阅读说明：本技术 一种类胡萝卜素的制备方法 (Method for preparing carotenoid ) 是由 於春峰 李宏龙 章文晋 文雁君 李林正 夏慧亭 张亚琼 郭玉莲 于 2021-08-02 设计创作，主要内容包括：本申请提供了一种类胡萝卜素的制备方法,属于类胡萝卜素加工技术领域。具体步骤包括：以类胡萝卜素和/或稀释剂和/或分散剂和/或填充剂,经真空充惰性气体正压乳化搅拌调配、自动控制超高温瞬时熔溶、惰性气体正压保护直接输送乳化剪切面、真空乳化、急速冷却和/或喷雾干燥,制备得到类胡萝卜素乳液或粉末产品。通过优化类胡萝卜素制备的工艺流程和各项限定条件,可以有效降低类胡萝卜素损失率,提高类胡萝卜素稳定性和生物利用度；使用本发明制备出的类胡萝卜素具有粒径小、全反式成分高、损失率低的优点。(The application provides a preparation method of carotenoid, belonging to the technical field of carotenoid processing. The method comprises the following specific steps: the carotenoid emulsion or powder product is prepared by filling carotenoid and/or diluent and/or dispersant and/or filler in vacuum into inert gas under positive pressure, emulsifying, stirring and blending, automatically controlling ultrahigh temperature instant melting, directly conveying an emulsifying shear surface under the protection of the positive pressure of the inert gas, emulsifying in vacuum, rapidly cooling and/or spray drying. By optimizing the technological process and various limiting conditions for preparing the carotenoid, the carotenoid loss rate can be effectively reduced, and the stability and bioavailability of the carotenoid are improved; the carotenoid prepared by the method has the advantages of small particle size, high all-trans component content and low loss rate.)

1. A process for producing a carotenoid,

the carotenoid emulsion or powder product is prepared by filling carotenoid and/or diluent and/or dispersant and/or filler in vacuum into inert gas under positive pressure, emulsifying, stirring and blending, automatically controlling ultrahigh temperature instant melting, directly conveying an emulsifying shearing surface under the protection of the positive pressure of the inert gas, emulsifying in vacuum, rapidly cooling and/or spray drying.

2. The method according to claim 1, comprising the steps of:

s1 preparation of carotenoid oil phase: adding carotenoid and/or diluent into a vacuum inert gas-filled positive pressure emulsification stirring mixing tank, stirring at a constant speed of 0-50 HZ for 0-60 min anticlockwise under a vacuum condition, then shearing at 0-50 HZ for 0-60 min clockwise, emulsifying and dispersing into a uniform oil phase solution, then pressurizing and filling inert gas, and replacing a vacuum state to enable the oil phase solution to be in an inert gas positive pressure protection state;

s2 preparation of aqueous phase solution: the dispersant and/or filler is added to the emulsification tank at a temperature: 20-90 ℃, vacuum degree: under the condition of-0.005 to-0.1 Mpa, firstly stirring at a constant speed of 0-50 HZ for 0-60 min anticlockwise, and then emulsifying at a constant speed of 0-50 HZ for 0-60 min clockwise until the solution is completely dissolved, wherein the aqueous phase solution is transparent and free of bubbles and floating foam;

s3 automatic control oxygen-free ultrahigh temperature instant melting: introducing the oil phase solution obtained in the step S1 into an ultrahigh-temperature heating pipe, automatically detecting the material temperature on line, and automatically switching a blanking emulsification mode if the material reaches the melting temperature; if the material temperature does not reach the material melting temperature, automatically starting a circulation mode for the material, and repeating the heating temperature and the heating time of the ultrahigh-temperature heating pipe until the material temperature reaches the melting material temperature;

s4 emulsification: conveying the material reaching the melting temperature to a position below the liquid level of the water phase through a feeding pipe, emulsifying and stirring for 5-60 min at 0-50 HZ by using a shearing head in an emulsifying tank until the material feeding is finished, and enabling the feeding pipe and the tank wall to be free of any floating oil to be hung on the wall to obtain the carotenoid emulsion;

s5 rapid cooling: cooling the carotenoid emulsion to below 30 ℃ through a cooling pipe, conveying the carotenoid emulsion to an aseptic storage tank, and carrying out aseptic filling to obtain the carotenoid emulsion.

3. The method of claim 2, further comprising a spray drying step after the rapid cooling:

spray drying the carotenoid emulsion to obtain carotenoid powder.

4. The method according to claim 2, wherein in S1, the carotenoid is selected from one or more of carotenes, β -apo-8' -carotenal, lutein esters, zeaxanthin, capsanthin, capsorubin, capsicum oleoresin, lycopene, bixin, canthaxanthin, astaxanthin obtained in any manner; the diluent is selected from one or more of oil and fat, emulsifier, antioxidant, antiseptic, stabilizer, acid, water retention agent, protective colloid, perfume, filler, and pH buffer.

5. The method according to claim 4,

the oil is selected from one or more of safflower oil, medium-chain triacylglycerol, corn oil, olive oil, sunflower seed oil, peanut oil and soybean oil;

the emulsifier is selected from one or more of water, tween, polyglycerol fatty acid ester, sucrose fatty acid ester, propylene glycol, glycerol, maltitol, sorbitol, glucose syrup, erythritol, xylitol, maltitol, sorbitol, glucose, white granulated sugar, trehalose, maltodextrin, xanthan gum, pectin, Arabic gum, cellulose, carboxymethyl cellulose, dietary fiber, microcrystalline cellulose, carboxymethyl cellulose, starch, cyclodextrin, starch and modified starch;

the antioxidant is selected from polyphenols and derivatives/extracts thereof: rosemary extract, carnosol, tocopherol;

and/or flavonoids and their derivatives/extracts: tea polyphenols, and folium Bambusae extract;

and/or esters, salts with antioxidant properties: lecithin, ascorbyl palmitate, ascorbic acid and one or more of salts thereof.

6. The method according to claim 2, wherein in S1, the vacuum conditions are: the stirring temperature is 0-45 ℃, and the vacuum degree is-0.005-0.1 Mpa; after the inert gas is pressurized and filled, the pressure in the tank is 0.005-5.0 Mpa.

7. The preparation method of claim 2, wherein in the step S3, the oil phase solution is fed into the ultra-high temperature heating pipe at a flow rate of 0 to 50HZ by using a screw pump; the heating temperature is as follows: and (3) heating at 0-300 ℃ for: < 5s, the heating time is defined as: the time required for the oil phase solution to flow into the heating pipe from the beginning to flow out of the heating pipe completely; the temperature of the molten material is 20-250 ℃.

8. The method according to claim 2, wherein in S5, the cooling temperature is: -50 ℃ to 0 ℃, cooling time: less than 5 s; the cooling time is defined as: the time required for the carotenoid emulsion to flow from the initial flow into the cooling tube to the full flow out of the cooling tube.

9. The use of the preparation method according to claim 2, wherein the prepared product can be widely used in the fields of food, health products, cosmetics, feed and pharmaceuticals.

Technical Field

The invention belongs to the technical field of carotenoid processing, and particularly relates to a preparation method and a process flow of carotenoid.

Background

The carotenoid product is a mature product applied to the existing food, medicine, health care products and cosmetics. The carotenoid not only has coloring effect, but also has antioxidant and nutritional effects, and some carotenoids have more medical and health-care effects.

Carotenoids are widely found in nature in terms of their origin and can be extracted from natural plants, obtained by microbial fermentation or by chemical synthesis. In terms of physicochemical properties, carotenoids are insoluble in water, have low solubility in oil, are very sensitive to light, heat and oxygen, and are not suitable for direct application. In the processing process of food, medicine and the like, the carotenoid is prepared into emulsion or powder products by using an emulsification embedding technology, so that the subsequent production and use are facilitated.

At present, the preparation of the carotenoid oil phase by chemical synthesis mostly adopts: and (3) preparing the oil phase by heating and dissolving the oil-soluble crystals at high temperature for a long time or dissolving the oil-soluble crystals in an organic solvent or assisting in dissolving the oil-soluble crystals and the like. For example, the preparation method of a beta carotene emulsion with publication No. CN109105723A and the preparation method of a beta carotene with publication No. CN108148444A for coloring with high content adopt high-temperature long-time hot melting. The preparation method can cause large loss of carotenoid components on one hand, and the carotenoid is easy to isomerize on the other hand. For example, the preparation method of the water-soluble carotenoid of the publication No. CN101297691A, the preparation method of the water-soluble nano-particles with high beta-carotene content of the publication No. CN101143132A, the preparation method of the finely dispersed carotenoid of the high all-trans form of the publication No. CN104146988A and the preparation method of the finely dispersed carotenoid of the high all-trans form of the publication No. CN101549273A adopt organic solvents to dissolve or assist in dissolving the carotenoid, which easily causes solvent residue and has great influence on the safety of products.

At present, carotenoid emulsification embedding is mostly adopted: the carotenoid oil phase is added directly to the normal pressure emulsified aqueous phase. However, this solution has two drawbacks: firstly, preparing a water phase at normal pressure, easily forming a water-gas two-phase miscible system, not facilitating the tight combination of the carotenoid and the water phase, and simultaneously pushing the carotenoid to aggregate to form large particles or floating demulsification and other unstable factors by floating or breaking of bubbles in the water phase; in addition, the oil has the phenomena of agglomeration, floating surface, tank wall adhesion and the like due to factors such as surface tension, temperature drop and the like, the oil phase is brought to the operation surface of the emulsifying machine by the water phase kinetic energy to carry out high-speed shearing dispersion, the oil phase is easily aggregated to form large particles due to the temperature difference and the relatively long time for bringing the oil phase to the operation surface, and the stability and the embedding rate of the carotenoid are greatly influenced.

At present, emulsion or dry liquid after carotenoid emulsification and embedding preparations is mostly adopted: the emulsion is cooled by natural cooling, interlayer cooling, exchanger cooling and other modes, the relative cooling time is long, the molecular kinetic energy in the emulsion is large, and the oil phase is easy to gather to form large particles, so that the stability of the product is not facilitated.

Therefore, aiming at the defects of the prior art, the invention adopts the combination of five process equipment of low-temperature vacuum inert gas filling positive pressure emulsification stirring batching, automatic control of oxygen-free ultrahigh temperature instant melting and dissolving, direct conveying of an emulsification shear surface material pipe by carotenoid oil liquid, vacuum state emulsification and rapid cooling for the first timeA method for preparing carotene. 1. The carotenoid loss rate is reduced by 10-20%; 2. the degradation rate of trans-carotenoid content is less than 10 percent; 3. carotenoid particle size D₉₀Less than 500nm, embedding rate higher than 95% and high biological utilization rate. The comprehensive cost is reduced, the product quality and the safety are improved, and the enterprise benefit is improved. Also overcomes the disadvantages of the conventional carotenoid products: high loss rate in the processing process, serious degradation of trans-form content, high solvent residue of products and the like.

Disclosure of Invention

The invention aims to provide a preparation method of carotenoid, which reduces the carotenoid loss rate and improves the carotenoid stability and bioavailability by optimizing the technological process and limiting conditions of carotenoid preparation.

In order to achieve the above objects, the present invention provides a method for preparing carotenoid,

the carotenoid emulsion or powder product is prepared by filling carotenoid and/or diluent and/or dispersant and/or filler in vacuum into inert gas under positive pressure, emulsifying, stirring and blending, automatically controlling ultrahigh temperature instant melting, directly conveying an emulsifying shear surface under the protection of the positive pressure of the inert gas, emulsifying in vacuum, rapidly cooling and/or spray drying.

Wherein, the oil phase liquid of the carotenoid can be dissolved or dispersed into fine particles and uniformly dissolved by filling inert gas into the mixture under vacuum at low temperature and positive pressure for emulsification and stirring, thereby reducing the particle size of the carotenoid, reducing the loss and preventing isomerization;

the oxygen-free ultrahigh temperature instant melting step is automatically controlled, so that the carotenoid can instantly reach a molten state, the particle size of the carotenoid is further reduced, the loss is reduced, and the isomerization is prevented;

directly conveying an emulsifying shear surface to enable the carotenoid to be instantly emulsified and dispersed, and uniformly combining an oil phase and a water phase to form a nano emulsion so as to improve the stability of an emulsified material;

in the vacuum state emulsification step, on one hand, the water phase is completely prepared and dissolved, is in a transparent bubble-free and froth-free state, and avoids a water-gas mixed two-phase system, on the other hand, the oil phase is directly emulsified with the water phase, and the oil phase is tightly wrapped by the water phase, so that a water-oil-gas three-phase emulsification system is avoided, the formed nano-emulsion material is increased in collision due to bubble breakage or floating, and the stability of the emulsion material is improved;

and a rapid cooling step, namely rapidly cooling the nano emulsified material, reducing the molecular kinetic energy of the emulsified material, enabling the emulsified material to be more stable, avoiding the increase of the particle size of the carotenoid, reducing the long-term high-temperature loss and preventing isomerization.

The preparation method specifically comprises the following steps:

s1 preparation of carotenoid oil phase: adding carotenoid and/or diluent into a low-temperature vacuum inert gas-filled positive-pressure emulsification stirring batching tank, stirring at a constant speed of 0-50 HZ for 0-60 min anticlockwise under a vacuum condition, then shearing at a clockwise direction of 0-50 HZ for 0-60 min, emulsifying and dispersing into a uniform oil phase solution, then pressurizing and filling inert gas, and replacing a vacuum state to enable the oil phase solution to be in an inert gas positive-pressure protection state;

s2 preparation of aqueous phase solution: the dispersant and/or filler is added to the emulsification tank at a temperature: 20-90 ℃, vacuum degree: under the condition of-0.005 to-0.1 Mpa, firstly stirring at a constant speed of 0-50 HZ for 0-60 min anticlockwise, and then emulsifying at a constant speed of 0-50 HZ for 0-60 min clockwise until the solution is completely dissolved, wherein the aqueous phase solution is transparent and free of bubbles and floating foam;

s3 automatic control oxygen-free ultrahigh temperature instant melting: introducing the oil phase solution obtained in the step S1 into an ultrahigh-temperature heating pipe, automatically detecting the material temperature on line, and automatically switching a blanking emulsification mode if the material reaches the melting temperature; if the material temperature does not reach the material melting temperature, automatically starting a circulation mode for the material, and repeating the heating temperature and the heating time of the ultrahigh-temperature heating pipe until the material temperature reaches the melting material temperature;

s4 emulsification: conveying the material reaching the melting temperature to a position below the liquid level of the water phase through a feeding pipe, emulsifying and stirring for 5-60 min at 0-50 HZ by using a shearing head in an emulsifying tank until the material feeding is finished, and enabling the feeding pipe and the tank wall to be free of any floating oil to be hung on the wall to obtain the carotenoid emulsion;

s5 rapid cooling: cooling the carotenoid emulsion to below 30 ℃ through a cooling pipe, conveying the carotenoid emulsion to an aseptic storage tank, and carrying out aseptic filling to obtain the carotenoid emulsion.

In a preferred embodiment, the spray drying step is further included after the rapid cooling step:

spray drying the carotenoid emulsion to obtain carotenoid powder.

In a preferred embodiment, in S1, the carotenoid is selected from one or more of carotene, β -apo-8' -carotenal, lutein ester, zeaxanthin, capsanthin, capsorubin, capsicol, lycopene, bixin, canthaxanthin, astaxanthin obtained in any manner; the diluent is selected from one or more of oil and fat, emulsifier, antioxidant, antiseptic, stabilizer, acid, water retention agent, protective colloid, perfume, filler, and pH buffer.

In a preferred embodiment, the oil is selected from one or more of safflower seed oil, medium-chain triacylglycerol, corn oil, olive oil, sunflower seed oil, peanut oil, soybean oil;

the emulsifier is selected from one or more of water, tween, polyglycerol fatty acid ester, sucrose fatty acid ester, propylene glycol, glycerol, maltitol, sorbitol, glucose syrup, erythritol, xylitol, maltitol, sorbitol, glucose, white granulated sugar, trehalose, maltodextrin, xanthan gum, pectin, Arabic gum, cellulose, carboxymethyl cellulose, dietary fiber, microcrystalline cellulose, carboxymethyl cellulose, starch, cyclodextrin, starch and modified starch;

the antioxidant is selected from polyphenols and derivatives/extracts thereof: rosemary extract, carnosol, tocopherol;

and/or flavonoids and their derivatives/extracts: tea polyphenols, and folium Bambusae extract;

and/or esters, salts with antioxidant properties: lecithin, ascorbyl palmitate, ascorbic acid and one or more of salts thereof.

In a preferred embodiment, in S1, the vacuum condition is: the stirring temperature is 0-45 ℃, and the vacuum degree is-0.005-0.1 Mpa; after the inert gas is pressurized and filled, the pressure in the tank is 0.005-5.0 Mpa, and the inert gas is preferably selected from nitrogen, argon and the like;

preferably, the vacuum conditions are: stirring at 15-40 ℃ and the vacuum degree of-0.1 Mpa, uniformly stirring at 10-30 HZ counterclockwise for 15-50 min, shearing at 15-48 HZ clockwise for 15-50 min, and emulsifying and dispersing to obtain a uniform oil phase solution.

In a preferred embodiment, in S2, the dissolving conditions of the dispersant and/or the filler are as follows: stirring at the temperature of 20-90 ℃ and the vacuum degree of-0.1 Mpa, stirring anticlockwise at 5-30 HZ for 10-30 min at a constant speed, emulsifying clockwise at 10-40 HZ for 10-30 min, and dissolving completely, wherein the aqueous phase solution is transparent and free of bubbles and floating foam;

in a preferred embodiment, in the step S3, the oil-phase solution is fed into the ultrahigh-temperature heating pipe by using a screw pump at a flow rate of 0 to 50HZ, preferably at a flow rate of 15 to 45 HZ;

the heating temperature is as follows: and (3) heating at 0-300 ℃ for: < 5s, the heating time is defined as: the time required for the oil phase solution to flow from the initial into the heating tube to the full flow out of the heating tube, preferably, the heating temperature: heating at 100-260 ℃ for: 2-4 s;

the temperature of the molten material is 20-250 ℃, and preferably, the temperature of the molten material is 50-190 ℃.

In a preferred embodiment, in S4, the at least one carotenoid oil phase liquid passes through a feeding pipe, and the feeding inclined ladder-face nozzle: forming an included angle with the upper part by 70-100 degrees and the lower part by 20-60 degrees, directly conveying the mixture below the liquid level of the water phase, stirring the mixture on the operating surface of the shearing head of the emulsifying tank by 20-50 HZ for 10-45 min, and separating a discharging pipe from the emulsifying shearing head: the distance between the upper surfaces: 0.01-5cm, the following spacing: 0.01-3 cm.

In a preferred embodiment, in S5, the cooling temperature is: -50 ℃ to 0 ℃, cooling time: less than 5 s; the cooling time is defined as: the time required for the carotenoid emulsion to flow from the initial flow into the cooling tube to the total flow out of the cooling tube, preferably, the cooling temperature: -40 to-5 ℃, cooling time: 2-4 s.

In a preferred embodiment, the prepared product can be widely applied to the fields of food, health products, cosmetics, feed and medicines.

Compared with the prior art, the slow-release carbamazepine capsule and the preparation method thereof have the following advantages:

1. in the steps of filling inert gas in vacuum, emulsifying, stirring and blending under positive pressure, preparing carotenoid oil phase liquid and preparing aqueous phase solution, stirring anticlockwise at a constant speed to uniformly mix materials, and then shearing clockwise at a high speed to finely disperse the materials; the reverse stirring and the forward shearing are in liquid phase collision, so that the uniformity is improved, and the particle size of the material can be reduced; in addition, the prepared carotenoid oil phase liquid enters an ultrahigh-temperature melting system in an oxygen-free environment filled with inert gas and then enters a vacuum emulsification and rapid cooling process, the carotenoid is in an oxygen-free state in the whole process, oxidation deformation can be effectively prevented, and the carotenoid loss rate is reduced.

2. And (3) directly conveying the material reaching the melting temperature to a high-speed shearing surface through a discharging pipe, and instantly emulsifying and dispersing the material into particles to be embedded by the coating wall material. If the water phase solution tank is not formed by vacuum high-speed shearing, three phases of water phase, gas phase and oil phase are emulsified, and the stability of the system is greatly influenced; if the blanking pipe is not arranged, the carotenoid oil solution directly falls on the water phase solution surface, and the oil has the phenomena of agglomeration, floating surface, tank wall attachment and the like due to factors such as surface tension, temperature drop and the like, thereby having great influence on the stability and the embedding rate of the carotenoid; if the blanking pipe is not attached to the high-speed shearing surface, the particle size is larger due to collision in the process of mixing the oil phase and the water phase. In the scheme of the invention, the blanking pipe is attached to the high-speed shearing surface to form an included angle, the included angle is directly conveyed below the liquid level of the water phase, and the oil phase and the water phase are directly emulsified, sheared and embedded, so that the formed particle size is smaller and the system stability is better.

3. The invention dries the carotenoid product: reduction of carotenoid loss by 10-20%, trans carotenoid content degradation rate less than 10%, high all-trans content, and carotenoid particle diameter D₉₀Less than 500nm, embedding rate higher than 95%, small particle size, high stability, high bioavailability, high nutritive value, high safety without solvent, etc. The industrial problems of high loss rate, serious degradation of trans-content, high product solvent residue and the like in the existing processing process are solved, the production of finished products can be effectively reduced, the product quality and safety are improved, the enterprise benefit is increased, and the method is particularly suitable for large-scale industrial production of the carotenoid.

4. The carotenoid product can be widely applied to food, medicine, health care products, special diet and cosmetics, and not only can play a role in coloring, but also has the effects of health and nutrition.

Drawings

FIG. 1 is a trans content profile of carotenoids prepared according to example 1 of the present invention.

FIG. 2 is a trans content map of carotenoids prepared according to the present invention in comparative example 1.

FIG. 3 is a trans content profile of carotenoids prepared according to example 3 of the present invention.

FIG. 4 is a trans content map of carotenoids prepared according to the present invention in comparative example 2.

FIG. 5 is a particle size spectrum of carotenoid prepared according to the present invention in example 1.

FIG. 6 is a particle size spectrum of carotenoid prepared according to the present invention in comparative example 1.

FIG. 7 is a particle size spectrum of carotenoid prepared according to the present invention example 3.

FIG. 8 is a particle size spectrum of carotenoid prepared according to the present invention in comparative example 2.

Fig. 9 is a flow chart of the present invention.

FIG. 10 is a diagram of an apparatus of the present invention.

FIG. 11 is a schematic representation of the feed tube and the shear head of the emulsifier in accordance with the present invention.

Detailed Description

Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available.

Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.

Example 1

6kg of beta-carotene crystals (content: 98.2%, trans content 95.1%), tocopherol: 1.0kg, deodorized rosemary extract: 1.0kg, sunflower seed oil: adding 52Kg of the mixture into a low-temperature vacuum inert gas filling positive pressure emulsification stirring batching tank, and stirring the mixture at the temperature of 20 ℃ and the vacuum degree: -0.08Mpa, stirring: 15HZ, stirring for 25min, and emulsifying: 35HZ, emulsifying for 30min, and emulsifying and dispersing the oil phase solution uniformly. Opening a nitrogen valve, pressurizing and filling nitrogen, replacing the vacuum state, filling nitrogen gas into the preparation tank: 0.3Mpa, the beta-carotene is in a positive pressure protection state by inert gas, and the positive pressure is favorable for material mixing;

360Kg of modified starch, 80Kg of maltodextrin, reverse osmosis membrane water: and (2) emulsifying and dissolving 660Kg in a vacuum emulsifying tank, stirring anticlockwise according to 10HZ at constant speed for 15min, and then emulsifying clockwise according to 25HZ for 15min, wherein the stirring temperature is as follows: 30 ℃, vacuum degree: 0.06MPa, complete dissolution, and a standing water phase solution is in a transparent bubble-free and froth-free state;

the beta-carotene oil phase liquid is sent into an ultrahigh temperature heating pipe through a screw pump 35HZ, and the temperature is as follows: 175 ℃, time: 2s, automatically detecting the temperature of the beta-carotene liquid molten material on line: feeding at 135 ℃ in an emulsification mode;

the emulsification tank heated the aqueous phase to 70 ℃, vacuum: 0.05Mpa, directly conveying the oil phase below the liquid level of the water phase through a material pipe (a pipe orifice of a blanking inclined step surface forms an included angle between 70-100 degrees at the upper part and 20-60 degrees at the lower part), and finishing the blanking of the oil phase and emulsifying on the working surface of a high-speed 36HZ shearing head of an emulsifying tank (the distance between the blanking pipe and the emulsifying shearing head is 0.01-5cm at the upper part and 0.01-3cm at the lower part): 20min, no floating oil wall is built on the surface of the emulsified material and the wall of the tank;

the temperature of the emulsified material passing through a rapid cooling pipe is as follows: -20 ℃, time: 3s, cooling the materials to 15 ℃;

conveying the emulsified material to a sterile storage tank, spray drying to obtain carotenoid powder, and detecting the content of beta-carotene: 1.15% (loss rate: 2.4%), all-trans content: 91.2% (degradation rate: 4.1%), particle size D90: 186nm, embedding rate: 99.5 percent.

Example 2

6.8kg of beta-carotene crystals (content: 97.2%, trans content 94.5%), the deodorized rosemary extract: 3.0Kg, span 8Kg, MCT oil: adding 18Kg of the mixture into a low-temperature vacuum inert gas filling positive pressure emulsification stirring batching tank, wherein the temperature is 35 ℃, and the vacuum degree is as follows: -0.09Mpa, stirring: 25HZ, stirring for 40min, and emulsifying: emulsifying for 45min at 40HZ, and emulsifying to obtain uniformly dispersed oil phase solution. Opening a nitrogen valve, pressurizing and filling nitrogen, replacing the vacuum state, filling nitrogen gas into the preparation tank: 3.0Mpa, the beta-carotene is in a positive pressure protection state by inert gas, and the positive pressure is favorable for material mixing;

105Kg of glycerin, 27.2Kg of polyglycerin fatty acid ester, 12Kg of sucrose fatty acid ester, reverse osmosis membrane water: emulsifying and dissolving 20Kg in a vacuum emulsifying tank, stirring anticlockwise according to 8HZ for 10min at uniform speed, then emulsifying clockwise according to 10HZ for 15min, and stirring at the temperature: 20 ℃, vacuum degree: 0.05MPa, complete dissolution, and a standing water phase solution is in a transparent bubble-free and froth-free state;

the beta-carotene oil phase liquid is sent into an ultrahigh temperature heating pipe through a screw pump 25HZ, and the temperature is as follows: 210 ℃, time: and 3s, automatically detecting the temperature of the beta-carotene liquid molten material on line: feeding at 165 ℃ in an emulsification mode;

the emulsification tank heats the aqueous phase to 75 ℃, vacuum: 0.07Mpa, directly conveying the oil phase below the liquid level of the water phase through a material pipe (a pipe orifice of a blanking inclined step surface forms an included angle between 70-100 degrees at the upper part and 20-60 degrees at the lower part), and finishing the blanking of the oil phase and emulsifying on the working surface of a high-speed 45HZ shearing head of the emulsifying tank (the distance between the blanking pipe and the emulsifying shearing head is 0.01-5cm at the upper part and 0.01-3cm at the lower part): 25min, no floating oil wall is built on the surface of the emulsified material and the wall of the tank;

the temperature of the emulsified material passing through a rapid cooling pipe is as follows: -35 ℃, time: 3s, cooling the materials to 18 ℃;

conveying the emulsified materials to an aseptic storage tank, aseptically filling to obtain carotenoid emulsion, and detecting the content of beta-carotene: 3.18% (loss rate: 3.8%), all-trans content: 90.3% (degradation rate: 4.4%), particle size D90: 240 nm.

Example 3

12.0kg of lutein crystals (content 84.6%, trans content 98.5%), deodorised rosemary extract: 3.0kg, tocopherol: 3.0Kg, 3.0Kg of mono-diglycerol fatty acid ester, MCT oil: adding 29.0Kg of the mixture into a low-temperature vacuum inert gas filling positive pressure emulsification stirring batching tank, wherein the temperature is 35 ℃, and the vacuum degree is as follows:

-0.09Mpa, stirring: 25HZ, stirring for 40min, and emulsifying: emulsifying for 45min at 40HZ, and emulsifying to obtain uniformly dispersed oil phase solution. Opening a nitrogen valve, pressurizing and filling nitrogen, replacing the vacuum state, filling nitrogen gas into the preparation tank: 2.5Mpa, the lutein is protected by inert gas positive pressure, and the positive pressure is favorable for material mixing;

emulsifying and dissolving 170Kg of glycerin and 80Kg of polyglycerol fatty acid ester in a vacuum emulsifying tank, stirring counterclockwise according to 15HZ firstly, stirring at uniform speed for 15min counterclockwise, then emulsifying clockwise according to 10HZ for 10min, and stirring at the temperature: 20 ℃, vacuum degree: 0.02MPa, complete dissolution, and a standing water phase solution is in a transparent bubble-free and froth-free state;

the lutein oil phase liquid is sent into an ultrahigh temperature heating pipe through a screw pump 30HZ, and the temperature is as follows: 160 ℃, time: and 3s, automatically detecting the temperature of the lutein liquid molten material on line: feeding at 125 ℃ in an emulsification mode;

the emulsification tank heated the aqueous phase to 55 ℃, vacuum: 0.06Mpa, directly conveying the oil phase below the liquid level of the water phase through a material pipe (a pipe orifice of a blanking inclined step surface forms an included angle between 70-100 degrees at the upper part and 20-60 degrees at the lower part), and finishing oil phase blanking and emulsification on the high-speed 45HZ shearing head working surface of the emulsification tank (the distance between the blanking pipe and the emulsification shearing head is 0.01-5cm at the upper part and 0.01-3cm at the lower part): 15min, no floating oil wall is built on the surface of the emulsified material and the wall of the tank;

the temperature of the emulsified material passing through a rapid cooling pipe is as follows: -30 ℃, time: 3s, cooling the materials to 10 ℃;

conveying the emulsified materials to an aseptic storage tank, carrying out aseptic filling to obtain lutein emulsion, and detecting the lutein content: 3.25% (loss rate: 4.0%), all-trans content: 95.2% (degradation rate: 3.4%), particle size D90: 380 nm.

Comparative example 1

360Kg of modified starch, 80Kg of maltodextrin, reverse osmosis membrane water: and (3) emulsifying and dissolving 660Kg in an emulsifying tank: 25HZ, temperature: completely dissolving at 30 ℃, standing a large amount of bubbles and floating foam on the surface of the water phase, and heating to 70 ℃ for later use;

6kg of beta-carotene crystals (content: 98.2%, trans content 95.1%), tocopherol: 1.0kg, deodorized rosemary extract: 1.0kg, sunflower seed oil: adding 52Kg of the mixture into a normal pressure thermosol, stirring uniformly, and heating to 135 ℃ for 55 min;

slowly adding beta-carotene oil phase liquid through a valve, emulsifying for 20min after finishing blanking in a 36HZ emulsified water phase tank, wherein the wall of the emulsifying tank is splashed with floating oil and a large amount of bubbles are in the emulsion, so that an oil, water and gas three-phase unstable system is easily formed;

cooling the emulsified material to 30 ℃ through a sandwich tank, wherein the time is as follows: 70 min;

conveying the emulsified material to a sterile storage tank, spray drying to obtain carotenoid powder, and detecting the content of beta-carotene: 0.96% (loss rate: 18.6%), all-trans content: 75.6% (degradation rate: 20.5%), particle size D90: 2300nm, embedding rate: 86.6 percent.

The results of comparing the data of example 1 with that of comparative example 1 are shown in table 1.

TABLE 1

Comparative example 2

Emulsifying and dissolving 170Kg of glycerin and 80Kg of polyglycerol fatty acid ester in an emulsifying tank, and emulsifying: 5HZ, temperature: dissolving completely at 20 deg.C and normal pressure, standing to remove a large amount of bubbles and froth on the surface of water phase, heating to 55 deg.C;

12.0kg of lutein crystals (content 84.6%, trans content 98.5%), deodorised rosemary extract: 3.0kg, tocopherol: 3.0Kg, 3.0Kg of mono-diglycerol fatty acid ester, MCT oil: adding 29.0Kg of the mixture into a normal pressure thermosol, stirring uniformly, heating to 125 ℃ for 45 min;

slowly adding lutein oil phase liquid through a valve, emulsifying for 15min after finishing blanking in a 45HZ emulsified water phase tank, wherein the wall of the emulsifying tank is splashed with floating oil and a large amount of bubbles are in the emulsion, so that an oil, water and gas three-phase unstable system is easily formed;

cooling the emulsified material to 25 ℃ through a sandwich tank, wherein the time is as follows: 55 min;

conveying the emulsified materials to an aseptic storage tank, carrying out aseptic filling to obtain lutein emulsion, and detecting the lutein content: 2.86% (loss rate: 15.4%), all-trans content: 81.7% (degradation rate: 17.1%), particle size D90: 1308 nm.

The results of comparing the data of example 3 with that of comparative example 2 are shown in Table 2.

TABLE 2

Finally, it should be noted that: it should be understood that the above examples are only for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.