Carotenoid oil suspension and preparation method thereof

Abstract

The invention belongs to the field of food processing, particularly relates to a carotenoid oil suspension and a preparation method thereof, and more particularly relates to a high-content and low-viscosity carotenoid oil suspension and a preparation method thereof. A dispersion medium of the carotenoid oil suspension provided by the invention comprises an oily substance, and the carotenoid oil suspension contains two parts of carotenoid particles shown as (i) and (ii): (i) carotenoid particles with Dv (90) greater than or equal to 0.01 mu m and less than or equal to 0.5 mu m; (ii) carotenoid particles having a Dv (90) of 3 [mu] m or more and 20 [mu] m or less; the mass ratio of the (i) part to the (ii) part is 1: (1-5). According to the invention, the particle size distribution of carotenoid particles is controlled by utilizing a homogenizing process, so that the requirement of low viscosity of the oil suspension can be met, and meanwhile, high content of effective components can be kept.

Description

Technical Field

[0001] The invention belongs to the field of food processing, and in particular relates to a carotenoid oil suspension and a preparation method thereof, and more particularly relates to a high-content, low-viscosity carotenoid oil suspension and a preparation method thereof. Background Art

[0002] Carotenoids are a class of polyene compounds with multiple unsaturated bonds, which are widely found in algae, fungi and plants. As one of the most important natural pigments, carotenoids have a wide range of biological activities, such as anti-oxidation, anti-cancer, retinal protection, cardiovascular health and prevention of prostate disease, etc. At the same time, they are also the main source of vitamin A in the body.

[0003] At present, the most common way for people to supplement carotenoids is through dietary supplements. Since most carotenoids are insoluble in water, slightly soluble in oil, and easily degraded by light, oxygen, moisture, heavy metals, oxidants or reducing agents, in practical applications, carotenoids are often required to be made into different dosage forms, such as oil suspensions, water-dispersible dry powders, etc., according to different product characteristics or application requirements, in order to meet the processing requirements of different products.

[0004] Carotenoid oil suspension is a common dosage form, which is a viscous fluid liquid made by evenly suspending carotenoids in vegetable oil and adding appropriate excipients. It can be used to fill soft capsules to make dietary supplements for human consumption. In order to optimize or improve carotenoid oil suspension, the prior art has conducted many aspects of research, for example,

[0005] Reference 1 discloses a method for preparing a β-carotene oil suspension, which comprises mixing β-carotene, an oil-phase antioxidant, an oil-phase emulsifier and a vegetable oil, and grinding them to obtain a β-carotene oil suspension. This study promotes the mixing of β-carotene and vegetable oil by adding an oil-phase emulsifier, improves the solubility of β-carotene in vegetable oil, reduces the loss rate of β-carotene during grinding, improves grinding efficiency and reduces the particle size of the oil suspension after grinding, thereby improving the stability and bioavailability of the β-carotene oil suspension. At the same time, the addition of an oil-phase emulsifier can also ensure that the final β-carotene oil suspension has good fluidity at room temperature.

[0006] Reference 2 discloses a method for preparing a low-viscosity and high-fluidity carotenoid oil suspension, which comprises mixing carotenoid crystals with tetrahydrofuran and ketone solvents in sequence, removing fat-soluble cellulose and phospholipids by recrystallization, and then mixing and grinding the mixture with vegetable oil to obtain the carotenoid oil suspension. This study reduces the viscosity of the carotenoid oil suspension by removing fat-soluble cellulose and phospholipids as much as possible during the preparation of carotenoid crystals, thereby making it easy to operate and uniformly fill when used to prepare soft capsules, and at the same time increasing the effective ingredient content of carotenoids in the oil suspension.

[0007] Reference 3 discloses a method for preparing a stable lutein oil suspension, which comprises mixing lutein with vegetable oil at a certain temperature, and suspending the lutein in the vegetable oil as particles of 0.1 to 5 μm by a high-pressure homogenizer, and then degassing and packaging the suspension after reduced pressure. The method for preparing the lutein oil suspension provided in this study has a simple process and a wide range of applications. The product does not contain surfactants and other antioxidants, has a high lutein content (up to 20% or more), and has the advantages of safety, stability and high bioavailability.

[0008] Reference 4 discloses a method for preparing a carotenoid oil suspension with high bioavailability, wherein carotenoids are mixed with an organic solvent, and after being completely dissolved, the mixture is injected into a high-speed stirring vegetable oil solution by atomization, and the organic solvent generated during atomization is recovered, and finally a carotenoid oil suspension with an average particle size of less than 5 μm is obtained. This study injects the carotenoid solution into the vegetable oil in an atomized form, and the organic solvent evaporates to precipitate the carotenoid in an amorphous form. Under high-speed stirring, the precipitated carotenoid crystals will not re-aggregate and enlarge the particle size, thereby ensuring that the carotenoid particles in the final oil suspension are fine enough, which is conducive to human absorption and utilization.

[0009] References:

[0010] Reference 1: CN115671047A;

[0011] Reference 2: CN101828693B;

[0012] Reference 3: CN101836954B;

[0013] Reference 4: CN102552173B. Summary of the invention

[0014] Problem that the invention aims to solve

[0015] In order to optimize and improve the various properties of carotenoid oil suspensions, such as viscosity, fluidity, active ingredient content, stability, bioavailability, etc., the prior art has conducted various studies, but such studies are still not sufficient. For example, in the oil suspension preparation method provided in Reference 1, a certain amount of oil phase emulsifier is required to assist in achieving the goals of high active ingredient content and low viscosity, and this component will remain in the final product, resulting in complex components of the final product; in the oil suspension preparation method provided in Reference 2, in order to achieve the goals of high active ingredient content and low viscosity, additional process steps are required to remove fat-soluble cellulose and phospholipid substances, resulting in a certain degree of complexity in the overall process; in the method provided in Reference 3, lutein needs to be mixed with vegetable oil at a certain temperature, and the temperature is high during the process, which may cause lutein decomposition and isomerization; the method provided in Reference 4 uses an organic solvent, which is prone to the problem of organic solvent residue; and References 3 and 4 focus on the relationship between the composition of the oil suspension components and the particle size and human absorbability, without considering other changes in the characteristics of the oil suspension that may occur during the process.

[0016] Since the various properties of the oil suspension affect each other, it is still difficult to prepare a carotenoid oil suspension with excellent properties in all aspects. To this end, the purpose of the present invention is to provide a carotenoid oil suspension with high active ingredient content and low viscosity, and to provide a simple preparation method thereof.

[0017] Solutions for solving problems

[0018] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0019] [1] A carotenoid oil suspension, characterized in that the dispersion medium of the carotenoid oil suspension comprises an oily substance, and the carotenoid oil suspension comprises two parts of carotenoid particles as shown in (i) and (ii):

[0020] (i) carotenoid particles with a Dv(90) of 0.01 μm or more and 0.5 μm or less;

[0021] (ii) carotenoid particles with a Dv(90) of 3 μm or more and 20 μm or less;

[0022] The mass ratio of the part (i) to the part (ii) is 1:(1-5).

[0023] [2] The carotenoid oil suspension according to [1], characterized in that the dispersion medium is a vegetable oil or a medium-chain triglyceride, and the vegetable oil includes at least one of sunflower oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, olive oil and cottonseed oil.

[0024] [3] The carotenoid oil suspension according to [1] or [2], characterized in that the carotenoid oil suspension also contains an antioxidant, and the antioxidant includes at least one of tocopherol, ascorbyl palmitate, tert-butylhydroquinone, propyl gallate and ethoxyquin.

[0025] [4] The carotenoid oil suspension according to any one of [1] to [3], characterized in that the carotenoid comprises at least one of β-carotene, lutein, zeaxanthin, lycopene and astaxanthin.

[0026] [5] A method for preparing a carotenoid oil suspension according to any one of [1] to [4], characterized in that the method comprises the following steps:

[0027] (a) mixing carotenoid crystals with an oily substance and an optional antioxidant, stirring and dispersing the mixture to form a suspension I;

[0028] (b) subjecting the suspension Ia derived from the suspension I to a first homogenization treatment to obtain a dispersion IA containing carotenoid particles having a Dv(90) of greater than or equal to 0.01 μm and less than or equal to 0.5 μm;

[0029] (c) subjecting the suspension Ib derived from the suspension I to a second homogenization treatment to obtain a dispersion IB containing carotenoid particles having a Dv(90) of 3 μm or more and 20 μm or less;

[0030] (d) mixing the dispersion IA and the dispersion IB in a mass ratio of 1:(1-5) to obtain the carotenoid oil suspension;

[0031] The steps (b) and (c) are performed simultaneously or in any order.

[0032] [6] The preparation method according to [5] is characterized in that, in the step (a), the Dv(90) of the carotenoid crystals is greater than or equal to 5 μm and less than or equal to 30 μm.

[0033] [7]. The preparation method according to [5] or [6], characterized in that in the step (a), the stirring and dispersing time is 0.5 to 1 h, and the stirring and dispersing speed is 8 to 10 m / s.

[0034] [8] The preparation method according to any one of [5] to [7] is characterized in that in the steps (b) and (c), the first homogenization treatment and the second homogenization treatment are cooled by cooling water, and the temperature of the cooling water for the first homogenization treatment and the second homogenization treatment is independently 4 to 15°C.

[0035] [9]. The preparation method according to any one of [5] to [8] is characterized in that in the step (b), the parameters of the first homogenization treatment include: a homogenization pressure of 900 to 1100 bar and a feed rate of 30 to 80 kg / h.

[0036]

[10] . The preparation method according to any one of [5] to [9] is characterized in that in the step (c), the parameters of the second homogenization treatment include: a homogenization pressure of 350 to 450 bar and a feed rate of 80 to 100 kg / h.

[0037] Effects of the Invention

[0038] Through the implementation of the above technical solution, the present invention achieves the following beneficial effects:

[0039] First, the present invention provides a carotenoid oil suspension, which can achieve the requirement of low viscosity of the oil suspension by controlling the particle size distribution of the carotenoid therein, so that the product has good fluidity at room temperature, avoiding the degradation loss caused by the need for an additional heating step in subsequent applications. At the same time, the carotenoid oil suspension provided by the present invention has a high content of effective ingredients, and the carotenoids are evenly dispersed in the medium. It is also easier to maintain a uniform dispersion state during subsequent applications, and has good stability, thereby improving the application performance of the product, improving the appearance quality of the final product, and meeting the needs of consumers. In addition, the carotenoid oil suspension provided by the present invention has simple ingredients, does not contain additional auxiliary preparations such as organic solvents, and is safe and environmentally friendly.

[0040] Furthermore, the present invention provides a method for preparing a carotenoid oil suspension, which can achieve the preparation of a high-content, high-trans carotenoid product and a high-stability product through a simple operation process and simple equipment. At the same time, the method provided by the present invention can well control the particle size of carotenoids through a homogenization process, and the homogenization process parameters can be appropriately adjusted according to different product application requirements, thereby producing carotenoid oil suspensions with different particle size distributions to meet industry requirements. In addition, through the homogenization process, large particles in the oil suspension can be reduced, thereby reducing sedimentation and stratification phenomena and improving product stability. In addition, in the preparation method provided by the present invention, by passing cooling water during the homogenization process, the degradation risk of the effective ingredients of the oil suspension caused by the heat generated during the homogenization process can be effectively reduced, thereby improving the homogenization efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0041] Figure 1 : A schematic diagram of the preparation method of the carotenoid oil suspension provided by the present invention. DETAILED DESCRIPTION

[0042] The following describes the embodiments of the present invention, but the present invention is not limited thereto. The present invention is not limited to the various structures described below, and various changes can be made within the scope of the invention claim, and the embodiments and examples obtained by appropriately combining the technical means disclosed in different embodiments and examples are also included in the technical scope of the present invention.

[0043] In the present invention, the terms "comprising", "having", "including" or "containing" may mean inclusive or open-ended, and do not exclude additional, uncited elements or method steps. At the same time, "comprising", "having", "including" or "containing" may also mean closed, excluding additional, uncited elements or method steps.

[0044] In the present invention, the word "may" includes both performing a certain process and not performing a certain process.

[0045] In the present invention, "optional" or "optionally" means that certain substances, components, execution steps, application conditions and other factors are used or not used.

[0046] In the present invention, a numerical range expressed using “a numerical value A to a numerical value B” or “a numerical value A-a numerical value B” means a range including the endpoints A and B.

[0047] In the present invention, the term "about" is used to define the numerical range and parameters of the present invention, which are approximate values. The relevant values ​​in the specific embodiments have been presented as accurately as possible. Unless otherwise explicitly stated, it should be understood that all ranges, quantities, values ​​and percentages used in the present invention are modified by "about". Here, "about" usually means that the actual value is within ±5%, ±3%, ±1% or ±0.5% of a specific value or range.

[0048] In the present invention, the references to "some specific / preferred embodiments", "other specific / preferred embodiments", "embodiments", etc., mean that the specific elements (e.g., features, structures, properties and / or characteristics) described in connection with the embodiments are included in at least one embodiment described herein, and may or may not exist in other embodiments. In addition, it should be understood that the elements may be combined in various embodiments in any suitable manner.

[0049] In the present invention, the unit names used are all international standard unit names, and if there is no special statement, the "%" used represents weight or mass percentage.

[0050] Unless otherwise defined, other technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

[0051] <First aspect>

[0052] The first aspect of the present invention provides a carotenoid oil suspension, wherein the dispersion medium comprises an oily substance, and the oil suspension comprises two parts of carotenoid particles as shown in (i) and (ii):

[0053] (i) carotenoid particles with a Dv(90) of 0.01 μm or more and 0.5 μm or less;

[0054] (ii) carotenoid particles with a Dv(90) of 3 μm or more and 20 μm or less;

[0055] The mass ratio of the part (i) to the part (ii) is 1:(1-5).

[0056] The present invention can achieve the requirement of low viscosity for the oil suspension with high content of active ingredients by controlling the particle size distribution of carotenoids in the carotenoid oil suspension, and can provide help for specific application scenarios of subsequent products.

[0057] In some embodiments, the Dv(90) of the carotenoid particles of part (i) may be 0.01 μm, 0.02 μm, 0.03 μm, 0.04 μm, 0.05 μm, 0.06 μm, 0.07 μm, 0.08 μm, 0.09 μm, 0.1 μm, 0.11 μm, 0.12 μm, 0.13 μm, 0.14 μm, 0.15μm, 0.16μm, 0.17μm, 0.18μm, 0.19μm, 0.2μm, 0.21μm, 0.22μm, 0.23μm, 0.2 4μm, 0.25μm, 0.26μm, 0.27μm, 0.28μm, 0.29μm, 0.3μm, 0.31μm, 0.32μm, 0.33μm, Preferably, the Dv(90) of the carotenoid particles in part (i) is greater than or equal to 0.05 μm and less than or equal to 0.45 μm; more preferably, the Dv(90) of the carotenoid particles in part (i) is greater than or equal to 0.1 μm and less than or equal to 0.4 μm; even more preferably, the Dv(90) of the carotenoid particles in part (i) is greater than or equal to 0.2 μm and less than or equal to 0.35 μm.

[0058] In some embodiments, the Dv(90) of the carotenoid particles in part (ii) may be 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm or 20 μm, etc.; preferably, the Dv(90) of the carotenoid particles in part (ii) is greater than or equal to 3 μm and less than or equal to 15 μm; more preferably, the Dv(90) of the carotenoid particles in part (ii) is greater than or equal to 4 μm and less than or equal to 12 μm; even more preferably, the Dv(90) of the carotenoid particles in part (ii) is greater than or equal to 4 μm and less than or equal to 10 μm.

[0059] In some embodiments, the mass ratio of the carotenoid particles in part (i) to the carotenoid particles in part (ii) can be 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5; preferably, the mass ratio of the carotenoid particles in part (i) to the carotenoid particles in part (ii) is 1:(1.5-3.5); more preferably, the mass ratio of the carotenoid particles in part (i) to the carotenoid particles in part (ii) is 1:(2-3).

[0060] It is generally understood in the art that the viscosity of the carotenoid oil suspension is closely related to the particle size distribution of the product. When the particle size is small, the viscosity of the oil suspension is high, which is inconvenient to use. However, the present invention unexpectedly discovered that by adding carotenoid particles with a smaller particle size than the main (higher proportion) carotenoid particles to the carotenoid oil suspension, a lubricating effect can be achieved, so that the oil suspension as a whole has a lower viscosity and better fluidity. In some embodiments, the viscosity of the carotenoid oil suspension provided by the present invention is 300-1300 cP.

[0061] In some embodiments, in the carotenoid oil suspension, the sum of the carotenoid particles of part (i) and part (ii) accounts for more than 90% of the carotenoid particles dispersed in the dispersion medium, preferably more than 95%, more preferably more than 98%. In some embodiments, in the carotenoid oil suspension, the carotenoid particles dispersed in the dispersion medium consist of the carotenoid particles of part (i) and part (ii).

[0062] The carotenoid oil suspension of the present invention is not particularly limited to a specific dispersion medium, and may include, for example, plant oil or medium-chain triglycerides and other physiologically acceptable substances.

[0063] In some embodiments, the dispersing medium of the carotenoid oil suspension of the present invention is a vegetable oil or a medium-chain triglyceride. In some embodiments, the oily substance in the carotenoid oil suspension of the present invention is a vegetable oil or a medium-chain triglyceride. In some embodiments, the vegetable oil includes at least one of sunflower oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, olive oil and cottonseed oil. In some specific embodiments, the vegetable oil is any one of sunflower oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, olive oil and cottonseed oil. For medium-chain triglycerides, it refers to triglycerides containing medium-chain fatty acids (fatty acids containing 6 to 12 carbon atom chains). The present invention does not specifically limit the medium chain triglycerides that can be used, such as but not limited to saturated caprylic acid triglyceride, saturated capric acid triglyceride, saturated caprylic acid-capric acid triglyceride, and complexes thereof, etc. The medium chain triglyceride can be synthesized by methods such as strong acid catalytic esterification, hydrolysis esterification, acyl chloride alcoholysis, biological enzyme direct esterification, biological enzyme transesterification, etc., and existing finished products can also be purchased through commercial channels. In some more specific embodiments, the dispersion medium of the carotenoid oil suspension of the present invention is sunflower oil or medium chain triglycerides.

[0064] In some embodiments, the carotenoid oil suspension of the present invention further comprises an antioxidant, which can effectively delay or inhibit the oxidation and rancidity of the dispersion medium such as oily substances, and ensure the quality of the product during the production and storage process. The present invention does not specifically limit the specific type of antioxidant.

[0065] In some embodiments, the antioxidant used in the carotenoid oil suspension of the present invention includes at least one of tocopherol, ascorbyl palmitate, tert-butylhydroquinone, propyl gallate and ethoxyquinoline. In some specific embodiments, the antioxidant used in the carotenoid oil suspension of the present invention is any one of tocopherol, ascorbyl palmitate, tert-butylhydroquinone, propyl gallate and ethoxyquinoline. In some more specific embodiments, the antioxidant used in the carotenoid oil suspension of the present invention is tocopherol.

[0066] The present invention does not particularly limit the specific usage amount of the antioxidant in the carotenoid oil suspension, as long as it meets the requirements of relevant laws and regulations.

[0067] In the carotenoid oil suspension of the present invention, a single carotenoid may be included, or multiple carotenoids may be included simultaneously. In some embodiments, the carotenoid includes at least one of β-carotene, lutein, zeaxanthin, lycopene and astaxanthin. In some specific embodiments, the carotenoid is any one of β-carotene, lutein, zeaxanthin, lycopene and astaxanthin. In some more specific embodiments, the carotenoid is β-carotene or astaxanthin.

[0068] Furthermore, in some embodiments, the carotenoid oil suspension provided by the present invention may contain 0.1% to 40% carotenoids by mass percentage.

[0069] <Second Aspect>

[0070] The second aspect of the present invention provides a method for preparing the carotenoid oil suspension described in the first aspect, comprising the following steps:

[0071] (a) mixing carotenoid crystals with an oily substance and an optional antioxidant, stirring and dispersing the mixture to form a suspension I;

[0072] (b) subjecting the suspension Ia derived from the suspension I to a first homogenization treatment to obtain a dispersion IA containing carotenoid particles having a Dv(90) of greater than or equal to 0.01 μm and less than or equal to 0.5 μm;

[0073] (c) subjecting the suspension Ib derived from the suspension I to a second homogenization treatment to obtain a dispersion IB containing carotenoid particles having a Dv(90) of 3 μm or more and 20 μm or less;

[0074] (d) mixing the dispersion IA and the dispersion IB in a mass ratio of 1:(1-5) to obtain the carotenoid oil suspension;

[0075] The steps (b) and (c) are performed simultaneously or in any order.

[0076] The schematic diagram of the preparation method of the carotenoid oil suspension provided by the present invention is as follows Figure 1 As shown, the specific process is: ① add the ground carotenoid crystals and oily substances into a stirring tank and stir and disperse; ② homogenize to obtain a small particle size product through homogenization 1; ③ obtain a relatively large particle size product through homogenization 2; ④ mix in a certain proportion to obtain a small particle size product. The types of carotenoids, oily substances and antioxidants described in the above preparation method are all as described in the first aspect.

[0077] The present invention uses a homogenization process to achieve the preparation of a high-content, low-viscosity carotenoid oil suspension with simple operation and simple equipment.

[0078] In order to facilitate the subsequent homogenization of the suspension and obtain a dispersion with a target particle size, the particle size of the carotenoid crystals described in step (a) can be appropriately controlled. In some embodiments, in the step (a), the Dv(90) of the carotenoid crystals is greater than or equal to 5 μm and less than or equal to 30 μm, for example, it can be 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm, 20 μm, 21 μm, 22 μm, 23 μm, 24 μm, 25 μm, 26 μm, 27 μm, 28 μm, 29 μm or 30 μm, etc.; preferably, in the step (a), the Dv(90) of the carotenoid crystals is greater than or equal to 5 μm and less than or equal to 25 μm; more preferably, in the step (a), the Dv(90) of the carotenoid crystals is greater than or equal to 8 μm and less than or equal to 23 μm.

[0079] The present invention does not specifically limit the method for obtaining the carotenoid crystals of the above-mentioned certain particle size. For example, the carotenoid crystals can be obtained by grinding the raw material. The specific grinding method includes but is not limited to airflow grinding. In some embodiments, the present invention uses airflow grinding equipment to adjust parameters to obtain the carotenoid crystals of the above-mentioned specific particle size. In some embodiments, the frequency of the airflow grinding is 200-300HZ.

[0080] In order to obtain a uniformly dispersed suspension I, the parameters of the stirring and dispersing in step (a) can be appropriately controlled. In some embodiments, the stirring and dispersing time is 0.5 to 1 h, and the stirring and dispersing speed is 8 to 10 m / s.

[0081] Furthermore, in order to make the final carotenoid oil suspension product contain carotenoid particles of different particle sizes, the present invention performs different homogenization treatments on the suspension I prepared in step (a). The homogenization treatment can be performed using a homogenizer. The present invention does not specifically limit the specific homogenization parameters, and the dispersion containing carotenoid particles of the target particle size can be finally obtained.

[0082] In some embodiments, in order to obtain a dispersion IA containing carotenoid particles with a Dv(90) greater than or equal to 0.01 μm and less than or equal to 0.5 μm, the parameters of the first homogenization treatment can be controlled to include: a homogenization pressure of 900 to 1100 bar, and a feed rate of 30 to 80 kg / h; preferably, the pressure of the first homogenization treatment is 950 to 1000 bar, and the feed rate is 40-60 kg / h.

[0083] In some embodiments, in order to obtain a dispersion IB containing carotenoid particles with a Dv(90) greater than or equal to 3 μm and less than or equal to 20 μm, the parameters of the second homogenization treatment can be controlled to include: a homogenization pressure of 350 to 450 bar, and a feed rate of 80 to 100 kg / h; preferably, the pressure of the second homogenization treatment is 380 to 450 bar, and the feed rate is 82-93 kg / h.

[0084] There is no particular limitation on the order of the first homogenization treatment and the second homogenization treatment, which may be performed in any order or simultaneously.

[0085] In order to avoid the heat generated during the homogenization process causing a large amount of degradation of carotenoids in the suspension, the present invention uses cooling water to cool the homogenization process in step (b) and step (c). The temperature of the cooling water for the first homogenization process and the second homogenization process can be independently 4 to 15°C, for example, can be independently 4°C, 5°C, 6°C, 7°C, 8°C, 9°C, 10°C, 11°C, 12°C, 13°C, 14°C or 15°C, etc.; preferably, the temperature of the cooling water can be independently 5-10°C.

[0086] Furthermore, by mixing the dispersion IA and the dispersion IB obtained in step (b) and step (c), an oil suspension containing carotenoids of different particle sizes can be obtained. In some embodiments, the mass ratio of the dispersion IA to the dispersion IB can be 1:1, 1:1.5, 1:2, 1:2.5, 1:3, 1:3.5, 1:4, 1:4.5, 1:5; preferably, the mass ratio of the dispersion IA to the dispersion IB is 1:(1.5-3.5); more preferably, the mass ratio of the dispersion IA to the dispersion IB is 1:(2-3). The present invention finds that by filling and mixing a portion of a sample with a smaller particle size into a carotenoid oil suspension sample with a large particle size, it can act as a lubricant, thereby improving the disadvantage of high viscosity of high-content products.

[0087] Furthermore, for the uniformity of the final product, after the dispersion IA and the dispersion IB are mixed, appropriate stirring operation may be performed to ensure uniform mixing.

[0088] Example

[0089] The embodiments of the present invention will be described in detail below in conjunction with examples, but those skilled in the art will appreciate that the following examples are only used to illustrate the present invention and should not be considered to limit the scope of the present invention. If no specific conditions are specified in the examples, they are carried out under normal conditions or conditions recommended by the manufacturer. Unless otherwise specified, the materials or instruments used are all commercially available conventional products.

[0090] Example 1

[0091] 1. β-carotene airflow grinding:

[0092] Add β-carotene crystals to the feed port of the air flow grinding equipment, equipment N2 feed speed: grinding frequency: 226HZ, filter bag: 700nm; grind to particle size: Dv(90) = 13.5μm.

[0093] 2. Preparation of 40% β-carotene suspension I:

[0094] 40 kg of the ground β-carotene crystals were mixed with 2 kg of tocopherol and 58 kg of sunflower oil, and stirred and dispersed for 1 hour at a stirring speed of 8 m / s to form a 40% β-carotene suspension I.

[0095] 3. Homogenizer homogenization:

[0096] (1) Preparation of dispersion IA: Turn on the homogenizer power supply, set the homogenization pressure to 1000 bar, connect the cooling water, the cooling water temperature is 6.5° C., feed 30 kg of the 40% β-carotene suspension I prepared in 2 above through a pneumatic pump at a feed rate of 50 kg / h, and homogenize twice until the particle size reaches Dv(90)=0.23 μm.

[0097] (2) Preparation of dispersion IB: Repeat the above steps and feed 70 kg of the 40% β-carotene suspension I prepared in step 2 through a pneumatic pump. Set the homogenizer to 380 bar, the cooling water temperature to 6.5° C., the feed rate to 85 kg / h, and homogenize twice until the particle size reaches: Dv(90)=5.6 μm.

[0098] 4. Mixing:

[0099] The dispersions IA and IB prepared in 3 above were mixed in a mass ratio of 1:2.5 and stirred to obtain a 40% β-carotene oil suspension.

[0100] Example 2

[0101] 1. β-carotene airflow grinding:

[0102] Add β-carotene crystals to the feed port of the air flow grinding equipment, equipment N2 feed speed: grinding frequency: 260HZ, filter bag: 700nm; grind to particle size: Dv(90)=16.8μm.

[0103] 2. Preparation of 30% β-carotene suspension I:

[0104] 30 kg of the ground β-carotene crystals were mixed with 2 kg of tocopherol and 68 kg of medium chain triglycerides, and stirred and dispersed for 0.6 h at a stirring speed of 9 m / s to form a 30% β-carotene suspension I.

[0105] 3. Homogenizer homogenization:

[0106] (1) Preparation of dispersion IA: Turn on the homogenizer power supply, set the homogenization pressure to 1000 bar, connect cooling water, the cooling water temperature is 7.5° C., feed 30 kg of the 30% β-carotene suspension I prepared in 2 above through a pneumatic pump at a feed rate of 60 kg / h, and homogenize twice until the particle size reaches Dv(90)=0.26 μm.

[0107] (2) Preparation of dispersion IB: Repeat the above steps and feed 70 kg of the 30% β-carotene suspension I prepared in step 2 through a pneumatic pump. Set the homogenizer to 450 bar, the cooling water temperature to 7.5° C., the feed rate to 90 kg / h, and homogenize twice until the particle size reaches: Dv(90)=7.6 μm.

[0108] 4. Mixing:

[0109] The dispersions IA and IB prepared in 3 above were mixed in a mass ratio of 1:2 and stirred to obtain a 30% β-carotene oil suspension.

[0110] Example 3

[0111] 1. Astaxanthin airflow grinding:

[0112] Add astaxanthin crystals to the feed port of the air flow grinding equipment, equipment N2 feed speed: grinding frequency: 280HZ, filter bag: 700nm; grind to particle size: Dv(90) = 21.5μm.

[0113] 2. Preparation of 40% astaxanthin suspension I:

[0114] 40 kg of the ground astaxanthin crystals were mixed with 2 kg of tocopherol and 58 kg of sunflower oil, and stirred and dispersed for 0.8 h at a stirring speed of 9 m / s to form a 40% astaxanthin suspension I.

[0115] 3. Homogenizer homogenization:

[0116] (1) Preparation of dispersion IA: Turn on the homogenizer power supply, set the homogenization pressure to 950 bar, connect the cooling water, the cooling water temperature is 8.0°C, feed 30 kg of the 40% astaxanthin suspension I prepared in 2 above through a pneumatic pump, the feed rate is 53 kg / h, and homogenize twice until the particle size reaches Dv(90)=0.29 μm.

[0117] (2) Preparation of dispersion IB: Repeat the above steps and feed 70 kg of the 40% astaxanthin suspension I prepared in step 2 through a pneumatic pump. Set the homogenization temperature to 420 bar, the cooling water temperature to 8.0° C., the feed rate to 86 kg / h, and homogenize twice until the particle size reaches: Dv(90)=9.5 μm.

[0118] 4. Mixing:

[0119] The dispersions IA and IB prepared in 3 above were mixed in a mass ratio of 1:2.5 and stirred to obtain a 40% astaxanthin oil suspension.

[0120] Comparative Example

[0121] 1. β-carotene airflow grinding:

[0122] Add β-carotene crystals to the feed port of the air flow grinding equipment, equipment N2 feed speed: grinding frequency: 450HZ, filter bag: 1000nm; grind to particle size: Dv(90) = 35μm.

[0123] 2. Preparation of 30% β-carotene suspension:

[0124] 30 kg of the ground β-carotene crystals were mixed with 2 kg of tocopherol and 68 kg of sunflower oil, and stirred and dispersed for 1 hour at a stirring speed of 9 m / s to form a 30% β-carotene suspension.

[0125] 3. Homogenization:

[0126] Turn on the homogenizer power supply, set the homogenization pressure to 800 bar, connect cooling water, the cooling water temperature is 5° C., feed the 30% β-carotene suspension prepared in 2 above through a pneumatic pump, the feed rate is 50 kg / h, and homogenize five times until the particle size reaches Dv(90)=9.3 μm to obtain a 30% β-carotene oil suspension.

[0127] Experimental example

[0128] The carotenoid content, viscosity, stability and retention rate of the oil suspensions finally prepared in Examples 1 to 3 and the comparative example were tested, and the experimental results are shown in Table 1. It can be seen that compared with the comparative example, the carotenoid oil suspensions prepared in the examples have a higher content of active ingredients, a lower viscosity, good stability and a high retention rate.

[0129] Table 1 Dispersion test results

[0130]

[0131] Stability coefficient test method: Take a 10mL centrifuge tube, weigh 10g of oil suspension and add it to the centrifuge tube. Set the centrifuge to 4000rpm at 25℃ for 47min. Use a vernier caliper to measure the oil separation layer height h1 and the total height of the oil suspension h, and calculate the lower layer ratio. R% = (1-(h1 / h)) × 100.

[0132] Industrial Applicability

[0133] The carotenoid oil suspension provided by the invention has a high content of effective ingredients, low viscosity, good stability, and industrial applicability. The preparation method of the carotenoid oil suspension provided by the invention has a simple operation process and is suitable for large-scale industrial production.

Claims

1. A carotenoid oil suspension, It is characterized in that The dispersion medium of the carotenoid oil suspension includes an oily substance, and the carotenoid oil suspension contains two parts of carotenoid particles as shown in (i) and (ii): (i) carotenoid particles with a Dv(90) of 0.01 μm or more and 0.5 μm or less; (ii) carotenoid particles with a Dv(90) of 3 μm or more and 20 μm or less; The mass ratio of the part (i) to the part (ii) is 1:(1-5).

2. The carotenoid oil suspension according to claim 1, It is characterized in that The dispersion medium is vegetable oil or medium-chain triglyceride, and the vegetable oil includes at least one of sunflower oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, olive oil and cottonseed oil.

3. The carotenoid oil suspension according to claim 1 or 2, It is characterized in that The carotenoid oil suspension also contains an antioxidant, which includes at least one of tocopherol, ascorbyl palmitate, tert-butylhydroquinone, propyl gallate and ethoxyquinoline.

4. The carotenoid oil suspension according to any one of claims 1 to 3, It is characterized in that The carotenoids include at least one of β-carotene, lutein, zeaxanthin, lycopene and astaxanthin.

5. A method for preparing the carotenoid oil suspension according to any one of claims 1 to 4, It is characterized in that The method comprises the following steps: (a) mixing carotenoid crystals with an oily substance and an optional antioxidant, stirring and dispersing the mixture to form a suspension I; (b) subjecting the suspension Ia derived from the suspension I to a first homogenization treatment to obtain a dispersion IA containing carotenoid particles having a Dv(90) of greater than or equal to 0.01 μm and less than or equal to 0.5 μm; (c) subjecting the suspension Ib derived from the suspension I to a second homogenization treatment to obtain a dispersion IB containing carotenoid particles having a Dv(90) of 3 μm or more and 20 μm or less; (d) mixing the dispersion IA and the dispersion IB in a mass ratio of 1:(1-5) to obtain the carotenoid oil suspension; The steps (b) and (c) are performed simultaneously or in any order.

6. The preparation method according to claim 5, It is characterized in that In the step (a), the Dv(90) of the carotenoid crystals is greater than or equal to 5 μm and less than or equal to 30 μm.

7. The preparation method according to claim 5 or 6, It is characterized in that In the step (a), the stirring and dispersing time is 0.5 to 1 h, and the stirring and dispersing speed is 8 to 10 m / s.

8. The preparation method according to any one of claims 5 to 7, It is characterized in that In the step (b) and the step (c), the first homogenization process and the second homogenization process are cooled by cooling water, and the temperature of the cooling water for the first homogenization process and the second homogenization process is independently 4 to 15°C.

9. The preparation method according to any one of claims 5 to 8, It is characterized in that In the step (b), the parameters of the first homogenization process include: a homogenization pressure of 900 to 1100 bar, and a feed rate of 30 to 80 kg / h.

10. The preparation method according to any one of claims 5 to 9, It is characterized in that In the step (c), the parameters of the second homogenization process include: a homogenization pressure of 350 to 450 bar, and a feed rate of 80 to 100 kg / h.

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