dissolving konjac gum and hydroxypropyl methylcellulose in water, and then adding glycerol to obtain a film-forming liquid; mixing the Pickering emulsion with a film-forming liquid to obtain an emulsion film-forming liquid; first casting the film-forming liquid to form a protective layer, then pouring the emulsion film-forming liquid on the protective layer to form a film to form an active layer, and drying the film. The double-layer film obtained by the method can effectively improve the utilization efficiency of essential oil active substances and realize the unidirectional release of essential oils in the film.

[0004] CN118592640A discloses a menthol-containing Pickering emulsion and a preparation method thereof. The menthol-containing Pickering emulsion provided by the present invention is prepared by using menthol and cyclodextrin composite particles as solid particle emulsifiers and soybean oil as oil phase, and the mass ratio of menthol to cyclodextrin is 1:2-5. The menthol-containing Pickering emulsion prepared by the method exhibits good storage stability and rheological properties within 30 days.

[0005] CN118614541A discloses a methyl ferulate-grapefruit essential oil nanoemulsion and a preparation method and application thereof. The preparation method comprises dissolving methyl ferulate in grapefruit essential oil to obtain an oil phase, successively adding Tween 80 and water to the oil phase, stirring to obtain a crude emulsion, and then subjecting the oil phase to ultrasonic treatment to obtain the methyl ferulate-grapefruit essential oil nanoemulsion.

[0006] The above method has the problems of complex raw materials, poor emulsion stability, and inability to effectively achieve the slow release of flavors. Therefore, providing an emulsion with strong stability and high flavor loading rate has become an urgent problem to be solved. Summary of the invention

[0007] In order to solve the above technical problems, the present invention provides an O1 / W / O2 type double emulsion and its preparation method and application. The emulsion provided by the present invention has simple raw materials, is cheap and easy to obtain, and has a simple preparation method and low cost; the obtained emulsion improves the stability of the flavor, has a high flavor loading rate, has good flavor carrying and lasting performance, and can realize the controlled release of the loaded flavor by changing the temperature.

[0008] To achieve this object, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides an O1 / W / O2 type double emulsion, wherein the O1 / W / O2 type double emulsion comprises an inner oil phase O1, an intermediate water phase W and an outer oil phase O2; the inner oil phase O1 comprises essence and a first solvent; the intermediate water phase W comprises a water-soluble emulsifier and water; the outer oil phase O2 comprises an oil-soluble emulsifier and a second solvent;

[0010] The water-soluble emulsifier comprises a combination of flaxseed gum, whey protein isolate and Tween 80.

[0011] The present invention loads the flavor in the inner oil phase O1, and the obtained O1 / W / O2 double emulsion has a unique multi-compartment structure of "two membranes and three phases", which can achieve stable encapsulation of the flavor through the hydrogen bond interaction between the substances in the system, has high stability and flavor embedding rate, and achieves a sustained release effect of the flavor by controlling the demulsification of the multiple interface membranes by temperature, and has good flavor carrying, flavor holding and flavor releasing properties.

[0012] The present invention further improves the emulsification effect by further compounding the water-soluble emulsifier and cooperating with multiple emulsifiers. The obtained O1 / W / O2 double emulsion has high stability and flavor embedding rate, and can better achieve the flavor sustained release effect.

[0013] Preferably, the first solvent comprises any one of ethanol, propylene glycol or caprylic acid glyceride or a combination of at least two thereof.

[0014] Preferably, the second solvent comprises any one of propylene glycol, triacetin or caprylic decanoic acid glyceride, or a combination of at least two thereof.

[0015] Preferably, the oil-soluble emulsifier includes any one of Span 80, monoglycerol fatty acid ester or sucrose fatty acid ester, or a combination of at least two thereof.

[0016] In the present invention, the combination of the specific oily emulsifier and the second solvent can further improve the emulsification effect, and the obtained emulsion formed by the outer oil phase and the water phase encapsulating the inner oil phase has better performance.

[0017] The change of the types of the above-mentioned solvents will lead to different interactions between the substances in the emulsion system, thus affecting its fragrance carrying and fragrance releasing effects.

[0018] Preferably, the mass ratio of the flavor to the first solvent is 1:(0.1-1.2), for example, it can be 1:0.1, 1:0.2, 1:0.4, 1:0.6, 1:0.8, 1:1.0, 1:1.2, etc., preferably 1:(0.15-0.5).

[0019] Preferably, the mass ratio of the water-soluble emulsifier to water is 1:(7-19), for example, it can be 1:7, 1:9, 1:11, 1:13, 1:15, 1:17, 1:19, etc., preferably 1:(7-11.5).

[0020] Preferably, the mass ratio of the oil-soluble emulsifier to the second solvent is 1:(7-19), for example, it can be 1:7, 1:9, 1:11, 1:13, 1:15, 1:17, 1:19, etc., preferably 1:(9-12).

[0021] Preferably, the mass ratio of the middle layer water phase W to the inner layer oil phase O1 is 1:(0.5-1.5), for example, it can be 1:0.5, 1:0.7, 1:0.9, 1:1.1, 1:1.3, 1:1.5, etc., preferably 1:(1-1.5).

[0022] Preferably, the mass ratio of the sum of the inner oil phase O1 and the middle water phase W to the outer oil phase O2 is 1:(0.5-1.5), for example, it can be 1:0.5, 1:0.7, 1:0.9, 1:1.1, 1:1.3, 1:1.5, etc., preferably 1:(0.8-1.2).

[0023] In the present invention, the ratios of the components interact with each other to achieve the technical effects achieved by the present invention. For example, if the amount of emulsifier is too little or too much, the emulsion will be unstable, and phenomena such as stratification, precipitation or demulsification will occur; the mass ratio of the essence solution to water, the middle layer water phase W to the inner layer oil phase O1, and the sum of the inner layer oil phase O1 and the middle layer water phase W to the outer layer oil phase O2 will affect the stability of the emulsion and the embedding rate of the essence. The present invention can further improve the various properties of the emulsion by limiting the ratios of the above components in the emulsion.

[0024] Preferably, the mass ratio of flaxseed gum, whey protein isolate and Tween 80 is 1:(0.5-1.5):(0.5-1.5).

[0025] The above-mentioned numerical value (0.5-1.5) can be, for example, 0.5, 0.6, 0.8, 1, 1.2, 1.4, 1.5, etc.

[0026] In a second aspect, the present invention provides a method for preparing the O1 / W / O2 double emulsion according to the first aspect, the preparation method comprising the following steps:

[0027] (1) Mixing the essence and the first solvent to obtain an inner oil phase O1; mixing the water-soluble emulsifier and water to obtain an intermediate water phase W; mixing the oil-soluble emulsifier and the second solvent to obtain an outer oil phase O2;

[0028] (2) adding the inner oil phase O1 to the middle water phase W, and after ultrasonic emulsification, obtaining O1 / W type colostrum; adding the O1 / W type colostrum to the outer oil phase O2, and after ultrasonic emulsification, obtaining the O1 / W / O2 type double emulsion.

[0029] Preferably, in step (1), the water-soluble emulsifier and water are mixed or the oil-soluble emulsifier and the second solvent are mixed, and the mixing is carried out under conditions of heating and stirring in a water bath.

[0030] Preferably, the temperatures of the water bath heating are independently 25-40°C, for example, 25°C, 30°C, 35°C, 40°C, etc.

[0031] Preferably, the stirring rate is independently 800-1200 r / min, for example, 800 r / min, 900 r / min, 1000 r / min, 1100 r / min, 1200 r / min, etc., and the stirring time is independently 2-10 min, for example, 2 min, 4 min, 6 min, 8 min, 10 min, etc.

[0032] Preferably, the adding method in step (2) is dropwise addition.

[0033] Preferably, the adding is carried out under conditions of heating in a water bath and stirring.

[0034] Preferably, the temperatures of the water bath heating are independently 25-40°C, for example, 25°C, 30°C, 35°C, 40°C, etc.

[0035] Preferably, the stirring rate is independently 800-1200 r / min, for example, 800 r / min, 900 r / min, 1000 r / min, 1100 r / min, 1200 r / min, etc., and the stirring time is independently 2-10 min, for example, 2 min, 4 min, 6 min, 8 min, 10 min, etc.

[0036] Preferably, the power of the ultrasonic emulsification in step (2) is independently 100-200 W, for example, 100 W, 120 W, 140 W, 160 W, 180 W, 200 W, etc., and the time of the ultrasonic emulsification is independently 2-10 min, for example, 2 min, 4 min, 6 min, 8 min, 10 min, etc.

[0037] By reasonably limiting the above parameters in the present invention, the prepared fragrance-carrying emulsion has optimal stability and a higher fragrance loading rate, thereby extending the storage time of the fragrance.

[0038] In a third aspect, the present invention provides a use of the O1 / W / O2 double emulsion according to the first aspect in cigarette flavoring.

[0039] Compared with the prior art, the present invention has at least the following beneficial effects:

[0040] The O1 / W / O2 double emulsion provided by the present invention is a unique "two-film three-phase" multi-compartment structure, which can achieve stable encapsulation of flavors through hydrogen bond interactions between substances in the system, has high stability and flavor embedding rate, and achieves a slow-release effect on flavors by controlling the demulsification of multiple interface films with temperature, and has good flavor carrying, flavor holding and flavor release performance. In the preferred embodiment, the droplet diameter in the emulsion is 20-50 μm, can be stably placed for 58-62 days, and can achieve slow release of flavors at 40-90°C. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 This is the appearance of the emulsion provided in Example 1-5 after being placed for 60 days.

[0042] Figure 2 Optical microscope images of the emulsions provided for Examples 1-5 after 60 days of storage. DETAILED DESCRIPTION

[0043] The technical solution of the present invention is further described below in conjunction with the accompanying drawings and through specific implementation methods. However, the following examples are only simplified examples of the present invention and do not represent or limit the scope of protection of the present invention. The scope of protection of the present invention shall be subject to the claims.

[0044] The flavor used in the following examples is menthol.

[0045] Example 1

[0046] This embodiment provides an O1 / W / O2 type double emulsion, comprising an inner oil phase O1, an intermediate water phase W and an outer oil phase O2; the inner oil phase O1 comprises essence and a first solvent (caprylic glyceride); the intermediate water phase W comprises a water-soluble emulsifier (flaxseed gum, whey protein isolate and Tween 80 in a mass ratio of 1:1.2:0.8) and water; the outer oil phase O2 comprises an oil-soluble emulsifier (Span 80) and a second solvent (propylene glycol);

[0047] The preparation of the O1 / W / O2 type double emulsion comprises the following steps:

[0048] (1) mixing the essence and the first solvent in a mass ratio of 1:0.2 to obtain an inner oil phase O1;

[0049] (2) mixing a water-soluble emulsifier and water in a mass ratio of 1:10.5, heating in a water bath at 35° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an intermediate layer aqueous phase W;

[0050] (3) mixing the oil-soluble emulsifier and the second solvent in a mass ratio of 1:9, heating in a water bath at 35° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an outer oil phase O2;

[0051] (4) Under heating and stirring conditions (35°C, 1000 r / min), the inner layer oil phase O1 was slowly dripped into the middle layer water phase W (the mass ratio of water phase W to oil phase O1 was 1:1.2), and stirring was continued for 5 minutes after the dropwise addition was completed. Then, ultrasonic emulsification was performed at 150 W for 5 minutes using an ultrasonic cell disruptor to obtain O1 / W colostrum;

[0052] (5) Under heating and stirring conditions (35°C, 1000 r / min), the O1 / W colostrum is slowly dripped into the outer oil phase O2 (the mass ratio of O1 / W colostrum to oil phase O2 is 1:1), and stirring is continued for 5 minutes after the dripping is completed. Subsequently, ultrasonic emulsification is performed using an ultrasonic cell disruptor at 150 W for 5 minutes to obtain the O1 / W / O2 double emulsion.

[0053] Example 2

[0054] This embodiment provides an O1 / W / O2 type double emulsion, comprising an inner oil phase O1, an intermediate water phase W and an outer oil phase O2; the inner oil phase O1 comprises essence and a first solvent (ethanol); the intermediate water phase W comprises a water-soluble emulsifier (flaxseed gum, whey protein isolate and Tween 80 in a mass ratio of 1:1.5:0.5) and water; the outer oil phase O2 comprises an oil-soluble emulsifier (Span 80) and a second solvent (caprylic decanoate);

[0055] The preparation of the O1 / W / O2 type double emulsion comprises the following steps:

[0056] (1) mixing the essence and the first solvent in a mass ratio of 1:0.5 to obtain an inner oil phase O1;

[0057] (2) mixing a water-soluble emulsifier and water in a mass ratio of 1:7, heating in a water bath at 25° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an intermediate layer aqueous phase W;

[0058] (3) mixing the oil-soluble emulsifier and the second solvent in a mass ratio of 1:12, heating in a water bath at 25° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an outer oil phase O2;

[0059] (4) Under heating and stirring conditions (25°C, 1000 r / min), the inner layer oil phase O1 was slowly dripped into the middle layer water phase W (the mass ratio of water phase W to oil phase O1 was 1:1.1), and stirring was continued for 5 min after the dropwise addition was completed. Then, ultrasonic emulsification was performed at 150 W for 5 min using an ultrasonic cell disruptor to obtain O1 / W colostrum;

[0060] (5) Under heating and stirring conditions (25°C, 1000 r / min), the O1 / W colostrum is slowly dripped into the outer oil phase O2 (the mass ratio of O1 / W colostrum to oil phase O2 is 1:1.2), and stirring is continued for 5 minutes after the dripping is completed. Subsequently, ultrasonic emulsification is performed using an ultrasonic cell disruptor at 150 W for 5 minutes to obtain the O1 / W / O2 double emulsion.

[0061] Example 3

[0062] The present embodiment provides an O1 / W / O2 type double emulsion, comprising an inner oil phase O1, an intermediate water phase W and an outer oil phase O2; the inner oil phase O1 comprises essence and a first solvent (caprylic acid glyceride); the intermediate water phase W comprises a water-soluble emulsifier (flaxseed gum, whey protein isolate and Tween 80 in a mass ratio of 1:0.5:1.5) and water; the outer oil phase O2 comprises an oil-soluble emulsifier (monoglycerol fatty acid ester) and a second solvent (triacetin);

[0063] The preparation of the O1 / W / O2 type double emulsion comprises the following steps:

[0064] (1) mixing the essence and the first solvent in a mass ratio of 1:0.15 to obtain an inner oil phase O1;

[0065] (2) mixing a water-soluble emulsifier and water in a mass ratio of 1:11.5, heating in a water bath at 40° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an intermediate layer aqueous phase W;

[0066] (3) mixing the oil-soluble emulsifier and the second solvent in a mass ratio of 1:10, heating in a water bath at 40° C., and stirring at a speed of 1000 r / min for 5 min using a magnetic stirrer to obtain an outer oil phase O2;

[0067] (4) Under heating and stirring conditions (40°C, 1000 r / min), the inner layer oil phase O1 was slowly dripped into the middle layer water phase W (the mass ratio of water phase W to oil phase O1 was 1:1.5), and stirring was continued for 5 minutes after the dropwise addition was completed. Then, ultrasonic emulsification was performed at 150 W for 5 minutes using an ultrasonic cell disruptor to obtain O1 / W colostrum;

[0068] (5) Under heating and stirring conditions (40°C, 1000 r / min), the O1 / W colostrum is slowly dripped into the outer oil phase O2 (the mass ratio of O1 / W colostrum to oil phase O2 is 1:0.8), and stirring is continued for 5 minutes after the dripping is completed. Subsequently, ultrasonic emulsification is performed using an ultrasonic cell disruptor at 150 W for 5 minutes to obtain the O1 / W / O2 double emulsion.

[0069] Example 4

[0070] This embodiment provides an O1 / W / O2 double emulsion, which differs from Embodiment 1 only in that, in the preparation method steps (2) to (5), the stirring speed is 1200 r / min and the stirring time is 9 min. For other matters, refer to Embodiment 1.

[0071] Example 5

[0072] This embodiment provides an O1 / W / O2 double emulsion, which differs from Embodiment 1 only in that in steps (4)-(5) of the preparation method, the ultrasonic power is 180 W and the stirring time is 8 min. For other matters, refer to Embodiment 1.

[0073] Example 6

[0074] This embodiment provides an O1 / W / O2 type double emulsion, which is different from Embodiment 1 only in that the mass ratio of the water-soluble emulsifier to water in the intermediate layer water phase W is 1:5. For other matters, refer to Embodiment 1.

[0075] Example 7

[0076] This embodiment provides an O1 / W / O2 type double emulsion, which is different from Embodiment 1 only in that the mass ratio of the water-soluble emulsifier to water in the intermediate layer water phase W is 1:15. For other matters, refer to Embodiment 1.

[0077] Example 8

[0078] This embodiment provides an O1 / W / O2 type double emulsion, which is different from Embodiment 1 only in that the mass ratio of the oil-soluble emulsifier to the second solvent in the outer oil phase O2 is 1:7. For other matters, refer to Embodiment 1.

[0079] Example 9

[0080] This embodiment provides an O1 / W / O2 type double emulsion, which is different from Embodiment 1 only in that the mass ratio of the oil-soluble emulsifier to the second solvent in the outer oil phase O2 is 1:19. For other matters, refer to Embodiment 1.

[0081] Example 10

[0082] This embodiment provides an O1 / W / O2 type double emulsion, which differs from Embodiment 1 only in that the mass ratio of the middle layer water phase W to the inner oil phase O1 is 1:0.5. For other matters, refer to Embodiment 1.

[0083] Embodiment 11

[0084] This embodiment provides an O1 / W / O2 type double emulsion, which differs from Embodiment 1 only in that the mass ratio of the middle layer water phase W to the inner oil phase O1 is 1:2.5. For other matters, refer to Embodiment 1.

[0085] Example 12

[0086] This embodiment provides an O1 / W / O2 double emulsion, which is different from Embodiment 1 only in that the mass ratio of O1 / W colostrum to oil phase O2 is 1:0.5. For other matters, refer to Embodiment 1.

[0087] Example 13

[0088] This embodiment provides an O1 / W / O2 type double emulsion, which is different from Embodiment 1 only in that the mass ratio of O1 / W type colostrum to oil phase O2 is 1:1.5. For other matters, refer to Embodiment 1.

[0089] Embodiment 14

[0090] This embodiment provides an O1 / W / O2 double emulsion, which differs from Embodiment 1 only in that, in the preparation method steps (2) to (5), the water bath heating temperature is 45° C., and the rest is referred to Embodiment 1.

[0091] Embodiment 15

[0092] This embodiment provides an O1 / W / O2 double emulsion, which differs from Embodiment 1 only in that in the preparation method steps (2)-(5), the stirring speed is 1500 r / min. For other matters, refer to Embodiment 1.

[0093] Example 16

[0094] This embodiment provides an O1 / W / O2 double emulsion, which is different from Embodiment 1 only in that in the preparation method steps (4)-(5), the ultrasonic power is 250 W. For other matters, refer to Embodiment 1.

[0095] Comparative Example 1

[0096] This comparative example provides an O1 / W / O2 type double emulsion, which is different from Example 1 only in that the water-soluble emulsifier lacks flaxseed gum, and its usage is distributed according to the ratio of whey protein isolate and Tween 80. For other references, refer to Example 1.

[0097] Comparative Example 2

[0098] This comparative example provides an O1 / W / O2 type double emulsion, which is different from Example 1 only in that the water-soluble emulsifier lacks whey protein isolate and its usage is distributed according to the ratio of flaxseed gum and Tween 80. For other reasons, refer to Example 1.

[0099] Comparative Example 3

[0100] This comparative example provides an O1 / W / O2 type double emulsion, which is different from Example 1 only in that the water-soluble emulsifier lacks Tween 80, and its usage is distributed according to the ratio of flaxseed gum and whey protein isolate. For other references, refer to Example 1.

[0101] Test Example 1

[0102] Embedding rate test

[0103] Test method: Take a certain amount of emulsion, use UV-visible spectrophotometer to measure its absorbance to obtain the embedding amount of flavor, and calculate the flavor embedding rate (a) according to the following formula:

[0104] Where m is the mass of the effective loaded flavor; M is the mass of the weighed emulsion.

[0105] The emulsions provided in Examples 1-16 and Comparative Examples 1-3 were tested, and the results are shown in Table 1.

[0106] Table 1

[0107]

[0108]

[0109] The test results show that:

[0110] (1) It can be seen from Examples 1 to 16 that the O1 / W / O2 double emulsion provided by the present invention has good stability and a high flavor embedding rate by reasonably limiting the component types and ratios and important parameters in the preparation method.

[0111] (2) By comparing Example 1 with Examples 6-13, it can be seen that the present invention can further improve the stability and flavor embedding rate by further optimizing the ratio of each component in the emulsion;

[0112] By comparing Example 1 with Examples 14-16, it can be seen that the present invention further optimizes the heating temperature, stirring speed and ultrasonic power in the preparation method, so that the obtained emulsion has better stability and a higher flavor embedding rate.

[0113] (3) By comparing Example 1 with Comparative Examples 1-3, it can be seen that the stability and fragrance carrying rate of the obtained emulsion are further improved by rationally compounding the water-soluble emulsifiers and cooperating with each other among the various emulsifiers in the present invention.

[0114] Test Example 2

[0115] Release rate test

[0116] Test method: Take a certain amount of emulsion and heat it at 40℃, 50℃, 60℃, 70℃, 80℃ and 90℃ for 15min respectively. Measure its absorbance with UV-visible spectrophotometer, obtain the release amount of flavor according to the standard curve, and calculate the flavor release rate (b) according to the following formula:

[0117] Where m t is the amount of flavor released at the corresponding temperature; M is the total amount of flavor in the emulsion.

[0118] The emulsions provided in Examples 1-16 and Comparative Examples 1-3 were tested, and the results are shown in Table 2.

[0119] Table 2

[0120]

[0121]

[0122] The test results show that:

[0123] (1) It can be seen from Examples 1 to 16 that the O1 / W / O2 double emulsion provided by the present invention can achieve the slow release of flavor within the temperature range of 40-90° C., effectively realizing the sustained release function of the emulsion.

[0124] (2) By comparing Example 1 with Examples 6-16, it can be seen that when the proportions of the components of the emulsion in Examples 6-13 are too high or too low, and when the heating temperature, stirring speed and ultrasonic power in the preparation methods provided in Examples 14-16 are increased, the flavor of the obtained product is released prematurely at a lower temperature, and the sustained-release effect is reduced.

[0125] (3) By comparing Example 1 with Comparative Examples 1-3, it can be seen that the present invention further improves the sustained-release effect of the emulsion obtained by rationally compounding the water-soluble emulsifier and the oil-soluble emulsifier, and cooperating with each other among the multiple emulsifiers.

[0126] Test Example 3

[0127] Morphology test

[0128] Use an optical microscope to observe the microscopic morphology of the emulsion: take 10 μL of the emulsion and drop it on a glass slide and fix it on the stage, and use a 20× objective lens to observe the droplet size, morphology, distribution and surface structure of the emulsion.

[0129] The overall appearance of the products provided in Examples 1-5 after being placed for 60 days is as follows Figure 1 As shown, the microscopic morphology Figure 2 As shown, it is shown that the emulsion system provided by the present invention is uniform, the emulsion droplet size is 20-50 μm, and the stability is good.

[0130] The applicant declares that the above is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily thought of by those skilled in the art within the technical scope disclosed by the present invention are within the protection scope and disclosure scope of the present invention.

Claims

1. An O1 / W / O2 double emulsion, characterized in that: The O1 / W / O2 type double emulsion comprises an inner oil phase O1, an intermediate water phase W and an outer oil phase O2; the inner oil phase O1 comprises essence and a first solvent; the intermediate water phase W comprises a water-soluble emulsifier and water; the outer oil phase O2 comprises an oil-soluble emulsifier and a second solvent; The water-soluble emulsifier comprises a combination of flaxseed gum, whey protein isolate and Tween 80.

2. The O1 / W / O2 double emulsion according to claim 1, characterized in that The first solvent includes any one of ethanol, propylene glycol or caprylic acid glyceride or a combination of at least two thereof; Preferably, the second solvent comprises any one of propylene glycol, triacetin or caprylic decanoic acid glyceride or a combination of at least two thereof; Preferably, the oil-soluble emulsifier includes any one of Span 80, monoglycerol fatty acid ester or sucrose fatty acid ester, or a combination of at least two thereof.

3. The O1 / W / O2 double emulsion according to claim 1 or 2, characterized in that: The mass ratio of the essence to the first solvent is 1:(0.1-1.2), preferably 1:(0.15-0.5); Preferably, the mass ratio of the water-soluble emulsifier to water is 1:(7-19), preferably 1:(7-11.5); Preferably, the mass ratio of the oil-soluble emulsifier to the second solvent is 1:(7-19), preferably 1:(9-12).

4. The O1 / W / O2 double emulsion according to any one of claims 1 to 3, characterized in that The mass ratio of the intermediate layer water phase W to the inner layer oil phase O1 is 1:(0.5-1.5), preferably 1:(1-1.5); Preferably, the mass ratio of the sum of the inner oil phase O1 and the middle water phase W to the outer oil phase O2 is 1:(0.5-1.5), preferably 1:(0.8-1.2).

5. The O1 / W / O2 double emulsion according to any one of claims 1 to 4, characterized in that The mass ratio of the flaxseed gum, whey protein isolate and Tween 80 is 1:(0.5-1.5):(0.5-1.5).

6. A method for preparing an O1 / W / O2 double emulsion according to any one of claims 1 to 5, characterized in that: The preparation method comprises the following steps: (1) Mixing the essence and the first solvent to obtain an inner oil phase O1; mixing the water-soluble emulsifier and water to obtain an intermediate water phase W; mixing the oil-soluble emulsifier and the second solvent to obtain an outer oil phase O2; (2) adding the inner oil phase O1 to the middle water phase W, and after ultrasonic emulsification, obtaining O1 / W type colostrum; adding the O1 / W type colostrum to the outer oil phase O2, and after ultrasonic emulsification, obtaining the O1 / W / O2 type double emulsion.

7. The preparation method according to claim 6, characterized in that: In step (1), the water-soluble emulsifier and water are mixed or the oil-soluble emulsifier and the second solvent are mixed, and the mixing is carried out under conditions of heating and stirring in a water bath; Preferably, the temperature of the water bath heating is independently 25-40°C; Preferably, the stirring rate is independently 800-1200 r / min, and the stirring time is independently 2-10 min.

8. The preparation method according to claim 6 or 7, characterized in that: The adding method in step (2) is dropwise addition; Preferably, the adding is carried out under conditions of heating in a water bath and stirring; Preferably, the temperature of the water bath heating is independently 25-40°C; Preferably, the stirring rate is independently 800-1200 r / min, and the stirring time is independently 2-10 min.

9. The preparation method according to any one of claims 6 to 8, characterized in that: The power of the ultrasonic emulsification in step (2) is independently 100-200W, and the time of the ultrasonic emulsification is independently 2-10min.

10. Use of the O1 / W / O2 double emulsion according to any one of claims 1 to 5 in cigarette flavoring.

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