A method for preparing a low-surfactant transparent emulsified nano flavor
Through the tandem ultrasonic treatment method, the problem of preparing stable and transparent emulsified nanoflavors in transparent beverages in the prior art is solved, and the preparation of nanoemulsions with high transparency and stability under low surfactants is achieved, reducing production costs and energy consumption.
Patent Information
- Application Number
- CN202311607902.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-11-29
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2043-11-29
AI Technical Summary
The prior art is difficult to prepare a stable and transparent emulsified nanoflavor in transparent beverages, and the traditional method requires a large amount of surfactants, which is costly and unfavorable to the creation of clean labels.
The oil phase was divided into three ultrasonic treatments by using tandem ultrasonic treatment to prepare transparent emulsified nanoflavors with particle sizes of 10-60 nm and diluted 100 times the light transmittance is 90%-99%, and the amount of surfactant is low.
It realizes the preparation of transparent emulsified nanoflavors with high transparency and stability under low surfactants, reducing energy consumption and production costs, and meeting the requirements of green production.
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Figure CN117717157B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of food additives, and in particular relates to a method for preparing a low-surfactant transparent emulsified nano flavor. Background Art
[0002] Emulsified flavors are usually made by dispersing oil-soluble flavors into distilled water through surfactants and emulsification equipment. Emulsified flavors allow all kinds of oil-soluble flavors to be used in aqueous solutions; however, traditional emulsified flavors are white and turbid, which limits their application in the transparent beverage market. For example, in carbonated beverages such as cola and Sprite, tea beverages, and certain functional beverages, flavors not only need to give the product a certain aroma, but also need to be clear and transparent in the beverage product and have good stability, and ordinary emulsified flavors are difficult to meet these requirements.
[0003] In recent years, many transparent emulsions that can be prepared have been developed, and their droplet size is 10 to 80 nm. According to the amount of emulsifier used, they can be divided into microemulsions and nanoemulsions. Microemulsions are stable, translucent or transparent dispersions that are spontaneously formed by mixing water phase, oil phase, a large amount of surfactants and co-surfactants in appropriate proportions. However, microemulsions require a large amount of surfactants, and the ratio of surfactant to oil is often greater than 2, which increases costs and is not conducive to the creation of clean labels. Nanoemulsions are systems with high interfacial area and small droplet size, transparent or translucent appearance, low viscosity and high dynamic stability. The high-energy method for preparing nanoemulsions includes high-pressure homogenization, microfluidization, ultrasound, etc., which reduces the droplet size through a large amount of energy input, and the emulsion presents a transparent appearance. High-pressure homogenizer is the most commonly used emulsification equipment in the industry. The energy it generates can effectively reduce the size of droplets in the emulsion, but a large amount of heat is generated during the processing, and the temperature rises, which may damage the components and affect heat-sensitive active ingredients. At the same time, the formation of transparent nanoemulsions depends on surfactants, and the ratio of surfactants to oil is often greater than 0.5. Due to the small amount of emulsifier used, the emulsion is prone to become unstable and phase separation due to reasons such as Ostwald ripening.
[0004] The ultrasonic method has not yet been widely used in the preparation of transparent emulsified nano-flavors. The cavitation force generated by ultrasound causes the coarse emulsion to be crushed into nano-emulsion. The required particle size and stability of the nano-emulsion can be obtained by changing the ultrasonic energy input and time. The common ultrasonic frequency range is 20Hz~1.0MHz, and the processing time range is 5min~30min. The method is to continuously or intermittently crush for a specific period of time at a specific frequency, and the efficiency is low.
[0005] At present, the ultrasonic method has the disadvantages of low frequency and single processing method and cannot be applied to the preparation of transparent emulsified nano-flavors. Summary of the invention
[0006] The purpose of this section is to summarize some aspects of embodiments of the present invention and briefly introduce some preferred embodiments. Some simplifications or omissions may be made in this section and the specification abstract and the invention title of this application to avoid blurring the purpose of this section, the specification abstract and the invention title, and such simplifications or omissions cannot be used to limit the scope of the present invention.
[0007] In view of the above problems and / or the problems existing in the prior art, the present invention is proposed.
[0008] Therefore, the object of the present invention is to overcome the deficiencies in the prior art and provide a method for preparing a low-surfactant transparent emulsified nano flavor.
[0009] In order to solve the above technical problems, the present invention provides the following technical solutions: a method for preparing a low-surfactant transparent emulsified nano flavor, comprising:
[0010] Add an acidity regulator and a preservative into pure water and stir evenly to prepare a water phase;
[0011] Adding an oil-soluble emulsifier and a weighting agent into the oily fragrance base and stirring evenly to prepare an oil phase;
[0012] adding the oil phase to the water phase to obtain a mixed phase;
[0013] After the mixed phase is subjected to the first ultrasonic treatment, a milky white solution is obtained, and the appearance does not change due to the extension of the ultrasonic treatment time;
[0014] The milky white solution was subjected to a second ultrasonic treatment to obtain a translucent emulsion with a slight white glow;
[0015] The semi-transparent emulsion is subjected to a third ultrasonic treatment to obtain a nano-transparent emulsion;
[0016] The particle size of the emulsion is 10-60 nm, the transmittance after being diluted 100 times is 90%-99%, and the mass ratio of the oil-soluble emulsifier to the oily fragrance base is ≤2.
[0017] As a preferred embodiment of the preparation method of the present invention, the acidity regulator is one of citric acid and sodium bicarbonate or a mixture of the two.
[0018] As a preferred embodiment of the preparation method of the present invention, the preservative is potassium sorbate.
[0019] As a preferred embodiment of the preparation method of the present invention, the oily fragrance base is a mixture of one or more natural essential oils or artificially formulated oil-soluble flavors.
[0020] As a preferred embodiment of the preparation method of the present invention, the oil-soluble emulsifier is a mixture of any one or more of Tween 20, polyglycerol ester or sucrose ester.
[0021] As a preferred embodiment of the preparation method of the present invention, the weighting agent is a mixture of one or more of rosin glycerol ester, sucrose acetate isobutyrate and caprylic decanoic acid glyceride.
[0022] As a preferred embodiment of the preparation method of the present invention, the frequency of the first ultrasonic treatment is 10-50 kHz; the frequency of the second ultrasonic treatment is 1.0-1.8 MHz; and the frequency of the third ultrasonic treatment is 2.0-3.0 MHz.
[0023] As a preferred embodiment of the preparation method of the present invention, the time of the first to third ultrasonic treatments is 3 to 10 minutes respectively.
[0024] As a preferred embodiment of the preparation method of the present invention, the nano transparent emulsion comprises, by weight of raw materials, 30 to 75 parts of pure water, 5 to 20 parts of oily fragrance base, 0.01 to 0.5 parts of acidity regulator, 0.01 to 0.2 parts of preservative, 2 to 10 parts of oil-soluble emulsifier and 5 to 25 parts of weighting agent.
[0025] Another object of the present invention is to overcome the deficiencies in the prior art and provide a transparent emulsified nano flavor with low surfactant prepared by a preparation method.
[0026] Beneficial effects of the present invention:
[0027] (1) The present invention innovatively uses a tandem ultrasonic method to achieve graded crushing of the emulsion, thereby preparing a transparent nano-emulsified flavor with good transparency and stability; the amount of surfactant added in the present invention is low, the raw material composition is simple, the added chemical components are small, and the raw material composition is formulated strictly in accordance with national standards. It is safe and reliable and meets the requirements of green production. At the same time, it overcomes the problem that the existing transparent emulsified nano-flavor has poor transparency and is unstable in water.
[0028] (2) The present invention enables the oil-soluble flavor base to be completely added to the transparent beverage product, and the aroma is richer, fuller and more coordinated compared with the water-soluble flavor except terpenes; and no high-pressure homogenization equipment is required in the preparation process, which reduces energy waste and saves costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative labor. Among them:
[0030] Figure 1 These are the appearance pictures of the emulsion after the first, second and third ultrasonic treatments;
[0031] Figure 2 The particle size and dispersion index (PDI) of the transparent nano-emulsified flavor of Examples 1 to 11;
[0032] Figure 3 The appearance diagram of the nanoemulsion flavor of Example 1, Comparative Example 1, Comparative Example 2 and Comparative Example 3;
[0033] Figure 4 is the light transmittance of the transparent nano-emulsified flavor of Examples 1 to 11 after centrifugation at 6000 r / min for 10 min;
[0034] Figure 5 The appearance of the nanoemulsion flavor of Example 4 and Comparative Example 5;
[0035] Figure 6 The particle size and dispersion index (PDI) of the transparent nano-emulsified flavor of Comparative Examples 1 to 5 are shown. DETAILED DESCRIPTION
[0036] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific implementation methods of the present invention are described in detail below in conjunction with the embodiments of the specification.
[0037] In the following description, many specific details are set forth to facilitate a full understanding of the present invention, but the present invention may also be implemented in other ways different from those described herein, and those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.
[0038] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The term "in one embodiment" that appears in different places in this specification does not necessarily refer to the same embodiment, nor does it refer to a separate or selective embodiment that is mutually exclusive with other embodiments.
[0039] Example 1
[0040] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 83.6 parts of pure water and mix well to obtain the aqueous phase;
[0041] (2) adding 2 parts of Tween 20 and 9 parts of rosin glycerol ester to 5 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0042] (3) adding the oil phase to the water phase to obtain a mixed phase, and subjecting the mixed phase to ultrasonic treatment at 20 kHz for 5 minutes to obtain a milky white solution immediately; subjecting the milky white solution to ultrasonic treatment at 1.6 MHz for 5 minutes to obtain a translucent emulsion with a slight white glow;
[0043] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0044] Example 2
[0045] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0046] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0047] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0048] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0049] Example 3
[0050] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 56.1 parts of pure water and mix well to obtain the aqueous phase;
[0051] (2) adding 7.5 parts of Tween 20 and 21 parts of rosin glycerol ester to 15 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0052] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0053] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0054] Example 4
[0055] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0056] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0057] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 10 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0058] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0059] Example 5
[0060] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0061] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0062] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 30 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0063] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0064] Example 6
[0065] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0066] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0067] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.0 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0068] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0069] Example 7
[0070] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0071] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0072] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase by 20 kHz ultrasonic wave for 5 min to obtain a milky white solution immediately; treating the milky white solution by 2.0 MHz ultrasonic wave for 5 min to obtain a translucent emulsion with a slight white glow;
[0073] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0074] Example 8
[0075] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0076] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0077] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0078] The semi-transparent emulsion was treated with 2.0 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0079] Example 9
[0080] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 70.1 parts of pure water and mix well to obtain the aqueous phase;
[0081] (2) adding 4.5 parts of Tween 20 and 15 parts of rosin glycerol ester to 10 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0082] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a translucent emulsion with a slight white glow;
[0083] The semi-transparent emulsion was treated with 3.0 MHz ultrasound for 5 min to obtain a nano-transparent emulsion.
[0084] Example 10
[0085] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 56.1 parts of pure water and mix well to obtain the aqueous phase;
[0086] (2) adding 7.5 parts of Tween 20 and 21 parts of rosin glycerol ester to 15 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0087] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 3 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 3 min to obtain a translucent emulsion with a slight white glow;
[0088] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 3 min to obtain a nano-transparent emulsion.
[0089] Embodiment 11
[0090] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 56.1 parts of pure water and mix well to obtain the aqueous phase;
[0091] (2) adding 7.5 parts of Tween 20 and 21 parts of rosin glycerol ester to 15 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0092] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase by 20 kHz ultrasonic wave for 8 min to obtain a milky white solution immediately; treating the milky white solution by 1.6 MHz ultrasonic wave for 8 min to obtain a translucent emulsion with a slight white glow;
[0093] The semi-transparent emulsion was treated with 2.4 MHz ultrasound for 8 min to obtain a nano-transparent emulsion.
[0094] Comparative Example 1
[0095] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 56.1 parts of pure water and mix well to obtain the aqueous phase;
[0096] (2) adding 7.5 parts of Tween 20 and 21 parts of rosin glycerol ester to 15 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0097] (3) The water-in-oil emulsion was prepared by a low-energy method. The water phase was placed on a magnetic stirrer at a speed of 1500 r / min. The oil phase was injected into the water phase at a uniform speed using a syringe. After the injection, stirring was continued for 6 h.
[0098] Comparative Example 2
[0099] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 56.1 parts of pure water and mix well to obtain the aqueous phase;
[0100] (2) adding 7.5 parts of Tween 20 and 21 parts of rosin glycerol ester to 15 parts of sweet orange essential oil, and mixing them evenly to obtain the sweet orange essential oil phase;
[0101] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase by 20 kHz ultrasonic treatment for 10 min.
[0102] Comparative Example 3
[0103] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 61.6 parts of pure water and mix well to obtain the aqueous phase;
[0104] (2) adding 9 parts of Tween 20 and 9 parts of rosin glycerol ester to 20 parts of sweet orange essential oil and mixing them evenly to obtain the oil phase;
[0105] (3) adding the oil phase to the water phase to obtain a mixed phase; treating the mixed phase with 20 kHz ultrasound for 5 min to obtain a milky white solution immediately; treating the milky white solution with 1.6 MHz ultrasound for 5 min to obtain a slightly transparent emulsion with white light;
[0106] The transparency of the slightly transparent emulsion did not change significantly after being treated with 2.4 MHz ultrasound for 5 minutes.
[0107] The light transmittance of the present invention is measured by diluting the transparent emulsified essence 100 times and measuring the light transmittance at a wavelength of 500 nm using an ultraviolet spectrophotometer.
[0108] Table 1
[0109]
[0110]
[0111] According to Table 1, it can be seen from Examples 1, 2 and 3 that the amount of oily fragrance added has a great influence on the transmittance of the transparent emulsified nano flavor. The greater the amount of oily fragrance added, the lower the transmittance. When the amount of oily fragrance added is 15%, the transmittance of the transparent emulsified nano flavor dilution with a concentration of 1% is 99.0%, and the degree of transparency is acceptable to the market.
[0112] It can be seen from Examples 2 and 4 to 9 that within a certain range, the greater the frequency of the ultrasonic wave, the better the light transmittance of the essence dilution liquid; but after increasing to a certain value, the light transmittance of the essence dilution liquid no longer changes.
[0113] It can be seen from Example 10, Example 2, and Example 11 that within a certain range, the longer the ultrasonic treatment time is, the better the transmittance of the flavor dilution; but when the time is increased to 10 minutes, the transmittance of the flavor dilution does not change significantly compared to 5 minutes.
[0114] It can be seen from Example 1, Comparative Example 1 and Comparative Example 2 that there is a huge difference in the transmittance of the emulsions prepared by the tandem ultrasonic method, the low energy method and the ultrasonic method. The traditional low energy method and the acoustic wave method cannot form a transparent nanoemulsion under this formula. The transmittance of the emulsion dilutions prepared by the two methods is below 50%, while the emulsion prepared by the tandem ultrasonic method has good transparency, and the transmittance of its dilution is 99.9%.
[0115] It can be seen from Example 1 and Comparative Example 3 that when the proportion of oil-soluble flavor exceeds the preferred proportion, the tandem ultrasound method cannot prepare a good transparent nanoemulsion. It can be seen from Example 1, Comparative Example 4 and Comparative Example 5 that only under the conditions of three-step tandem ultrasound and ultrasound frequency from low to high can a good transparent nanoemulsion be prepared. Comparative Example 4 uses a two-step ultrasound method, and the transmittance of its dilution is only 38.2%. Comparative Example 5 is treated with 2.4MHz ultrasound for 15min, and the emulsion prepared by it quickly stratifies and is unstable.
[0116] according to Figure 1 It can be seen that the emulsion is turbid after the first ultrasonic treatment; the emulsion is translucent after the second ultrasonic treatment, but still glows white; the emulsion is clear and transparent after the third ultrasonic treatment, and the reference line is clearly visible.
[0117] according to Figure 2 , the particle size range of Examples 1 to 3 is 12 to 38 nm, the larger the proportion of oily fragrance base, the larger the particle size, the PDI is less than 0.3, and the transparent emulsified nano flavor has good dispersibility and stability; the particle size and PDI of Examples 4 to 9 are greatly affected by the ultrasonic frequency, the higher the frequency, the smaller the emulsion particle size and PDI, but after the first to third ultrasonic frequencies are increased to 20kHZ, 1.6MHz and 2.4MHZ, respectively, the emulsion particle size and PDI no longer change significantly; the ultrasonic treatment time of Examples 10, 2 and 11 is 3min, 5min and 10min, respectively. When the ultrasonic treatment time is less than 5min, the emulsion particle size and PDI decrease with the increase of the treatment time. When the ultrasonic treatment time is 10min, the emulsion particle size and PDI no longer change significantly.
[0118] according to Figure 3It can be seen that only the tandem ultrasonic method and the formula in the preferred ratio of this scheme can successfully prepare transparent emulsified nano flavors. The emulsion prepared by the formula exceeding the preferred ratio is not completely transparent. The emulsion prepared by the low energy method and ultrasonic method is milky and opaque.
[0119] according to Figure 4 It can be seen that after centrifugation at 6000r / min for ten minutes in Examples 1 to 11, the transmittance is still maintained above 90%, proving that the transparent nano-emulsified flavor prepared by the tandem ultrasound method has good centrifugal stability.
[0120] according to Figure 5 It can be seen that only the three-step serial ultrasonic method and the formula in the preferred ratio of this scheme can successfully prepare transparent emulsified nano-flavor. The emulsions prepared by the two-step serial ultrasonic method and the single-step ultrasonic method are not completely transparent and may even be stratified. Only the ultrasonic process with graded crushing can prepare transparent and stable nano-emulsions.
[0121] according to Figure 6 It can be seen that under the same formula, the emulsions prepared by low energy method, one-step ultrasound and two-step ultrasound all have larger particle sizes, and the PDI value is greater than the emulsion prepared by tandem ultrasound method, and the stability is poor. When the oil phase ratio exceeds the preferred ratio, the emulsion particle size is greater than 200nm and is opaque.
[0122] Comparative Example 4
[0123] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 83.6 parts of pure water and mix well to obtain the aqueous phase;
[0124] (2) adding 2 parts of Tween 20 and 9 parts of rosin glycerol ester to 5 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0125] (3) adding the oil phase to the water phase to obtain a mixed phase, and subjecting the mixed phase to 1.6 MHz ultrasonic treatment for 5 min to obtain a turbid emulsion;
[0126] The state of the turbid emulsion did not change significantly after being treated with 2.4 MHz ultrasound for 5 min.
[0127] Comparative Example 5
[0128] (1) Add 0.1 parts of potassium sorbate and 0.3 parts of citric acid to 83.6 parts of pure water and mix well to obtain the aqueous phase;
[0129] (2) adding 2 parts of Tween 20 and 9 parts of rosin glycerol ester to 5 parts of sweet orange essential oil and mixing well to obtain the oil phase;
[0130] (3) The oil phase was added to the water phase to obtain a mixed phase. After the mixed phase was treated with 2.4 MHz ultrasound for 15 min, the transparency of the emulsion did not change significantly and the emulsion separated into layers quickly after standing.
[0131] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present invention can be modified or replaced by equivalents without departing from the spirit and scope of the technical solutions of the present invention, which should all be included in the scope of the present invention.
Claims
1. A method for preparing a low-surfactant transparent emulsified nano flavor, characterized in that: include, Add an acidity regulator and a preservative into pure water and stir evenly to prepare a water phase; Adding an oil-soluble emulsifier and a weighting agent into the oily fragrance base and stirring evenly to prepare an oil phase; adding the oil phase to the water phase to obtain a mixed phase; The mixed phase was subjected to a first ultrasonic treatment at a frequency of 10 to 50 kHz to obtain a milky white solution whose appearance did not change due to the extension of the ultrasonic treatment time; The milky white solution was subjected to a second ultrasonic treatment at a frequency of 1.0-1.8 MHz to obtain a translucent emulsion with a slight white glow; The semi-transparent emulsion is subjected to a third ultrasonic treatment at a frequency of 2.0-3.0 MHz to obtain a nano-transparent emulsion; Among them, the emulsion particle size is 10~60nm, the transmittance after dilution 100 times is 90%~99%, and the mass ratio of oil-soluble emulsifier to oily fragrance base is ≤2; Among them, calculated by weight of raw materials, there are 30 to 75 parts of pure water, 5 to 15 parts of oily fragrance base, 0.01 to 0.5 parts of acidity regulator, 0.01 to 0.2 parts of preservative, 2 to 7.5 parts of oil-soluble emulsifier, and 5 to 25 parts of weighting agent.
2. The preparation method according to claim 1, characterized in that: The acidity regulator is one of citric acid and sodium bicarbonate or a mixture of the two.
3. The preparation method according to claim 1 or 2, characterized in that: The preservative is potassium sorbate.
4. The preparation method according to claim 1 or 2, characterized in that: The oily fragrance base is a mixture of one or more natural essential oils or artificially formulated oil-soluble flavors.
5. The preparation method according to claim 1, characterized in that: The oil-soluble emulsifier is any one or more of Tween 20, polyglycerol ester or sucrose ester.
6. The preparation method according to claim 1, characterized in that: The weighting agent is a mixture of one or more of rosin glycerol ester, sucrose acetate isobutyrate and caprylic decanoic acid glyceride.
7. The preparation method according to claim 1, characterized in that: The duration of the first to third ultrasonic treatments is 3 to 10 minutes each.
8. A low-surfactant transparent emulsified nano flavor obtained by the preparation method described in any one of claims 1 to 7.
Citation Information
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