Water dispersible ceramide product as well as preparation method and preparation system thereof
Through the ultrasonic microfluidic process, the dispersed ceramide phase and the aqueous phase are emulsified in the ultrasonic nanodisperser, and the additive phase is added, which solves the problem of time-consuming and labor-intensive preparation of ceramides in water and the prior art, and realizes the preparation of water-dispersed nanoceramide products with uniform particle size and stable particle size, and improves production flexibility and efficiency.
Patent Information
- Application Number
- CN202311207253.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-18
- Publication Date
- 2025-03-18
- Estimated Expiration
- 2043-09-18
AI Technical Summary
Ceramide is difficult to dissolve in water and is easy to crystallize and precipitate, which limits its wide application. In the prior art, such as the use of liposome wrapping, there are problems such as small loading of active substances and uneven particle sizes. The preparation method is often intermittent operation, which is time-consuming and labor-intensive, and has low flexibility.
A new continuous flow preparation process for water-dispersed nanoceramides was developed using ultrasonic microfluidic technology. The dispersed ceramide phase and the aqueous phase were emulsified by the ultrasonic nanodisperser, and the additive phase was added at different nodes to achieve the preparation of water-dispersed nanoceramide products with uniform particle size and stable system.
The preparation of water-dispersed nanoceramide products with uniform particle size and stable particle size is achieved, the process flow is simplified, production flexibility and efficiency are improved, and stability can be maintained under different storage conditions.
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Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of nanomaterials, and in particular relates to a water-dispersible ceramide product and a preparation method and a preparation system thereof. Background Art
[0002] Ceramide is a compound formed by sphingosine and fatty acids connected by amide bonds. It has multiple biological activities and is widely used in medical diagnosis and treatment and cosmetics. In the medical field, studies have found that it plays a certain therapeutic role in obesity prevention, cancer, and cardiovascular disease; in the cosmetic field, it has the effects of maintaining the skin barrier, moisturizing, anti-aging, and whitening. However, ceramide has stable properties, neat and orderly molecular arrangement, and extremely high crystallinity. Its poor solubility in water and easy crystallization have limited its wide application.
[0003] There are two common solutions: one is to dissolve ceramide in oil and then disperse the oil phase to prepare an oil-in-water emulsion system, and the other is to use liposomes to encapsulate ceramide. Among them, the use of liposomes to encapsulate ceramide has problems such as small active substance loading and uneven particle size; its preparation method is often thin film hydration method and high-pressure homogenization method. Thin film hydration method cannot achieve large-scale production and is only suitable for laboratory research and development; while thin film hydration method or high-pressure homogenization are intermittent operations, production is time-consuming and labor-intensive, and product production flexibility is low. Only fixed products can be produced at a time and cannot be temporarily adjusted.
[0004] Therefore, developing a water-dispersible nanoceramide with uniform particle size and stable system and determining a new process that is simple, continuous and adjustable at any time is of great significance to promote the widespread application of ceramide. Summary of the invention
[0005] The object of the present invention is to provide a water-dispersible ceramide product and a preparation method and system thereof to solve at least one of the above-mentioned problems.
[0006] According to one aspect of the present invention, a method for preparing a water-dispersible ceramide product is provided, comprising the following steps:
[0007] (1) Mix the raw materials for preparing the ceramide phase, heat to 60-90° C., stir at 100-1000 rpm, stir for 10-60 min, obtain the ceramide phase, and keep warm for later use;
[0008] (2) Mix the raw materials for preparing the aqueous phase, heat to 60-90° C., stir at 100-1000 rpm, stir for 10-60 min, obtain the aqueous phase, and keep warm for later use;
[0009] (3) preparing an additive phase according to production requirements, wherein the additive phase includes a first additive phase, a second additive phase, and a third additive phase;
[0010] (4) firstly placing the ceramide phase and the water phase into an ultrasonic nano-disperser for emulsification and dispersion, adding the third additional phase at the third node, and mixing the emulsified material with the third additional phase at the third node through a micro-mixing structure to obtain a product;
[0011] Alternatively, the first additional phase is added to the first node, mixed with the ceramide phase through a micro-mixing structure, and then emulsified and dispersed in an ultrasonic nano-dispersor with the water phase, and the third additional phase is added to the third node, and the emulsified material is mixed with the third additional phase through a micro-mixing structure at the third node to obtain a product;
[0012] Alternatively, the second additional phase is added at the second node, mixed with the water phase through a micro-mixing structure, and then enters the ultrasonic nano-disperser with the ceramide phase for emulsification and dispersion, and the third additional phase is added at the third node. The emulsified material is mixed with the third additional phase through a micro-mixing structure at the third node to obtain the product;
[0013] The first node is arranged between the outflow end of the ceramide phase and the ultrasonic nano-disperser, the second node is arranged between the outflow end of the water phase and the ultrasonic nano-disperser, and the third node is arranged on the discharge pipe.
[0014] Of course, according to actual production conditions, the first additional phase can be added at the first node, and mixed with the ceramide phase through a micro-mixing structure to obtain a first mixture; the second additional phase can be added at the second node, and mixed with the water phase through a micro-mixing structure to obtain a second mixture, the first mixture and the second mixture can be pumped into an ultrasonic nano-disperser for emulsification and dispersion, the third additional phase can be added at the third node, and the emulsified material can be mixed with the third additional phase at the third node through a micro-mixing structure to obtain a product.
[0015] The present invention develops a new continuous flow preparation process for water-dispersible nanoceramide based on ultrasonic microfluidic technology, and continuously produces water-dispersible nanoceramide through continuous flow; at the same time, an additive phase feeding node is set, and the additive phase is increased or decreased at any time according to production needs, and the production product is adjusted in real time. All pipelines are equipped with a temperature control system, which can be heated, kept warm or cooled according to the actual production process. The process can be applied to the continuous preparation of other materials, not limited to water-dispersible nanoceramide; and the process preparation process is simple, does not require high pressure, and is flexible in production, and the product can be adjusted at any time according to the production task.
[0016] In some embodiments, the flow rate ratio of the ceramide phase, the aqueous phase, and the additive phase is set according to the required content. Among them, the three are calculated according to the flow rate ratio: ceramide phase flow rate: aqueous phase flow rate: additive phase flow rate is (1 to 30): (1 to 30): (1 to 30). Specifically, the ceramide phase flow rate range can be 1-200 mL / min, the aqueous phase flow rate range can be 1-200 mL / min, and the additive phase flow rate range can be 1-200 mL / min. Of course, the flow rates of the three can also be adjusted according to the above ratio.
[0017] In some embodiments, the ultrasonic nanodisperser has a frequency of 19.5-100 KHz and a power setting of 1-1000W.
[0018] In some embodiments, each node is provided with a micro-mixing structure to ensure that the materials are mixed evenly after entering. The micro-mixing structure used includes but is not limited to the structures disclosed in patents 202222930543.6, 202110770263.0, and 202121541511.6 applied by the inventor team, as well as common mixing structures such as T-type, Y-type, and spiral types.
[0019] In some embodiments, the amount of preservative added at the third node in the preparation process is 10-60% of the total preservative phase mass.
[0020] In some embodiments, the ceramide phase includes, by mass fraction, 10-80% ceramide, 0-15% phospholipids, 0-10% sterols, and 0-80% oil; wherein ceramide is one or more of ceramide NP, ceramide AP, ceramide EOP, and ceramide NG; phospholipids include but are not limited to soybean lecithin, hydrogenated lecithin, egg yolk lecithin, etc., sterols include but are not limited to cholesterol, phytosterols, phytosterol esters, etc., and oils include but are not limited to peanut oil, coconut oil, soybean oil, caprylic / capric triglyceride, isononyl isononanoate, squalane, liquid paraffin, etc.
[0021] Among them, ceramide NP is ceramide 3, which can also be represented by N-stearoyl-phytosphingosine; ceramide AP is also called ceramide 6; ceramide EOP is ceramide 1 (Octad ecanoic acid, 27-[[(1S,2S,3R)-2,3-dihydroxy-1-(hydroxymethyl)heptadecyl]amino]-27-oxoheptacosyl ester), whose chemical formula is C 63 H 125 NO6, CAS is 179186-46-0; Ceramide NG is also known as ceramide 2.
[0022] In some embodiments, the aqueous phase includes, by mass fraction, 1-25% of a polyol, 0-10% of an emulsifier (emulsifier may not be added when preparing liposomes), and the remainder is deionized water; wherein the polyol includes but is not limited to glycerol, propylene glycol, 1,3-butylene glycol, 1,4-butylene glycol, and 1,2-pentanediol; the emulsifier includes but is not limited to glycerol stearate, sorbitan fatty acid esters, polyoxyethylene sorbitan fatty acid esters, cetearyl alcohol polyoxyethylene ether 20, hydrogenated castor oil polyoxyethylene ether, octyldodecanol, sodium oleate, sodium dodecyl sulfate, polyoxyethylene lauryl ether, and the like.
[0023] In some embodiments, the ingredients of the additive phase depend on the actual production situation, including but not limited to water-soluble or oil-soluble materials, oil, flavors, preservatives, thickeners, water, etc. Among them, the first additive phase includes at least one of oil-soluble materials and oil, the second additive phase includes at least one of water-soluble materials and water; the third additive phase includes at least one of flavors, preservatives, thickeners, water, and water-soluble materials, which play the role of preservatives and dilution systems. The preservatives used are commonly used preservatives, such as phenoxyethanol, methyl paraben and other preservatives.
[0024] In some embodiments, the oil includes, but is not limited to, peanut oil, coconut oil, soybean oil, caprylic / capric triglyceride, isononyl isononanoate, squalane, liquid paraffin, etc.;
[0025] According to a second aspect of the present invention, there is provided a system for preparing a water-dispersible ceramide product, comprising: a first raw material tank for preparing a ceramide phase, the first raw material tank being provided with a first pipeline connected thereto, the first pipeline being provided with a first node;
[0026] A second raw material tank for preparing the water phase, the second raw material tank is provided with a second pipeline connected thereto, the second pipeline is provided with a second node; the first pipeline is connected to the second pipeline to form a material mixing node, and the mixed material flows out from the third pipeline; and an ultrasonic nano-disperser, the first end of which is connected to the third pipeline to receive the mixed material, the second end is connected to the discharge pipe, and the discharge pipe is provided with a third node; the first node, the second node, and the third node are all provided with a micro-mixing structure to ensure uniform mixing of the materials. The first pipeline is connected to the second pipeline and the third pipeline through a tee.
[0027] According to a third aspect of the present invention, a water-dispersible ceramide product is provided. The ceramide product is prepared by mixing a ceramide phase, an aqueous phase and an additive phase, wherein the flow rate ratio of the three phases is: ceramide phase flow rate: aqueous phase flow rate: additive phase flow rate is (1 to 30): (1 to 30): (1 to 30). Specifically, the ceramide phase flow rate can be 1-200 mL / min, the aqueous phase flow rate can be 1-200 mL / min, and the additive phase flow rate can be 1-200 mL / min; its particle size is 50-200 nm, and after being stored at 4° C., 25° C., and 40° C. for 155 days, its particle size remains at 50-200 nm.
[0028] The water-dispersible ceramide product of the present invention, through formula optimization, uses molecular blending to inhibit the crystallization of ceramide molecules, adds a compound emulsifier to molecules with similar properties to ceramide molecules, such as soybean lecithin and cholesterol, to reduce interfacial energy, optimizes the addition ratio, and improves system stability. Among them, the emulsifier plays the role of a surfactant. BRIEF DESCRIPTION OF THE DRAWINGS
[0029] Figure 1 Schematic diagram of the preparation system, where 1, 2, and 3 represent the first node, the second node, and the third node, respectively.
[0030] Figure 2 This is the microscopic morphology of ceramide nanoemulsion.
[0031] Figure 3 This is the particle size distribution diagram of ceramide nanoemulsion. DETAILED DESCRIPTION
[0032] The present invention will be further described in detail below in conjunction with specific embodiments. Unless otherwise specified, the following raw materials are commercially available.
[0033] Schematic diagram of the preparation system of water-dispersible ceramide products Figure 1 As shown, the direction of the arrow indicates the direction of material flow, and the preparation system consists of the following structure:
[0034] A first raw material tank for preparing a ceramide phase, wherein the first raw material tank is provided with a first pipeline connected thereto, the first pipeline is provided with a first node, and a micro-mixing structure is provided at the first node;
[0035] A second raw material tank for preparing an aqueous phase, the second raw material tank is provided with a second pipeline connected thereto, the second pipeline is provided with a second node, and a micro-mixing structure is provided at the second node; the first pipeline is connected to the second pipeline and a material mixing node is formed at the connection point, and the mixed material flows out from the third pipeline; the first pipeline is connected to the second pipeline and the third pipeline through a tee.
[0036] It also includes an ultrasonic nano-disperser, whose first end is connected to the third pipeline for receiving the material flowing out of the third pipeline after mixing, and the second end is connected to the discharge pipe, on which a third node is provided, and the product flowing out of the discharge pipe is the finished product.
[0037] Among them, the first node, the second node and the third node are all provided with micro-mixing structures to ensure uniform mixing of the materials; the first node adds oil-soluble materials or oil, the second node adds water-soluble materials, and the third node adds preservatives or water-soluble materials.
[0038] The following examples are based on Figure 1 The preparation system shown is completed.
[0039] Example 1
[0040] A method for preparing water-dispersible ceramide, the specific steps are as follows:
[0041] 1. Raw material preparation
[0042] Ceramide phase: add the formulated amount of ceramide, phospholipids, sterols and oil into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for use; wherein the mass percentage of each component is ceramide NP 42%, soybean lecithin 14%, cholesterol 2% and soybean oil 42%.
[0043] Aqueous phase: Add the formulated amount of water, glycerol and polyoxyethylene sorbitan fatty acid ester into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for later use; wherein the components by mass percentage are 90% deionized water, 5% glycerol and 5% polyoxyethylene sorbitan fatty acid ester.
[0044] The added phase is only the preservative phase: add the formulated amount of water and phenoxyethanol into the raw material tank, stir at a speed of 300 rpm, stir for 20 minutes, and set aside; wherein the mass percentage of each component is 90% of deionized water and 10% of phenoxyethanol.
[0045] 2. Process parameter setting
[0046] The flow rates of each phase were determined according to the ceramide content required by the formula, specifically: ceramide phase flow rate 3 mL / min, water phase flow rate 24 mL / min, and additive phase flow rate 3 mL / min.
[0047] The frequency of the ultrasonic nano-disperser is 19.9KHz and the power is set to 100W.
[0048] 3. Product production
[0049] Production process such as Figure 1As shown, the water phase is opened first, and when the water phase flows out from the outlet of the ultrasonic nano-disperser, the ultrasonic nano-disperser is turned on; then the ceramide phase is opened, and when the emulsion flows out from the outlet of the ultrasonic nano-disperser, the preservative phase is opened, and the preservative phase is added from the third node. Finally, the expected product, i.e., ceramide nano-emulsion, is obtained at the discharge port. The transmission electron microscope and dynamic light scattering measurement particle size distribution results are shown in the attached Figure 2-3 , average particle size 87nm.
[0050] The storage stability of the ceramide nanoemulsion prepared in Example 1 under different storage conditions was tested. The experimental results are shown in Table 1.
[0051] Table 1 Experimental results of stability of ceramide nanoemulsion prepared in Example 1
[0052]
[0053] Example 2 (composite ceramide, composite surfactant)
[0054] A method for preparing water-dispersible ceramide, the specific steps are as follows:
[0055] 1. Raw material preparation
[0056] Ceramide phase: Add the formulated amount of ceramide, phospholipids, sterols and oil into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for use. Among them, the components by mass percentage are ceramide 42% (including ceramide NP 37%, ceramide AP 3.5%, salicyloyl phytosphingosine 3.5%), soybean lecithin 14%, cholesterol 2%, and soybean oil 42%.
[0057] Water phase: Add the formulated amount of water, polyol and emulsifier into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for later use. The components by mass percentage are 90% deionized water, 5% glycerol, 4.5% polyoxyethylene sorbitan fatty acid ester, and 0.5% sorbitan fatty acid ester.
[0058] The only added phase is the preservative phase: add the water and preservative in the formula amount into the raw material tank, stir at a speed of 300 rpm, stir for 20 minutes, and set aside. Among them, the components are 90% deionized water and 10% phenoxyethanol by mass percentage.
[0059] 2. Process parameter setting
[0060] Determine the flow rate of each phase according to the ceramide content required by the formula.
[0061] The flow rate of the ceramide phase was 3 mL / min; the flow rate of the water phase was 24 mL / min; and the flow rate of the preservative phase was 3 mL / min.
[0062] Ultrasonic nanodisperser frequency 19.9KHz, power setting 100W
[0063] 3. Product production
[0064] First open the water phase, and when the water phase flows out from the outlet of the ultrasonic nano-disperser, start the ultrasonic nano-disperser; open the ceramide phase, and then open the preservative phase when waiting for the emulsion to flow out from the outlet of the ultrasonic nano-disperser. The preservative phase is added from the third node, and finally the expected product, i.e., ceramide nano-emulsion, is obtained at the discharge port with an average particle size of 110 nm.
[0065] The storage stability of the ceramide nanoemulsion prepared in Example 2 under different storage conditions was tested. The experimental results are shown in Table 2.
[0066] It can be seen from the stability test results in Table 1 and Table 2 that the water-dispersible ceramide product obtained by the preparation method of the present invention has a particle size of 50-200 nm after being stored at 4° C., 25° C., and 40° C. for 155 days, and has good stability.
[0067] Table 2 Experimental results of stability of ceramide nanoemulsion prepared in Example 2
[0068]
[0069] Example 3 (addition phase addition, taking oil-soluble substances as an example)
[0070] A method for preparing water-dispersible ceramide, the specific steps are as follows:
[0071] 1. Raw material preparation
[0072] Ceramide phase: Add the formulated amount of ceramide, phospholipids, sterols and oil into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for use. Among them, the components by mass percentage are ceramide 42% (including ceramide NP 37%, ceramide AP 3.5%, salicyloyl phytosphingosine 3.5%), soybean lecithin 14%, cholesterol 2%, and soybean oil 42%.
[0073] Water phase: Add the formulated amount of water, polyol and emulsifier into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for later use. The components by mass percentage are 90% deionized water, 5% glycerol, and 5% polyoxyethylene sorbitan fatty acid ester.
[0074] Add phase two:
[0075] Preservative phase: Add the formulated amount of water and preservative into the raw material tank, stir at 300 rpm, stir for 20 minutes, and set aside. The components are deionized water 90% and phenoxyethanol 10% by mass percentage.
[0076] Squalane phase: Add the formula amount of squalane and caprylic / capric triglyceride into the raw material tank, heat to 60°C, stir at 300rpm, stir for 20min, and keep warm for later use. The mass percentage of each component is 20% squalane and 80% caprylic / capric triglyceride. (Note: Squalane is a liquid oily substance and can be fed alone. In this case, other oils were added for the purpose of example.)
[0077] 2. Process parameter setting
[0078] Determine the flow rate of each phase according to the ceramide content required by the formula.
[0079] The flow rate of the ceramide phase was 3 mL / min; the flow rate of the water phase was 21 mL / min; the flow rate of the squalane phase was 3 mL / min; and the flow rate of the preservative phase was 3 mL / min.
[0080] The frequency of the ultrasonic nano-disperser is 19.9KHz and the power is set to 100W.
[0081] 3. Product production
[0082] First, the water phase was opened, and when the water phase flowed out from the outlet of the ultrasonic nano-disperser, the ultrasonic nano-disperser was turned on; then the ceramide phase was opened, and the squalane phase was added to the ceramide phase from the first node. Then, when the emulsion flowed out from the outlet of the ultrasonic nano-disperser, the preservative phase was opened, and the preservative phase was added from the third node, and finally the expected product, i.e., ceramide nano-emulsion, was obtained at the outlet, and the average particle size of the product was 144nm.
[0083] Example 4 (addition of oil-soluble vitamin E)
[0084] A method for preparing water-dispersible ceramide, the specific steps are as follows:
[0085] 1. Raw material preparation
[0086] Prepare ceramide phase: add the formulated amount of ceramide, phospholipids, sterols and oil into the raw material tank, heat to 60°C, stir at 500rpm, stir for 20min, and keep warm for use. Among them, the components by mass percentage are ceramide NP 20%, soybean lecithin 39%, cholesterol 2%, and caprylic acid glyceride 39%.
[0087] Prepare the water phase: add the formulated amount of water, polyol and emulsifier into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for later use. The components by mass percentage are 90% deionized water, 5% glycerol, and 5% polyoxyethylene sorbitan fatty acid ester.
[0088] The added phase is 2 phases:
[0089] Preservative phase: Add the formulated amount of water and preservative into the raw material tank, stir at 300 rpm, stir for 20 minutes, and set aside. The components are 90% deionized water and 10% phenoxyethanol by mass percentage.
[0090] Vitamin E phase: Add the formulated amount of vitamin E and caprylic glyceryl caprylate into the raw material tank, heat to 60°C, stir at 300 rpm, stir for 30 minutes, and keep warm for later use. The mass percentage of each component is 1% vitamin E and 99% caprylic glyceryl caprylate.
[0091] 2. The process parameters are set according to the ceramide content required by the formula and the flow rate of each phase is determined.
[0092] The flow rate of the ceramide phase was 3 mL / min; the flow rate of the water phase was 21 mL / min; the flow rate of the vitamin E phase was 3 mL / min; and the flow rate of the preservative phase was 3 mL / min.
[0093] The frequency of the ultrasonic nano-disperser is 19.9KHz and the power is set to 100W.
[0094] 3. Product production
[0095] First, open the water phase, and when the water phase flows out from the outlet of the ultrasonic nano-disperser, start the ultrasonic nano-disperser; then open the ceramide phase and the vitamin E phase to enter the nano-disperser after the mixing is completed in the rear section of the first node. Then, when the emulsion flows out from the outlet of the ultrasonic nano-disperser, open the preservative phase, and add the preservative phase from the third node. Finally, the ceramide product with added vitamin E is obtained at the discharge port, and the average particle size of the product is 130nm.
[0096] Example 5 (addition of water-soluble vitamin C)
[0097] A method for preparing water-dispersible ceramide, the specific steps are as follows:
[0098] 1. Raw material preparation
[0099] Prepare ceramide phase: add the formulated amount of ceramide, phospholipids, sterols and oil into the raw material tank, heat to 60°C, stir at 500rpm, stir for 20min, and keep warm for use. Among them, the components by mass percentage are ceramide NP 20%, soybean lecithin 39%, cholesterol 2%, and caprylic acid glyceride 39%.
[0100] Prepare the water phase: add the formulated amount of water, polyol and emulsifier into the raw material tank, heat to 60°C, stir at 300rpm, stir for 30min, and keep warm for later use. The components by mass percentage are 90% deionized water, 5% glycerol, and 5% polyoxyethylene sorbitan fatty acid ester.
[0101] The added phase is two phases:
[0102] Preservative phase: Add the formulated amount of water and preservative into the raw material tank, stir at 300 rpm, stir for 20 minutes, and set aside. The components are deionized water 90% and phenoxyethanol 10% by mass percentage.
[0103] Vitamin C phase: Add the formulated amount of vitamin C, polyol, emulsifier and deionized water into the raw material tank, stir at 300 rpm, stir for 30 minutes, and set aside. The components by mass percentage are vitamin C 1%, glycerol 5%, polyoxyethylene sorbitan fatty acid ester 5%, and deionized water 89%.
[0104] 2. The process parameters are set according to the ceramide content required by the formula and the flow rate of each phase is determined.
[0105] The flow rate of the ceramide phase is 3 mL / min; the flow rate of the water phase is 21 mL / min; the flow rate of the vitamin C phase is 3 mL / min; and the flow rate of the preservative phase is 3 mL / min.
[0106] The frequency of the ultrasonic nano-disperser is 19.9KHz and the power is set to 100W.
[0107] 3. Product production
[0108] First, the water phase and the vitamin C phase are opened, and the vitamin C phase is added from the second node. When the water phase flows out from the outlet of the ultrasonic nano-disperser, the ultrasonic nano-disperser is turned on; then the ceramide phase is opened. Then, when the emulsion flows out from the outlet of the ultrasonic nano-disperser, the preservative phase is opened, and the preservative phase is added from the third node. Finally, the ceramide product with added vitamin C is obtained at the outlet, and the average particle size of the product is 305nm.
[0109] Example 6 (Product conversion production diagram)
[0110] 1. Raw material preparation
[0111] Ceramide phase: Add the formulated amount of ceramide and steroids into the raw material tank, heat to 60°C, stir at 300 rpm, stir for 30 minutes, and keep warm for later use.
[0112] Oil phase: Add the formulated amount of oil into the raw material tank, heat to 60°C, stir at 300 rpm, stir for 30 minutes, and keep warm for later use.
[0113] Water phase: Add the formulated amount of water, polyol and emulsifier into the raw material tank, heat to 60°C, stir at 300 rpm, stir for 30 minutes, and keep warm for later use.
[0114] Add Phase 2:
[0115] Lecithin phase: Add the formulated amount of lecithin into the raw material tank, heat to 60°C, stir at 300 rpm, stir for 30 min, and keep warm for later use.
[0116] Preservative phase: Add the formulated amount of water and preservative into the raw material tank, stir at 300 rpm, stir for 20 minutes, and set aside.
[0117] 2. Process parameter setting
[0118] Determine the flow rate of each phase according to the ceramide content required by the formula.
[0119] 3. Product conversion production
[0120] Ceramide nanoemulsion: open the ceramide phase, water phase, oil phase, and preservative phase. Add the oil phase to the ceramide phase from the first node, and the preservative phase to the emulsion from the third node.
[0121] Switch to produce ceramide liposomes: turn off the oil phase and add the phospholipid phase from the first node, then the nanoemulsion will be changed to produce liposomes.
[0122] Then switch to produce ceramide suspension: close the phospholipid phase, and only open the ceramide phase, water phase, and preservative phase. Add the preservative phase to the emulsion from the third node, and the product will be ceramide nanosuspension.
[0123] The above are only some embodiments of the present invention. For those skilled in the art, several modifications and improvements can be made without departing from the creative concept of the present invention, which all belong to the protection scope of the present invention.
Claims
1. A method for preparing a water-dispersible ceramide product, characterized in that: The steps include: (1) mixing the raw materials for preparing the ceramide phase, heating at 60-90° C., and stirring at a speed of 100-1000 rpm for 10-60 min to obtain the ceramide phase; (2) mixing the raw materials for preparing the aqueous phase, heating at 60-90° C., and stirring at a speed of 100-1000 rpm for 10-60 min to obtain an aqueous phase; (3) preparing an additive phase, wherein the additive phase includes a first additive phase, a second additive phase, and a third additive phase; (4) firstly placing the ceramide phase and the water phase into an ultrasonic nano-disperser for emulsification and dispersion, adding the third additional phase at the third node, and mixing the emulsified material with the third additional phase at the third node through a micro-mixing structure to obtain a product; Alternatively, the first additional phase is added to the first node, mixed with the ceramide phase through a micro-mixing structure, and then emulsified and dispersed in an ultrasonic nano-dispersor with the water phase, and the third additional phase is added to the third node, and the emulsified material is mixed with the third additional phase through a micro-mixing structure at the third node to obtain a product; Alternatively, the second additional phase is added at the second node, mixed with the water phase through a micro-mixing structure, and then enters the ultrasonic nano-disperser with the ceramide phase for emulsification and dispersion, and the third additional phase is added at the third node. The emulsified material is mixed with the third additional phase through a micro-mixing structure at the third node to obtain the product; The first node is arranged between the outflow end of the ceramide phase and the ultrasonic nano-disperser, the second node is arranged between the outflow end of the water phase and the ultrasonic nano-disperser, and the third node is arranged on the discharge pipe.
2. The preparation method according to claim 1, characterized in that: The frequency of the ultrasonic nano-disperser is 19.5-100 KHz, and the power setting is 1-1000W.
3. The preparation method according to claim 1 or 2, characterized in that: The first node, the second node and the third node are all provided with micro-hybrid structures.
4. The preparation method according to claim 3, characterized in that: The volume contents of the ceramide phase, water phase and additive phase are calculated according to the flow rate ratio: ceramide phase flow rate: water phase flow rate: additive phase flow rate is (1-30): (1-30): (1-30).
5. The preparation method according to claim 4, characterized in that: The ceramide phase comprises, by mass fraction, 10-80% ceramide, 0-15% phospholipids, 0-10% sterols, and 0-80% oil.
6. The preparation method according to claim 4 or 5, characterized in that: The water phase comprises, by mass fraction, 1-25% of polyol, 0-10% of emulsifier, and the remainder is deionized water.
7. The preparation method according to claim 4 or 5, characterized in that: The first added phase includes at least one of oil-soluble materials and oil, the second added phase includes at least one of water-soluble materials and water, and the third added phase includes at least one of flavors, preservatives, thickeners, water, and water-soluble materials.
8. The preparation method according to claim 7, characterized in that: The oil comprises at least one of peanut oil, coconut oil, soybean oil, caprylic / capric triglyceride, isononyl isononanoate, squalane and liquid paraffin.
9. A preparation system for implementing any one of the preparation methods described in 1-8, characterized in that: include: A first raw material tank, wherein the first raw material tank is provided with a first pipeline connected thereto, and the first pipeline is provided with a first node; a second raw material tank, wherein the second raw material tank is provided with a second pipeline connected thereto, and the second pipeline is provided with a second node; the first pipeline is connected to the second pipeline and a material mixing node is formed at the connection point, and the mixed material flows out from a third pipeline; and The ultrasonic nano-disperser has a first end connected to the third pipeline and a second end connected to a discharge pipe, on which a third node is arranged; the first node, the second node and the third node are all provided with a micro-mixing structure.
10. The water-dispersible ceramide product obtained by the preparation method according to claims 1-8, characterized in that: The particle size of the water-dispersible ceramide product is 50-200 nm; and after being stored at 4° C., 25° C., and 40° C. for 155 days, the particle size remains at 50-200 nm.
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