Beverage nanoemulsion prepared by high-shear process
The preparation of beverage nanoemulsions through high shear mixing technology solves the problem of time and energy consumption in the prior art, and realizes the stability and efficient preparation of concentrated beverage nanoemulsions.
Patent Information
- Application Number
- CN202210352976.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2015-11-25
- Filing Date
- 2016-11-18
- Publication Date
- 2025-08-05
- Estimated Expiration
- 2036-11-18
AI Technical Summary
The prior art consumes time and energy in preparing beverage nanoemulsions, and cannot process concentrated viscous emulsions. The high-pressure homogenizer is prone to clogging and cannot meet the beverage stability needs.
The beverage nanoemulsion was prepared using high shear mixing technology, and a mixture of oil, emulsifier and water was mixed by a high shear stirrer to obtain a nanoemulsion with a particle size of 0.05 microns to 1 micron and a viscosity of 2,800 cp/10s-1 to 50,000 cp/10s-1, with the high pressure homogenization step omitting.
The batch cycle time is shortened, the demand for high-pressure homogenization is reduced, the stability of concentrated beverage nanoemulsions is achieved, and the preparation process is simplified.
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Figure CN114732096B_ABST
Abstract
Description
[0001] This application is a divisional application of application No. 201680068947.3. Background Art
[0002] The present disclosure relates to beverage nanoemulsions and methods of making such beverage nanoemulsions. More particularly, the present disclosure relates to methods of making beverage nanoemulsions using a high shear process.
[0003] Beverage nanoemulsions usually have a particle size of less than 1 micron, i.e. 95 <1 micron oil-in-water emulsions. Such nanoemulsions contain flavor oils or cloud oils, emulsifiers, water, and optionally preservatives. The oil level in the emulsion concentrates ranges between 6% and 10% by weight. In addition, using a weight ratio of emulsifier to oil greater than 1:1, combined with d 95 Target oil particle size of <1 micron to ensure physical stability in the beverage nanoemulsion and final beverage product.
[0004] The current manufacturing process for preparing such beverage nanoemulsions consists of the following two steps: (1) dispersing / dissolving the emulsifier in water and then adding the cloud oil or flavor oil to form an emulsion premix in a mixing tank; the emulsion particle size is usually d 95 >2 microns, further particle size reduction is required; (2) the emulsion premix formed in step (1) is pumped into a high-pressure homogenizer (pressure between 3000 psi and 5000 psi) to break down the oil droplet size into the target particle size (d 95 <1 micron). This two-step process is both time-consuming and energy-intensive. Furthermore, the current process cannot produce concentrated, viscous emulsions with low water content. High-pressure homogenizers, due to their inherent design (their small orifices are prone to clogging), are unable to process concentrated, viscous emulsions. Therefore, alternative methods for preparing concentrated beverage nanoemulsions are needed to address these limitations. Summary of the Invention
[0005] This Summary is intended to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key or essential features of the invention.
[0006] In one aspect, the present invention provides a method for preparing concentrated and diluted nanoemulsions that eliminates the homogenization step, thereby reducing batch cycle time by up to 50%. The method involves using high shear mixing techniques to prepare highly concentrated oil-in-water nanoemulsions. Nanoemulsion particle sizes that meet target sizes for beverage stability can be achieved using high shear mixing techniques without the need for a homogenization step when using high oil levels / high viscosities. The concentrated emulsion can be supplied as is or diluted to the desired oil level and viscosity.
[0007] In one aspect, the present disclosure provides a method for preparing a beverage nanoemulsion, the method comprising the following steps:
[0008] (a) providing a mixture comprising oil, an emulsifier, water, and optionally a preservative; and
[0009] (b) mixing the mixture using a high shear mixer to obtain a nanoemulsion, wherein the mixture has a shear strength of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 50,000cp / 10s -1 viscosity;
[0010] and
[0011] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 .
[0012] In one aspect, the mixture comprises 12% to 40% oil by weight.
[0013] In one aspect, the present disclosure provides a beverage nanoemulsion comprising:
[0014] (a) 12 to 40% by weight of oil;
[0015] (b) 1 to 30 wt % of an emulsifier;
[0016] (c) optionally a preservative; and
[0017] (d) water;
[0018] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 and 2,800cp / 10s -1 Up to 50,000cp / 10s -1 viscosity.
[0019] The weight % content in this specification refers to the amount of active ingredients in the final beverage nanoemulsion. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Some embodiments are illustrated by way of example and not by way of limitation in the accompanying drawings.
[0021] Figure 1 The viscosities of untreated Formulations A to C are shown.
[0022] Figure 2 The particle size of the emulsion obtained after high shear treatment of pre-emulsified Formulation A is shown, as well as the particle size of pre-emulsified Formulation A.
[0023] Figure 3The particle size of the emulsion obtained after high shear treatment of pre-emulsified Formulation B is shown, as well as the particle size of pre-emulsified Formulation B.
[0024] Figure 4 Shown are the emulsion particle sizes obtained after high shear treatment of pre-emulsified Formulation C.
[0025] Figure 5 The particle size of the emulsion obtained after high shear treatment of non-pre-emulsified Formulation C is shown, as well as the particle size of non-pre-emulsified Formulation C.
[0026] Figure 6 The particle sizes of the pre-high shear mixtures obtained in Formulations A to C are shown.
[0027] Figure 7 The particle size of the high shear mixtures obtained in Formulations A to C is shown.
[0028] Figure 8 Shown are the emulsion particle sizes obtained by high pressure homogenization of pre-emulsified Formulation A after two passes at 3000 psi, 4000 psi, and 5000 psi.
[0029] Figure 9 Shown are the emulsion particle sizes obtained by high pressure homogenization of pre-emulsified Formulation A after three passes at 3000 psi, 4000 psi, and 5000 psi.
[0030] Figure 10 Shown are the emulsion particle sizes obtained by high pressure homogenization of pre-emulsified Formulation B after one pass at 3000 psi, 4000 psi, and 5000 psi.
[0031] Figure 11 The effects of pressure, number of passes, and emulsion concentration on the emulsion particle size obtained after high-pressure homogenization of pre-emulsified formulations A and B are shown. DETAILED DESCRIPTION
[0032] definition
[0033] Unless otherwise specified or the context clearly indicates, as used herein, the numerical values disclosed herein should be understood to be within the normal tolerance range of the art, for example within 10% of the stated value. The weight % content in this specification refers to the content of the active ingredient in the final beverage nanoemulsion.
[0034] Open-ended terms such as “including,” “having,” “comprising,” and “containing” mean “comprising.” These open transition phrases are used to introduce an open list of elements, method steps, etc. that does not exclude additional, unrecited elements or method steps.
[0035] The transitional phrase "consisting of" and variations thereof exclude any elements, steps or ingredients not recited other than the impurities normally associated therewith.
[0036] The transitional phrase "consists essentially of" or variations such as "consist essentially of" or "consisting essentially of" excludes any elements, steps, or ingredients not recited except those that do not materially change the basic or novel characteristics of the specified method, structure, or composition.
[0037] In addition, the indefinite articles "a" and "an" placed before elements or components in the present invention are non-limiting articles with respect to the number of instances (i.e., the number of times the element or component occurs). Therefore, "a" or "an" should be understood to include one or at least one, and the singular form of the element or component also includes the plural form unless the number is obviously intended to be singular.
[0038] As used herein, the terms "invention" or "disclosure" are non-limiting terms and are not intended to refer to any single embodiment of a particular invention, but rather encompass all possible embodiments as described in this application.
[0039] Method for preparing beverage nanoemulsion
[0040] In one aspect, the present disclosure provides a method for preparing a beverage nanoemulsion, the method comprising the following steps:
[0041] (a) providing a mixture comprising oil, an emulsifier, water, and optionally a preservative; and
[0042] (b) mixing the mixture using a high shear mixer to obtain a nanoemulsion, wherein the mixture has a shear strength of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 50,000cp / 10s -1 viscosity;
[0043] and
[0044] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 .
[0045] In one aspect, the mixture comprises 12% to 40% oil by weight.
[0046] In one aspect, the method of preparing a beverage nanoemulsion further comprises adding water to the nanoemulsion to obtain a diluted nanoemulsion, wherein the diluted nanoemulsion contains 6 wt% to 10 wt% oil, and wherein the diluted nanoemulsion has a particle size d of 0.05 microns to 1 micron. 95 .
[0047] In one aspect, the present disclosure provides a beverage nanoemulsion comprising:
[0048] (a) 12 to 40% by weight of oil;
[0049] (b) 1 to 30 wt % of an emulsifier;
[0050] (c) optionally a preservative; and
[0051] (d) water;
[0052] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 and 2,800cp / 10s -1 Up to 50,000cp / 10s -1 viscosity.
[0053] In some embodiments, the oil used in the present disclosure is a hydrophobic clouding agent. The hydrophobic clouding agent can be selected from sterol esters, stanol esters, and combinations thereof.
[0054] In addition to providing turbidity, sterol esters and stanol esters have also been shown to provide health benefits, such as reducing low-density lipoprotein (LDL) cholesterol levels in humans if about 1.3 grams is consumed regularly per day. Sterol esters and stanol esters are esterified forms of free sterols and free stanols, respectively. Stanols are saturated or hydrogenated forms of sterols or plant sterols.
[0055] Phytosterols can be derived from vegetable oils or tall oil. Common sources of plant oil sterols include, but are not limited to, coconut oil, corn oil, cottonseed oil, olive oil, palm oil, peanut oil, rapeseed oil, canola oil, safflower oil, linseed oil, cottonseed oil, soybean oil, sunflower oil, walnut oil, and avocado oil. Additionally, sterols can be derived from tall oil. Tall oil can be obtained from coniferous trees.
[0056] Unlike free sterols, stanols in free and esterified forms are not readily available from natural sources. Therefore, free sterols must be hydrogenated to produce free stanols, and free sterols and free stanols must be esterified to produce sterol esters and stanol esters. Suitable esterified forms of sterols and stanols are available from Raisio Benecol and McNeil Nutritionals under the trade name Obtained from Archer Daniels Midland Company under the trade name Obtained from Cognis Corporation under the trade name Obtained from MultiBene MultiBeneGroup under the trade name and commercially available from other well-known companies in the field.
[0057] In some embodiments, oils include, but are not limited to, unflavored oils, flavored oils, and combinations thereof.
[0058] As known to those skilled in the art, non-limiting examples of flavorless oils include medium chain triglycerides, vegetable oils, grapeseed oil, and the like. Non-limiting examples of suitable vegetable oils include soybean oil, palm oil, rapeseed oil, sunflower seed oil, peanut oil, cottonseed oil, olive oil, avocado oil, coconut oil, safflower oil, other vegetable oils known to those skilled in the art, and combinations thereof. In one embodiment, the oil is coconut oil.
[0059] As known in the art, non-limiting examples of flavor oils include citrus oils, kola nut oil, essential oils, etc. Non-limiting examples of essential oils include almond oil, grapefruit oil, cinnamon oil, lemon oil, lime oil, tangerine oil, peppermint oil, orange oil, etc., and combinations thereof, as known to those skilled in the art.
[0060] In some embodiments, the oil is present in the beverage nanoemulsion in an amount of 10% to 50% by weight. In some embodiments, the oil is present in the beverage nanoemulsion in an amount of 12% to 40% by weight, 12% to 35% by weight, 12% to 30% by weight, 12% to 25% by weight, 12% to 20% by weight, 16% to 40% by weight, 16% to 35% by weight, 16% to 30% by weight, 16% to 25% by weight, 16% to 20% by weight, 20% to 40% by weight, 20% to 35% by weight, 20% to 30% by weight, 20% to 25% by weight, 25% to 40% by weight, 25% to 35% by weight, 25% to 30% by weight, 30% to 40% by weight, 30% to 35% by weight, and 35% to 40% by weight. In some embodiments, the oil is present in the beverage nanoemulsion in an amount of 14% to 30% by weight, 14% to 28% by weight, 14% to 26% by weight, 14% to 24% by weight, 14% to 22% by weight, and 14% to 20% by weight. In some embodiments, the oil is present in the beverage nanoemulsion in an amount of 16% to 20% by weight. The desired amount of oil can depend on the viscosity of the nanoemulsion.
[0061] In some embodiments, a beverage nanoemulsion having a higher percentage of oil can be diluted with water to obtain a beverage nanoemulsion having a lower percentage of oil.
[0062] In some embodiments, the emulsifiers used in the present disclosure include, but are not limited to, gum arabic, modified starch, pectin, xanthan gum, guar gum, propylene glycol alginate, monoglycerides, diglycerides, sodium dioctyl sulfosuccinate (DOSS), polyoxyethylene (20) sorbitan monolaurate ( 20), polyoxyethylene (20) sorbitan monopalmitate ( 40), polyoxyethylene (20) sorbitan monostearate ( 60), polyoxyethylene (20) sorbitan monooleate ( 80), Sorbitan monolaurate ( 20), Sorbitan monopalmitate ( 40), betaine, other emulsifiers known to those skilled in the art, and combinations thereof. Preferably, the emulsifier is selected from gum arabic, modified starch, pectin, xanthan gum, guar gum, propylene glycol alginate, and combinations thereof. In one embodiment, the emulsifier is modified starch.
[0063] In some embodiments, the emulsifier is present in the beverage nanoemulsion in an amount of 1% to 40% by weight. In some embodiments, the oil is present in the beverage nanoemulsion in an amount of 1% to 30%, 1% to 25%, 1% to 20%, 1% to 15%, 5% to 30%, 5% to 25%, 5% to 20%, 5% to 15%, 10% to 30%, 10% to 25%, 10% to 20%, 10% to 15%, 15% to 30%, 15% to 25%, 15% to 20%, 20% to 30%, and 20% to 25% by weight. In some embodiments, the oil is present in the beverage nanoemulsion in amounts of 14%, 16%, 18%, 20%, 22%, 24%, 26%, 28%, and 30% by weight. The amount of emulsifier required can depend on the amount of oil present and the type of emulsifier and should be sufficient to prepare a stable nanoemulsion.
[0064] In some embodiments, the beverage nanoemulsion further comprises a preservative. Non-limiting examples of preservatives include citric acid, sorbic acid, benzoic acid, their alkali metal salts, and any mixtures thereof.
[0065] The high shear mixing step can be performed by any suitable agitator known to those skilled in the art. Non-limiting examples of suitable agitators include turbine agitators, static agitators, and other high shear agitators known to those skilled in the art. Turbine agitators are available from Scott Static mixers (sometimes referred to in the art as motionless mixers or in-line mixers) come in a variety of sizes and geometries and are commercially available from companies known in the art such as Sulzer Corp., Winterthur, Switzerland, Chemineer Inc., Dayton, Ohio, a subsidiary of Charles Ross & Son Co., Hauppauge, NY, and Sulzer Chemtech Ltd.
[0066] A high shear mixer has two parallel surfaces arranged in close proximity. The material to be mixed is placed between the surfaces. The shear rate is the relative velocity of the surfaces divided by the distance between the surfaces. The surfaces can have a variety of configurations, such as parallel plates or annular cylindrical surfaces. Any shear mixer known in the art that can achieve the shear rates described herein can be used. The shear rate (s) of a gamma rotor stator mixer is -1 ) is the rotor tip speed V 尖端 The ratio between the stator and rotor tip speed V (m / s) and the distance g (m) between the stator and rotor. 尖端 =π*D*n, where D is the rotor diameter (m) and n is the rotational speed in revolutions per second (n is defined as RPM / 60).
[0067] In some embodiments, the mixture comprises oil and the emulsifier is at 20,000s -1 to 300,000s -1 In some embodiments, the mixture comprises oil and the emulsifier is stirred at a shear rate of at least 20,000 s -1 30,000s -1 50,000s -1 , 100,000s -1 , 150,000s -1 , 200,000s -1 250,000s -1 and 300,000s -1 In some embodiments, the mixture comprises oil and the emulsifier is stirred at a shear rate of 20,000 s -1 to 300,000s -1 30,000s -1 to 300,000s-1 50,000s -1 to 300,000s -1 , 100,000s -1 to 300,000s -1 , 150,000s -1 to 300,000s -1 , 200,000s -1 to 300,000s -1 250,000s -1 to 300,000s -1 , 20,000s -1 to 250,000s -1 , 20,000s -1 to 200,000s -1 , 20,000s -1 to 200,000s -1 , 20,000s -1 to 150,000s -1 , 20,000s -1 Up to 100,000s -1 , 20,000s -1 to 50,000s -1 and 20,000s -1 to 30,000s -1 Stirring at a shear rate.
[0068] The viscosity of a mixture comprising oil, emulsifier and water can be measured using an Anton Paar RheoQC rheometer. The viscosity of such an emulsion versus shear rate is measured using a concentric cylinder (CC27) measuring cup and corresponding spindle. Measuring the viscosity of the same sample using different types of equipment may result in different measured values. The values discussed herein are measured using an Anton Paar RheoQC rheometer and should be compared to measurements of the same equipment. In some embodiments, the mixture has a viscosity of 2,800 cp / 10s during at least a portion of the high shear stirring period. -1 Up to 50,000cp / 10s -1 In some embodiments, the mixture has a viscosity of 3000 cp / 10s -1 Up to 50,000cp / 10s -1 、5000cp / 10s -1 Up to 50,000cp / 10s -1 、10,000cp / 10s -1 Up to 50,000cp / 10s -1 、20,000cp / 10s-1 Up to 50,000cp / 10s -1 、30,000cp / 10s -1 Up to 50,000cp / 10s -1 and 40,000cp / 10s -1 Up to 50,000cp / 10s -1 In some embodiments, the mixture has a viscosity of 2800 cp / 10s -1 Up to 40,000cp / 10s -1 、2800cp / 10s -1 Up to 30,000cp / 10s -1 、2800cp / 10s -1 Up to 20,000cp / 10s -1 、2800cp / 10s -1 Up to 10,000cp / 10s -1 、2800cp / 10s -1 Up to 5000cp / 10s -1 、2800cp / 10s -1 Up to 4000cp / 10s -1 , and 2800cp / 10s -1 Up to 3000cp / 10s -1 .
[0069] The particle size of the beverage nanoemulsion can be measured using a laser diffraction particle size analyzer that is capable of measuring particle sizes between 30 nm and 3000 μm. The particle size distribution of the nanoemulsion is measured using a Horiba LA-950 model. Unless otherwise specified, the particle size or particle diameter in this disclosure refers to the particle diameter. 95 In some embodiments, the nanoemulsion has a particle size d 95 In some embodiments, the beverage nanoemulsion has a particle size d 95 0.05 micron, 0.1 micron, 0.2 micron, 0.3 micron, 0.4 micron, 0.5 micron, 0.6 micron, 0.7 micron, 0.8 micron and 0.9 micron. In some embodiments, the beverage nanoemulsion has a particle size d 95 0.1 μm to 1 μm, 0.2 μm to 1 μm, 0.3 μm to 1 μm, 0.4 μm to 1 μm, 0.5 μm to 1 μm, 0.6 μm to 1 μm, 0.7 μm to 1 μm, 0.8 μm to 1 μm, and 0.9 μm to 1 μm. In some embodiments, the beverage nanoemulsion has a particle size d 95 0.2 micron to 0.8 micron, 0.3 micron to 0.6 micron, and 0.4 micron to 0.5 micron.
[0070] Those skilled in the art will appreciate that the beverage nanoemulsions according to the present invention may be incorporated into a beverage at any suitable stage during the beverage manufacturing process.
[0071] The following examples are intended to illustrate specific preferred embodiments of the present invention, but are not intended to limit the scope of the present invention.
[0072] Example
[0073] Concentrated beverage nanoemulsions can be prepared using a mixing tank equipped with an internal or external high shear rotor stator agitator. Disclosed herein is a method for preparing concentrated nanoemulsions (12% to 40% oil by weight) using high shear mixing. Also disclosed herein is a method for preparing diluted nanoemulsions (6% to 10% oil by weight) by diluting the concentrated nanoemulsion to the desired level with water. The disclosed method reduces batch cycle time and eliminates the need for high pressure homogenization.
[0074] Example 1: Formulations A to C
[0075] The three types of formulations used are shown in Table 1. Formulation A is a standard formulation containing 10% by weight coconut oil. Formulations B and C are more concentrated than Formulation A, resulting in 38% and 50% reductions in volume, respectively. Formulations A to C were obtained by mixing the specified amounts of coconut oil, modified food starch, sodium benzoate, citric acid, and water.
[0076] Table 1: Compositions of three formulations used to prepare beverage nanoemulsions .
[0077]
[0078]
[0079] Formulations A to C have different viscosities. Formulations B and C have higher viscosities than Formulation A ( Figure 1 and Table 2). Formulation C could not be processed through a high-pressure homogenizer due to its high viscosity. Viscosities were measured comparing the shear rates of Formulations A to C using a Paar RheoQC rheometer with a concentric cylinder (CC27) measuring cup and corresponding spindle.
[0080] Table 2: Viscosities of the three formulations after mixing the ingredients without further processing .
[0081] <![CDATA[10s -1 ]]> <![CDATA[100s -1 ]]> <![CDATA[250s -1 ]]> Recipe A 35.6 46.4 47 Recipe B 2980 1950 1570 Recipe C 25600 10300 5650
[0082] Example 2: High shear treatment of pre-emulsified mixture
[0083] Formulations A to C were pre-emulsified at 25°C for 30 minutes using a pre-mix vessel equipped with a turbine agitator running at 150 RPM.
[0084] The pre-emulsified mixture was then processed in a high shear rotor stator mixer. Figures 2 to 4 The shear range of the rotor stator stirrer housing is as follows: 25kRPM for 300000s -1 , 20kRPM is 240,000s -1 , 15kRPM is 180,000s -1 .
[0085] Pre-emulsified Formulation A (10 wt% oil) had a d 95 ,like Figure 2 As shown in the middle curve 210. In the recirculation mode with up to 3 passes and up to 300,000s -1 The pre-emulsified Formulation A was processed using a high shear rotor stator agitator at a shear rate of (25 kRPM) for 5 minutes. Figure 2 The middle curves 220, 230, and 240 show the particle size (d 95 ) are 5.0μm, 4.1μm and 3.1μm respectively.
[0086] Pre-emulsified Formulation B (16 wt% oil) had a particle size (d 95 ),like Figure 3 The particle size (d) of the emulsion obtained after three high shear treatments at 15k, 20k and 25k RPM is shown in the middle curve 310. 95 ) are 0.83μm, 0.65μm and 0.69μm respectively. Figure 3 This is shown as curves 320 , 330 and 340 .
[0087] For pre-emulsified formulation C (20 wt% oil), a particle size (d 95 ) is less than 0.5μm( Figure 4 ) lotion, only 180,000s -1 to 300,000s -1 Curves 410, 420 and 430 show that the particle sizes of the emulsions obtained after a high shear treatment at 15k, 20k and 25k RPM are 0.43 μm, 0.37 μm and 0.44 μm, respectively.
[0088] Example 3: High Shear Treatment of Non-Pre-Emulsified Mixtures
[0089] Recirculation mode with up to 3 passes and a range of 180,000s -1(15kRPM) to 300,000s -1 Formulation C (20 wt% oil) was processed at a shear rate of (25 kRPM) using a high shear rotor stator agitator at 25-40°C for 5 minutes.
[0090] The results are as follows Figure 5 shown. Figure 5 The middle curves 520, 530 and 540 show that the particle size (d 95 ) are 0.69μm, 0.63μm and 0.57μm respectively.
[0091] Example 4: Comparison of the mixture before high shear and the emulsion after high shear
[0092] Formulations A to C were added to a batch mixer equipped with a central stirrer and an in-line rotor stator high shear mixer. High shear was paused in the tank and each formulation was mixed at an agitator speed of 150 RPM at 20°C. The particle size of the resulting high shear mixture was measured and the results were recorded. Figure 6 Curves 610, 620 and 630 show that the particle size (d 95 ) are 40μm, 15μm and 4μm respectively.
[0093] The mixture was then stirred with a rotor-stator high shear mixer at a speed of 2500 RPM and 30,000 s -1 The mixture was treated for 10 minutes at a shear rate of 1000 nm. The particle size of the emulsion after high shear was measured. Figure 7 Curves 710, 720 and 730 show that the particle size (d 95 ) are 1.05μm, 0.32μm and 0.29μm respectively.
[0094] Example 5: High-pressure homogenization of pre-emulsified formula A
[0095] In contrast, experiments were conducted by high pressure homogenization to prepare nanoemulsions from formulations A to C. As described in Example 2, formulations A to C each obtained a pre-emulsified mixture.
[0096] The pre-emulsified mixture was processed through an APV high pressure homogenizer 1, 2, and 3 times at pressures between 3000 psi and 5000 psi. Figure 8 Curve 830 in FIG. 1 shows that Formulation A (10 wt. % oil) can produce a nanoemulsion with a particle size (d ) less than 1 μm after two homogenizations at 5000 psi. 95 ). Figure 9Curves 910, 920 and 930 in FIG. 3 show that after three homogenizations at 3000 psi, 4000 psi and 5000 psi, Formula A can make the nanoemulsion have a particle size (d 95 ).
[0097] Example 6: High-pressure homogenization of pre-emulsified formulation B
[0098] The pre-emulsified mixture of Formulation B (16 wt% oil) was processed through the APV high pressure homogenizer once, twice, and three times at pressures between 3000 psi and 5000 psi. The pre-emulsified Formulation B was difficult to process through the benchtop high pressure homogenizer due to its higher viscosity. The pre-emulsified mixture of Formulation B could not be processed through the larger high pressure homogenizer due to its higher viscosity. The pre-emulsified mixture of Formulation C could not be processed through either the benchtop or larger high pressure homogenizers due to its even higher viscosity.
[0099] Figure 10 Curves 1010, 1020 and 1030 in FIG. 3 show that the obtained emulsions have a particle size (d) less than 1 μm after only one homogenization at 3000 psi, 4000 psi and 5000 psi, respectively. 95 ).
[0100] For pre-emulsified formulas A and B, the effects of pressure and number of passes on emulsion particle size are as follows: Figure 11 When the number of passes is zero, the particle size (d 95 ) is greater than 4 μm, while the particle size of pre-emulsified formula B (d 95 ) is less than 1μm.
[0101] The above description of the specific embodiments will fully reveal the general nature of the present invention so that others can easily modify and / or adjust these specific embodiments for various applications without departing from the overall concept of the present disclosure by applying the knowledge of the technical field without undue experimentation. Therefore, based on the teachings and guidance given herein, these adjustments and modifications are intended to fall within the meaning and scope of equivalents of the disclosed embodiments. It should be understood that the wording or terminology herein is for descriptive rather than limiting purposes, and thus the terms or wording of this specification should be interpreted by those skilled in the art in accordance with the teachings and guidance.
[0102] The breadth and scope of the present disclosure should not be limited by any of the above-described exemplary embodiments, but should be defined only in accordance with the following claims and their equivalents.
[0103] All aspects, embodiments, and options described herein may be combined in any and all variations.
[0104] All publications, patents, and patent applications mentioned in this specification are herein incorporated by reference to the same extent as if each individual publication, patent, or patent application was specifically and individually indicated to be incorporated by reference.
[0105] This application specifically relates to the following technical solutions.
[0106] 1. A method for preparing a beverage nanoemulsion, the method comprising the following steps:
[0107] (a) providing a mixture comprising oil, an emulsifier, water, and optionally a preservative; and
[0108] (b) mixing the mixture using a high shear mixer to obtain the nanoemulsion, wherein the mixture has a shear strength of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 50,000cp / 10s -1 viscosity; and
[0109] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 .
[0110] 2. The method according to technical solution 1, wherein the mixture contains 12% to 40% by weight of the oil.
[0111] 3. The method according to any one of technical solutions 1 and 2, wherein the oil is an odorless oil, and the odorless oil is selected from medium-chain triglycerides, grape seed oil, soybean oil, palm oil, rapeseed oil, sunflower seed oil, peanut oil, cottonseed oil, olive oil, avocado oil, coconut oil, safflower oil and combinations thereof.
[0112] 4. The method according to any one of technical solutions 1 and 2, wherein the oil is a flavor oil, and the flavor oil is selected from citrus oil, cola nut oil, almond oil, grapefruit oil, cinnamon oil, lemon oil, lime oil, tangerine oil, mint oil, orange oil and combinations thereof.
[0113] 5. The method according to any one of technical solutions 1 and 2, wherein the oil is a hydrophobic turbidity agent, and the hydrophobic turbidity agent is selected from sterol esters, stanol esters and combinations thereof.
[0114] 6. The method according to any one of technical solutions 1 to 5, wherein the oil is present in an amount of 14 wt % to 28 wt %.
[0115] 7. The method according to any one of technical solutions 1 to 5, wherein the oil is present in an amount of 20 wt %.
[0116] 8. The method according to any one of technical solutions 1 to 7, wherein the emulsifier is selected from gum arabic, modified starch, pectin, xanthan gum, guar gum, propylene glycol alginate and combinations thereof.
[0117] 9. The method according to any one of technical solutions 1 to 8, wherein the emulsifier is present in an amount of 1 wt % to 30 wt %.
[0118] 10. The method according to any one of technical solutions 1 to 8, wherein the emulsifier is present in an amount of 10 wt % to 30 wt %.
[0119] 11. The method according to any one of technical solutions 1 to 10, wherein the mixture is stirred at 20,000 s -1 to 300,000s -1 Stirring at a shear rate.
[0120] 12. The method according to any one of technical solutions 1 to 10, wherein the mixture is stirred at 30,000 s -1 to 250,000s -1 Stirring at a shear rate.
[0121] 13. The method according to any one of technical solutions 1 to 12, wherein the nanoemulsion has a particle size d of 0.2 to 0.8 microns. 95 .
[0122] 14. The method according to any one of technical solutions 1 to 12, wherein the nanoemulsion has a particle size d of 0.3 to 0.6 microns. 95 .
[0123] 15. The method according to any one of technical solutions 1 to 14, wherein the mixture has a flow rate of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 30,000cp / 10s -1 viscosity.
[0124] 16. The method according to technical solution 1, further comprising adding water to the nanoemulsion to obtain a diluted nanoemulsion, wherein the diluted nanoemulsion contains 6% to 10% by weight of the oil, and wherein the diluted nanoemulsion has a particle size d of 0.05 μm to 1 μm. 95 .
[0125] 17. A beverage nanoemulsion, comprising:
[0126] (a) oil in an amount of 12% to 40% by weight;
[0127] (b) an emulsifier in an amount of 1% to 30% by weight;
[0128] (c) optionally a preservative; and
[0129] (b) water;
[0130] The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 and 2800cp / 10s -1 Up to 50,000cp / 10s -1 viscosity.
[0131] 18. The nanoemulsion of claim 17, wherein the oil is an odorless oil selected from the group consisting of medium-chain triglycerides, grapeseed oil, soybean oil, palm oil, rapeseed oil, sunflower seed oil, peanut oil, cottonseed oil, olive oil, avocado oil, coconut oil, safflower oil, and combinations thereof.
[0132] 19. The nanoemulsion according to technical solution 17, wherein the oil is a flavor oil selected from citrus oil, cola nut oil, almond oil, grapefruit oil, cinnamon oil, lemon oil, lime oil, tangerine oil, mint oil, orange oil, and combinations thereof.
[0133] 20. The nanoemulsion according to technical solution 17, wherein the oil is a hydrophobic turbidity agent, and the hydrophobic turbidity agent is selected from sterol esters, stanol esters and combinations thereof.
[0134] 21. The nanoemulsion according to any one of technical solutions 17 to 20, wherein the oil is present in an amount of 14 wt % to 28 wt %.
[0135] 22. The nanoemulsion according to any one of technical solutions 17 to 20, wherein the oil is present in an amount of 20 wt%.
[0136] 23. The nanoemulsion according to any one of technical solutions 17 to 22, wherein the emulsifier is selected from gum arabic, modified starch, pectin, xanthan gum, guar gum, propylene glycol alginate and combinations thereof.
[0137] 24. The nanoemulsion according to any one of technical solutions 17 to 23, wherein the emulsifier is present in an amount of 10 wt % to 30 wt %.
[0138] 25. The nanoemulsion according to any one of technical solutions 17 to 23, wherein the emulsifier is present in an amount of 20 wt% to 30 wt%.
[0139] 26. The nanoemulsion according to any one of technical solutions 17 to 25, wherein the nanoemulsion has a particle size d of 0.2 to 0.8 microns.95 .
[0140] 27. The nanoemulsion according to any one of technical solutions 17 to 25, wherein the nanoemulsion has a particle size d of 0.3 microns to 0.6 microns. 95 .
[0141] 28. The nanoemulsion according to any one of technical solutions 17 to 27, wherein the nanoemulsion has a viscosity of 2800 cp / 10s -1 Up to 30,000cp / 10s -1 viscosity.
Claims
1. A beverage nanoemulsion, comprising: (a) oil in an amount of 12% to 40% by weight; (b) an emulsifier in an amount of 1% to 30% by weight; (c) optionally a preservative; and (b) water; The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 and 2800cp / 10s -1 Up to 50,000cp / 10s -1 The viscosity, wherein the nanoemulsion is not processed by a high pressure homogenizer during preparation, and The nanoemulsion was prepared by using a high shear mixer at 150,000 s -1 to 300,000s -1 formed at a shear rate of .
2. The nanoemulsion of claim 1 , wherein the oil is an odorless oil selected from the group consisting of medium chain triglycerides, grapeseed oil, soybean oil, palm oil, rapeseed oil, sunflower seed oil, peanut oil, cottonseed oil, olive oil, avocado oil, coconut oil, safflower oil, and combinations thereof.
3. The nanoemulsion of claim 1, wherein the oil is a flavor oil selected from the group consisting of citrus oil, cola nut oil, almond oil, grapefruit oil, cinnamon oil, lemon oil, lime oil, tangerine oil, peppermint oil, orange oil, and combinations thereof.
4. The nanoemulsion of claim 1, wherein the oil is a hydrophobic clouding agent selected from the group consisting of sterol esters, stanol esters, and combinations thereof.
5. The nanoemulsion of claim 1, wherein the oil is present in an amount of 14% to 28% by weight.
6. The nanoemulsion of claim 1, wherein the emulsifier is selected from the group consisting of gum arabic, modified starch, pectin, xanthan gum, guar gum, propylene glycol alginate, and combinations thereof.
7. The nanoemulsion of claim 1, wherein the emulsifier is present in an amount of 20% to 30% by weight.
8. The nanoemulsion of claim 1, wherein the nanoemulsion has a particle size d of 0.2 to 0.8 microns. 95 .
9. A beverage nanoemulsion prepared by a method comprising the steps of: using a high shear mixer at 150,000 s -1 to 300,000s -1 A mixture comprising 12% to 40% by weight of oil, an emulsifier, and optionally a preservative is mixed at a shear rate of 2,800 cp / 10s during at least a portion of the stirring period to obtain the nanoemulsion; wherein the mixture has a shear rate of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 50,000cp / 10s -1 viscosity; The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 ,and wherein the mixture is not processed through a high pressure homogenizer.
10. The nanoemulsion of claim 9, wherein the oil is present in an amount of 14% to 28% by weight.
11. The nanoemulsion of claim 9, wherein the emulsifier is present in an amount of 10% to 30% by weight.
12. A method for preparing a beverage nanoemulsion comprising using a high shear mixer at 150,000 s -1 to 300,000s -1 A mixture comprising 12% to 40% by weight of oil, an emulsifier, and optionally a preservative is mixed at a shear rate of 2,800 cp / 10s during at least a portion of the stirring period to obtain the nanoemulsion; wherein the mixture has a shear rate of 2,800 cp / 10s during at least a portion of the stirring period. -1 Up to 50,000cp / 10s -1 viscosity; The nanoemulsion has a particle size of 0.05 μm to 1 μm. 95 ,and wherein the mixture is not processed through a high pressure homogenizer.
13. The method of claim 12, wherein the emulsifier is present in an amount of 10% to 30% by weight.
14. The method of claim 12, wherein the mixture comprises a preservative selected from the group consisting of citric acid, sorbic acid, benzoic acid, alkali metal salts thereof, and any mixtures thereof.
15. The method of claim 14, wherein the preservative is present in an amount of 0.15% to 0.3% by weight.
16. The method of claim 12, further comprising adding water to the nanoemulsion to obtain A diluted nanoemulsion is obtained, wherein the diluted nanoemulsion comprises 6 wt % to 10 wt % of oil.
Citation Information
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