WO2019024548A1 - 一种脂溶性营养素微胶囊及其制备方法 - Google Patents

一种脂溶性营养素微胶囊及其制备方法 Download PDF

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WO2019024548A1
WO2019024548A1 PCT/CN2018/084596 CN2018084596W WO2019024548A1 WO 2019024548 A1 WO2019024548 A1 WO 2019024548A1 CN 2018084596 W CN2018084596 W CN 2018084596W WO 2019024548 A1 WO2019024548 A1 WO 2019024548A1
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Prior art keywords
fat
soluble
soluble nutrient
vitamin
microcapsule
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PCT/CN2018/084596
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English (en)
French (fr)
Inventor
李建东
胡柏剡
陈志荣
石立芳
李其川
朱小勇
邱贵生
张其磊
杨优敏
蔡林普
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浙江新和成股份有限公司
浙江大学
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Application filed by 浙江新和成股份有限公司, 浙江大学 filed Critical 浙江新和成股份有限公司
Priority to EP18841964.2A priority Critical patent/EP3607837B1/en
Priority to KR1020197028655A priority patent/KR20190126830A/ko
Priority to JP2020502198A priority patent/JP7205835B2/ja
Priority to CA3065840A priority patent/CA3065840A1/en
Priority to US16/605,683 priority patent/US20200029596A1/en
Priority to MX2019014381A priority patent/MX2019014381A/es
Publication of WO2019024548A1 publication Critical patent/WO2019024548A1/zh

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A23P10/35—Encapsulation of particles, e.g. foodstuff additives with oils, lipids, monoglycerides or diglycerides
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/105—Aliphatic or alicyclic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/111—Aromatic compounds
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/174—Vitamins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/15—Vitamins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/15—Vitamins
    • A23L33/155—Vitamins A or D
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P10/00—Shaping or working of foodstuffs characterised by the products
    • A23P10/30—Encapsulation of particles, e.g. foodstuff additives
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
    • A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B01J13/043—Drying and spraying
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2250/00—Food ingredients
    • A23V2250/30—Other Organic compounds
    • A23V2250/314—Ubiquinone, coenzyme Qn
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2250/00—Food ingredients
    • A23V2250/70—Vitamins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02—Making microcapsules or microballoons
    • B01J13/06—Making microcapsules or microballoons by phase separation

Definitions

  • the invention relates to the field of food and feed additives, in particular to a fat-soluble nutrient microcapsule and a preparation method thereof.
  • the fat-soluble nutrient of the present invention mainly refers to a fat-soluble vitamin, a carotenoid and a coenzyme Q 10 .
  • Vitamins are a kind of trace organic regulating substances that humans and animals must obtain from foods to maintain normal physiological functions. They play an important role in the growth, metabolism and development of the body; carotenoids are an important class of natural pigments. In general, it can improve the animal's fecundity, immune function, and has many physiological functions such as anti-oxidation, coloration and the ability to strengthen the communication between cells and cell seams.
  • Coenzyme Q 10 is a fat-soluble steroid that activates human cells and The energy of cell energy has the functions of improving human immunity, enhancing anti-oxidation, delaying aging and enhancing vitality of the human body. It is widely used in cardiovascular diseases in medicine, and is widely used in nutrition and health care products and food additives at home and abroad.
  • vitamins, carotenoids and coenzyme Q 10 are very unstable substances, they are extremely sensitive to light, heat and oxygen, and are not suitable for direct addition in feed or food. Therefore, many researchers and companies have developed their own As a method for stabilizing these active substances, such fat-soluble nutrients are usually prepared as microcapsules as an additive.
  • the fat-soluble nutrient microcapsules are generally prepared by dissolving nutrients and other fat-soluble core materials in oil or organic solvents to form an oil phase, and then mixing with water containing water-soluble wall materials, using high-pressure homogenization and high-speed shearing. Emulsification by high-speed jet, ultrasonic cavitation, grinding, etc., followed by spray granulation and drying to obtain microcapsules.
  • the patent CN101873848B improves the wall material of the microcapsule, which reports a preparation of a lipophilic health component comprising a lipophilic health component and a protective colloid, wherein the protective colloid is a modified starch having emulsifying ability,
  • the lipophilic health component is selected from the group consisting of vitamin A, CoQ10, and esters thereof.
  • Patent CN103549157B develops a microcapsule preparation method: adding a protein active enzyme to an emulsion containing nutrients, granulating, crosslinking, and drying to obtain a water-repellent vitamin microcapsule.
  • Patent US8685446B2 provides a multi-walled microcapsule that is embedded with multiple protective colloids.
  • the emulsion is easy to be layered in the process of waiting for spray drying after the completion of the emulsification, and the upper concentrated fat-soluble nutrient small oil beads are easily aggregated and become large oil beads, thereby affecting the package of the final product. Buried effect and bioavailability. Because of these influencing factors, the usual fat-soluble nutrient microcapsule products are partially lost in the preparation process, and the mass ratio of the active ingredient to the added fat-soluble nutrient in the final product is generally 90-96:100.
  • the object of the present invention is to solve the problem that the fat-soluble nutrient microcapsules of the prior art lose some nutrients in the preparation process, and provide a fat-soluble nutrient microcapsule with high stability and high active substance content and a preparation method thereof.
  • the present invention provides a fat-soluble nutrient microcapsule, which is in weight percentage, and the specific composition thereof is:
  • the ratio of the fat-soluble nutrient which remains active in the fat-soluble nutrient microcapsule to the initially added fat-soluble nutrient is 0.990-0.997:1.
  • the ratio of the fat-soluble nutrient which remains active in the microcapsules to the initially added fat-soluble nutrient is hereinafter referred to simply as the retention rate of the active substance, which indicates the loss of fat-soluble nutrients during the preparation.
  • the invention also provides a preparation method of the fat-soluble nutrient microcapsule, which comprises mixing a molten fat-soluble nutrient oil phase or a pre-dispersion comprising a fat-soluble core material and an aqueous phase containing a water-soluble wall material or respectively feeding under high pressure
  • the emulsion or dispersion obtained in the series cavitation emulsifier is subjected to spray granulation and drying to obtain a fat-soluble nutrient microcapsule.
  • the fat-soluble nutrient microcapsule of the present invention directly uses a fat-soluble nutrient melt oil or a pre-dispersion as an oil phase, does not require the addition of an additional fat or an organic solvent, and the microcapsule-embedded effective fat-soluble nutrient is in the preparation process. The loss is small and the retention rate of the active substance is high.
  • the method for preparing the fat-soluble nutrient microcapsule of the present invention adopts a continuous multi-stage series cavitation emulsification or dispersion method, which greatly reduces the emulsification or dispersion time, and effectively reduces the deterioration of the fat-soluble nutrient during the emulsification or dispersion process;
  • the emulsion or dispersion prepared by the emulsification or dispersion method has good stability, and the obtained microcapsule has high embedding rate, and the surface of the microcapsule is substantially free of fat-soluble nutrient residues, and the prepared nutrient microcapsule has high stability.
  • the preparation method of the fat-soluble nutrient microcapsule of the invention has low energy consumption and high efficiency.
  • the fat-soluble nutrient microcapsule of the present invention requires only a small amount of an antioxidant to be added, and a high retention rate of the active material can be maintained without adding a fat-soluble antioxidant.
  • the fat-soluble nutrient of the present invention is a vitamin A derivative, a vitamin E derivative, vitamin D, carotenoid, and coenzyme Q.
  • the fat-soluble nutrient is an unstable nutrient, and specifically may be vitamin A acetate, vitamin A palmitate, vitamin E acetate, vitamin E palmitate, vitamin D2, vitamin D3, and beta-carotene.
  • the antioxidants of the present invention are propyl gallate, BHT, tea polyphenol, alpha-tocopherol, L-ascorbic acid-6-palmitate, tea polyphenol palmitate, sodium ascorbate, ascorbic acid, thiodipropyl One or more of dilauryl acid ester and lipoic acid.
  • the antioxidant is a water-soluble antioxidant, and may be one or more of ascorbic acid, sodium ascorbate, erythorbic acid, and sodium erythorbate.
  • water-soluble antioxidants are beneficial to reduce the amount of oil phase in the process of emulsification or dispersion, increase the embedding rate of microcapsules, reduce the amount of oil phase exposed on the surface of microcapsules, and improve the stability of fat-soluble nutrients in spray granulation and drying stages.
  • the wall material of the present invention is a water soluble colloid and a carbohydrate.
  • the water-soluble colloid is one or more of gelatin, gum arabic, gelatinizable modified starch, and octenyl succinate starch.
  • the carbohydrate is one or more of dextrin, glucose, white granulated sugar, fructose, maltose, cellophane, and corn starch.
  • the present invention also provides a method for preparing the above-mentioned fat-soluble nutrient microcapsule, which comprises mixing a molten fat-soluble nutrient oil phase or a pre-dispersion comprising a fat-soluble core material and an aqueous phase containing a water-soluble wall material or respectively feeding under high pressure
  • the emulsion or dispersion obtained in the series cavitation emulsifier is subjected to spray granulation and drying to obtain a fat-soluble nutrient microcapsule.
  • the molten fat-soluble nutrient oil phase refers to a liquid oil phase of a fat-soluble nutrient obtained at a temperature higher than a melting point of a fat-soluble nutrient.
  • the pre-dispersion of the fat-soluble nutrient refers to a nutrient solid suspension obtained by putting fat-soluble nutrients into water and uniformly dispersing them by grinding or the like.
  • the multistage tandem cavitation emulsifier described above refers to an emulsifier in which a plurality of cavitation emulsifiers having abrupt shrinkage-expansion cross sections are used in series.
  • the cavitation emulsifier is composed of a contraction section and an expansion section which are connected to each other. In each stage of the emulsifier, the fluid first passes through the contraction section and then enters the expansion section. In the cavitation emulsifier, the outlet of the constricted section and the outlet of the expanded section do not overlap all or part of the outlet direction of the constricted section.
  • the decrease in the internal diameter of the constricted section is reduced (and not closed), and the fluid produces a high velocity in the constricted section that is significantly higher than the entrance of the constricted section and reaches a maximum at the junction of the constricted section and the expanded section.
  • the fluid collides with the wall of the expansion section at a high speed, causing cavitation, thereby achieving an emulsification or dispersion effect.
  • the multi-stage series cavitation emulsifier is a series cavitation emulsifier of 3 or more.
  • the multistage tandem cavitation emulsifier is selected according to the physical properties of the fat-soluble nutrients, particularly the melt oil or the pre-dispersion of the fat-soluble nutrients and the viscosity of the water-soluble wall material solution.
  • the multi-stage tandem cavitation emulsifier is a 5-10 stage series cavitation emulsifier.
  • homogeneous emulsification or dispersion can be completed in a very short time by passing the fluid under high pressure at a high speed through a multistage series cavitation emulsifier.
  • the high pressure is 100-500 MPa.
  • the outlet velocity of the fluid in the contraction section of the cavitation emulsifier reaches a maximum value and impinges on the wall surface of the expansion section, thereby forming a plurality of cavitation emulsification or dispersion, which can be disposable in a short time.
  • Complete emulsification or dispersion Complete emulsification or dispersion.
  • the above oil phase is a molten fat-soluble nutrient or pre-dispersion, and no additional fat or organic solvent is added.
  • the surface of the fat-soluble nutrient in contact with the external environment is small, and in combination with the above-mentioned emulsification or dispersion method, the prepared microcapsules have high active ingredients, and the active ingredients are almost no loss during the preparation.
  • the above preparation method can be carried out under the protection of nitrogen.
  • nitrogen protection can eliminate the effects of oxygen on the nutrients in the environment and ensure the stability of fat-soluble nutrients during the preparation of microcapsules.
  • the water used in the above aqueous phase can be deoxidized in advance to further eliminate the influence of oxygen in the environment and improve the stability of the fat-soluble nutrients during the preparation of the microcapsules.
  • the mass ratio of the hydrophilic wall material to the water is from 0.5 to 1:1.
  • the above drying process may be spray drying, spray granulation-fluidization drying or the like.
  • Vitamin A microcapsule and preparation thereof are Vitamin A microcapsule and preparation thereof
  • the emulsion is continuously granulated into a spray granulation tower sprayed with corn starch, and then fluidized and dried to obtain vitamin A acetate fine particles.
  • the content of each component is determined as shown in Table 1, and the production process is calculated.
  • the vitamin A acetate retention rate was 99.7%.
  • the vitamin A acetate microparticles were placed in a stability test at 25 ° C. After 6 months, the vitamin A acetate content in the microparticles was measured, and the retention rate of vitamin A acetate was calculated to be 98.2% after 6 months.
  • Vitamin D3 microcapsule and preparation thereof are Vitamin D3 microcapsule and preparation thereof
  • the content of each component was measured as shown in Table 1, and the retention rate of vitamin D3 in the production process was calculated to be 99.2%.
  • the vitamin D3 dry powder was placed at 25 ° C for stability test. After 6 months, the vitamin D3 content in the vitamin D3 dry powder was measured. The retention rate of vitamin D3 was calculated to be 98.5% after 6 months.
  • the lutein crystals 5.3Kg and water 30Kg were put into a ball mill and ground to 5 ⁇ m or less to obtain a pre-dispersion; 1050 L of drinking water was placed in the batching kettle, and then 190 kg of sodium octenyl succinate, 60 Kg of glucose, 250 Kg of dextrin, 5 Kg of VC sodium was stirred at a temperature to obtain a hydrosol solution; the predispersion and the hydrosol solution were uniformly mixed under stirring to obtain a dispersion.
  • the above dispersion is pumped into a 6-stage series cavitation emulsifier by a high-pressure pump, the pressure of the apparatus is adjusted to 500 MPa, continuous dispersion is performed, a lutein dispersion is obtained at the outlet, and the lutein dispersion is continuously passed into the spray drying tower.
  • the spray drying was carried out to obtain a dry powder of lutein, and the content of each component was measured as shown in Table 1.
  • the lutein retention rate in the production process was calculated to be 99.6%.
  • the lutein dry powder was placed at 25 ° C for stability test. After 6 months, the content of lutein in the dry powder of lutein was measured.
  • the retention rate of lutein was calculated to be 99.2% after 6 months.
  • Vitamin A microcapsule and preparation thereof are Vitamin A microcapsule and preparation thereof
  • the content of each component is determined as shown in Table 1, and vitamin A in the production process is calculated.
  • the acetate retention rate was 94.2%.
  • the vitamin A was placed in a stability test at 25 ° C. After 6 months, the vitamin A acetate content in the vitamin A acetate microparticles was measured. The retention rate of vitamin A acetate was calculated to be 88.1% after 6 months. .
  • Vitamin D3 microcapsule and preparation thereof are Vitamin D3 microcapsule and preparation thereof
  • the content of each component was measured as shown in Table 1, and the vitamin D3 retention rate during the production process was calculated to be 96.5%.
  • the above vitamin D3 dry powder was placed at 25 ° C for stability test, and after 6 months, the vitamin D3 content in the vitamin D3 dry powder was measured, and the retention rate of vitamin D3 was calculated to be 93.5% after 6 months.
  • tocopherol into the melt kettle, and then add 5.3Kg of lutein crystals, heat up to 180 °C to melt all the materials, then cool to 90 °C to get melted oil; put 1050L of drinking water into the emulsifier, and then cast
  • the gelled modified starch 190 Kg, fructose 60 Kg, and dextrin 250 Kg were stirred at a temperature to obtain a hydrosol solution.
  • the above lutein melt oil was added dropwise to the emulsification kettle, and the emulsion was obtained by shearing at a high speed for 20 minutes.
  • the lutein emulsion was sprayed into a spray drying tower for spray drying to obtain a dry powder of lutein.
  • the content of each component was determined as shown in Table 1.
  • the lutein retention rate during the production process was calculated to be 75.6%.
  • the lutein dry powder was placed in a stability test at 25 ° C. After 6 months, the content of lutein in the dry powder of lutein was measured, and the retention rate of lutein was calculated to be 72.2% after 6 months.
  • the group distribution ratio and the cavitation emulsifier series and pressure are according to Table 1, and the preparation process is different according to the second embodiment (Examples 4, 5, 10) or the third embodiment (Examples 6, 7, 8, and 9). Nutrient microcapsules were used to determine the content of each component, and the retention and stability of the nutrients were calculated. The results are shown in Table 1.

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Abstract

本发明公开了一种脂溶性营养素微胶囊及其制备方法，该脂溶性营养素微胶囊的重量百分比组成为：脂溶性营养素0.2-51.6％、抗氧化剂0.2-5.0％、壁材41.4-97.6％、水分2.0-5.0％，所述的脂溶性营养素微胶囊中保持活性的脂溶性营养素与初始添加的脂溶性营养素的比值为0.99-0.997:1。该脂溶性营养素微胶囊的制备方法包括乳化和制粒过程，其中，乳化是在空化乳化器中进行，通过该制备方法可以使脂溶性营养素微胶囊的营养素活性物质损失少，并且稳定性高。

Description

一种脂溶性营养素微胶囊及其制备方法 技术领域
本发明涉及食品、饲料添加剂领域，具体涉及一种脂溶性营养素微胶囊及其制备方法。
背景技术
本发明所述的脂溶性营养素主要是指脂溶性维生素、类胡萝卜素和辅酶Q 10。维生素是人和动物为维持正常的生理功能而必须从食物中获得的一类微量有机调节物质，在机体生长、代谢、发育过程中发挥着重要的作用；类胡萝卜素是一类重要天然色素的总称，能够提高动物繁殖力、免疫功能，具有抗氧化、着色及加强细胞与细胞缝间联接交流的能力等多种生理功能；辅酶Q 10是一种脂溶性醌类化合物，能激活人体细胞和细胞能量的营养，具有提高人体免疫力、增强抗氧化、延缓衰老和增强人体活力等功能，医学上广泛用于心血管系统疾病，国内外广泛将其用于营养保健品及食品添加剂。
由于维生素、类胡萝卜素和辅酶Q 10均是非常不稳定的物质，对光、热和氧极其敏感，不适合直接在饲料或食品中添加，因此不少研究人员及公司开发出了各自用于稳定这些活性物质的方法，作为本领域常用的方法，通常将这类脂溶性营养素制备成微胶囊作为添加剂使用。
脂溶性营养素微胶囊的制备方法通常是将营养素和其它脂溶性芯材溶于油脂或者有机溶剂中配成油相，再与包含水溶性壁材的水相混合，使用高压均质、高速剪切、高速射流、超声波空化、研磨等方法进行乳化，再进行喷雾造粒、干燥，得到微胶囊。
为了提高脂溶性微胶囊的稳定性，本领域技术人员通常会对微胶囊的壁材、油相油脂或有机溶剂的选择、添加支撑结构等方面进行改良。如专利CN101873848B改良了微胶囊的壁材，其报道了一种亲脂性健康成分的制剂，包含亲脂性健康成分和保护性胶体，其中所述保护性胶体是具有乳化能力的改性淀粉，所述亲脂性健康成分选自维生素A、CoQ10及它们的 酯构成的组。专利CN103549157B开发了一种微胶囊制备方法：将包含营养素的乳液中加入蛋白活性酶，再造粒、交联反应后干燥，得到斥水型维生素微胶囊。专利US8685446B2提供了一种多重壁材的微胶囊，其采用了多重保护胶体进行包埋。
现有技术中对微胶囊制备技术的乳化过程中如何提高脂溶性营养素的稳定性，通常是在油相中添加抗氧化剂。如WO2016169942A1、CN101902922B、CN106063534A、CN101744790B等专利中，均是通过添加脂溶性抗氧化剂来保证乳化过程中脂溶性营养素的稳定性。但是由于乳化方法，如高速剪切、高压均质、超声波乳化等存在以下问题：1)乳化过程需要分批进行且在敞开环境中，单批乳化时间长，乳化时剪切部位温度高，易使脂溶性营养素变质；2)高速剪切机、高压均质机、超声波乳化器等所需电机功率大，能耗高；4)由于是机械作用，油相表面与外环境接触面大，脂溶性营养素易变质；3)由于分批操作，乳化完成后在等待喷雾干燥的过程中乳液易分层，上部聚集的脂溶性营养素小油珠易聚并成大油珠，从而影响最终产品的包埋效果和生物利用度。因为这些影响因素，通常的脂溶性营养素微胶囊产品在制备过程中会有部分损失，最终产品中的活性成分与添加的脂溶性营养素的质量比一般为90-96:100。
发明内容
本发明的目的在于解决现有技术的脂溶性营养素微胶囊在制备过程会损失部分营养素的问题，提供了一种高稳定性、高活性物质含量的脂溶性营养素微胶囊及其制备方法。
为解决上述技术问题，本发明提供了一种脂溶性营养素微胶囊，以重量百分比计，其具体组成为：
Figure PCTCN2018084596-appb-000001
所述的脂溶性营养素微胶囊中保持活性的脂溶性营养素与初始添加的脂溶性营养素的比值为0.990-0.997:1。所述的微胶囊中保持活性的脂溶性营养素与初始添加的脂溶性营养素的比值在下文中简称为活性物质的 保留率，可以说明在制备过程中脂溶性营养素的损失大小。
本发明还提供了该脂溶性营养素微胶囊的制备方法，将包含脂溶性芯材的熔融脂溶性营养素油相或预分散体和包含水溶性壁材的水相混合或者分别在高压下通入多级串联空化乳化器中进行乳化或分散，得到的乳化液或分散液进行喷雾造粒、干燥，即得到脂溶性营养素微胶囊。
同现有技术相比，本发明的有益效果如下：
1)本发明所述的脂溶性营养素微胶囊直接以脂溶性营养素熔油或预分散体为油相，不需要添加额外的油脂或者有机溶剂，且微胶囊包埋的有效脂溶性营养素在制备过程中损失小，活性物质的保留率高。
2)本发明所述的脂溶性营养素微胶囊的制备方法采用了连续多级串联空化乳化或分散方法，大幅减少了乳化或分散时间，有效减少了乳化或分散过程中脂溶性营养素的变质；同时，该乳化或分散方法制备得到的乳液或分散液稳定性好，最终得到的微胶囊包埋率高，微胶囊表面基本无脂溶性营养素残留，制备的营养素微胶囊稳定性高。
3)本发明所述的脂溶性营养素微胶囊的制备方法能耗低、效率高。
4)本发明所述的脂溶性营养素微胶囊仅需添加少量的抗氧化剂，其中在不添加脂溶性抗氧化剂的情况下，也能保持活性物质的高保留率。
具体实施方式
本发明所述的脂溶性营养素为维生素A衍生物、维生素E衍生物、维生素D、类胡萝卜素、辅酶Q。作为优选，所述的脂溶性营养素为不稳定营养素，具体的可以为维生素A醋酸酯、维生素A棕榈酸脂、维生素E醋酸酯、维生素E棕榈酸脂、维生素D2、维生素D3、β-胡萝卜素、虾青素、番茄红素、斑蝥黄、叶黄素、辅酶Q10中的一种。
本发明所述的抗氧化剂为没食子酸丙酯、BHT、茶多酚、α-生育酚、L-抗坏血酸-6-棕榈酸酯、茶多酚棕榈酸酯、抗坏血酸钠、抗坏血酸、硫代二丙酸二月桂酯、硫辛酸中的一种或多种。作为优选的，所述的抗氧化剂为水溶性抗氧化剂，可以为抗坏血酸、抗坏血酸钠、异抗坏血酸、异抗坏血酸钠中的一种或多种。选择水溶性抗氧化剂，有利于降低乳化或分散过程中油相的数量，提高微胶囊包埋率，降低裸露在微胶囊表层的油相量，提高喷雾造粒、干燥阶段脂溶性营养素的稳定性。
本发明所述的壁材为水溶性胶体和碳水化合物。所述的水溶性胶体为明胶、阿拉伯胶、可凝胶化的改性淀粉、辛烯基琥珀酸淀粉酯中的一种或多种。所述的碳水化合物为糊精、葡萄糖、白砂糖、果糖、麦芽糖、纤维糖、玉米淀粉中的一种或多种。
本发明还提供了上述脂溶性营养素微胶囊的制备方法，将包含脂溶性芯材的熔融脂溶性营养素油相或预分散体和包含水溶性壁材的水相混合或者分别在高压下通入多级串联空化乳化器中进行乳化或分散，得到的乳化液或分散液进行喷雾造粒、干燥，即得到脂溶性营养素微胶囊。所述的熔融脂溶性营养素油相是指，在高于脂溶性营养素熔点温度下，得到的脂溶性营养素的液态油相。所述的脂溶性营养素的预分散体是指，将脂溶性营养素投入水中，通过研磨等手段使其均匀分散得到的营养素固体悬浮液。
上述的多级串联空化乳化器是指将多个带有突变的收缩—扩张截面的空化乳化器进行串联使用的乳化器。所述的空化乳化器由相互连通的收缩段和扩张段组成，每一级乳化器中，流体先经过收缩段，再进入扩张段。所述的空化乳化器中，收缩段的出口和扩张段的出口在收缩段的出口方向上不全部和不部分重叠。所述的收缩段内径突变的减小(且不闭合)，流体在收缩段内产生明显高于收缩段入口处的高速，且在收缩段和扩张段的连接处达到最大值。流体在高速下碰撞扩张段的壁面，产生空化现象，从而达到乳化或分散效果。所述的多级串联空化乳化器为3级及以上的串联空化乳化器。本发明中，所述的多级串联空化乳化器是根据脂溶性营养素的物性，尤其是脂溶性营养素的熔融油或预分散体及水溶性壁材溶液的粘度来进行选择。作为优选的，所述的多级串联空化乳化器为5-10级的串联空化乳化器。
在本发明中，通过使流体在高压下，高速通过多级串联空化乳化器，在极短时间内即可完成均质乳化或分散。所述的高压压力为100-500MPa。在所述高压下，流体在空化乳化器的收缩段出口速度达到最大值，并撞击在扩张段壁面上，由此来形成多次的空化乳化或分散，能在短时间内，一次性完成乳化或分散。
上述的油相为熔融的脂溶性营养素或预分散体，不添加额外的油脂或有机溶剂。在微胶囊制备过程中，与外环境接触的脂溶性营养素表面小， 再结合上述的乳化或分散方法，制得的微胶囊包埋的活性成分高，制备过程中活性成分几乎无损失。
上述的制备方法可在氮气保护下进行。使用氮气保护，可以排除环境中氧对营养素的影响，保证在微胶囊制备过程中脂溶性营养素的稳定性。
上述水相中所用的水可预先进行脱氧处理，进一步排除环境中氧的影响，提高微胶囊制备过程中脂溶性营养素的稳定性。所述的水相中，亲水性壁材和水的质量比为0.5-1:1。
上述的干燥工艺可以为喷雾干燥、喷雾造粒-流态化干燥等。
以下采用具体实施例的方式进一步详细地说明本发明，然而，本发明不限于以下所述的实施例。
实施例一
维生素A微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000002
准确称取维生素A醋酸酯结晶360Kg，投入熔油釜中，升温使物料全部熔化得到融油；放饮用水1000L到配料釜中，再投明胶300Kg、葡萄糖100Kg、维生素C 20Kg、糊精110Kg，升温搅拌溶解，得到水溶胶溶液。用泵分别将上述熔油釜中融油、配料釜中水溶胶溶液用高压泵泵入5级串联空化乳化器中，调整压力为400Mpa，进行连续乳化，在出口处得到维生素A醋酸酯乳液，将该乳液连续通入喷有玉米淀粉的喷雾造粒塔中造粒，再经流态化干燥，得到维生素A醋酸酯微粒，测定各组分的含量如表1所示，计算生产过程中维生素A醋酸酯保留率为99.7％。将维生素A醋酸酯微粒放置于25℃条件下进行稳定性试验，通过6个月后检测微粒中维生素A醋酸酯含量，可计算得到6个月后维生素A醋酸酯的保留率为98.2％。
实施例二
维生素D3微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000003
把维生素D3油55Kg打入熔油釜中，向釜中加入BHT 5Kg，升温使物料全部熔化得到融油；放饮用水980L到配料釜中，再投入白砂糖200Kg、明胶150Kg、糊精630Kg，升温搅拌溶解，得到水溶胶溶液。用泵分别将上述熔油釜中融油、配料釜中水溶胶溶液用高压泵泵入4级串联空化乳化器中，调整压力为200Mpa，进行连续乳化，在出口处得到维生素D3乳液，将该乳液连续通入喷雾干燥塔中进行喷雾干燥，得到维生素D3干粉，测定各组分的含量如表1所示，计算生产过程中维生素D3的保留率为99.2％。将维生素D3干粉放置于25℃条件下进行稳定性试验，通过6个月后检测维生素D3干粉中维生素D3的含量，可计算得到6个月后维生素D3的保留率为98.5％。
实施例三
叶黄素微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000004
将叶黄素结晶5.3Kg、水30Kg投入球磨机中研磨至5μm以下，得到预分散体；放饮用水1050L到配料釜中，再投辛烯基琥珀酸淀粉钠190Kg、葡萄糖60Kg、糊精250Kg、VC钠5Kg，升温搅拌溶解得到水溶胶溶液；将上述预分散体与水溶胶溶液在搅拌下混合均匀，得到分散液。用高压泵 将上述分散液泵入6级串联空化乳化器中，调整设备压力为500Mpa，进行连续分散，在出口处得到叶黄素分散液，将叶黄素分散液连续通入喷雾干燥塔中进行喷雾干燥，得到叶黄素干粉，测定各组分的含量如表1所示，计算生产过程中叶黄素保留率为99.6％。将叶黄素干粉放置于25℃条件下进行稳定性试验，通过6个月后检测叶黄素干粉中叶黄素的含量，可计算得到6个月后叶黄素的保留率为99.2％。
对比例一
维生素A微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000005
准确称取生育酚20Kg，投入熔油釜中，再投入维生素A醋酸酯结晶360Kg，升温使物料全部熔化得到融油；放饮用水1000L到乳化釜中，再投明胶300Kg、葡萄糖100Kg、糊精110Kg，升温搅拌溶解，得到水溶胶溶液。将熔油釜中维生素A醋酸酯融油滴加到乳化釜中，高速剪切20min，得到乳化液。将上述乳化液通入喷有玉米淀粉的喷雾造粒塔中造粒，再流态化干燥，得到维生素A醋酸酯微粒，测定各组分的含量如表1所示，计算生产过程中维生素A醋酸酯保留率为94.2％。将维生素A放置于25℃条件下进行稳定性试验，通过6个月后检测维生素A醋酸酯微粒中维生素A醋酸酯的含量，可计算得到6个月后维生素A醋酸酯的保留率为88.1％。
对比例二
维生素D3微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000006
Figure PCTCN2018084596-appb-000007
把维生素D3油55Kg打入熔油釜中，向釜中加入BHT 5Kg，升温使物料全部熔化得到融油；放饮用水980L到乳化釜中，再投入白砂糖200Kg、明胶150Kg、糊精630Kg，升温搅拌溶解，得到水溶胶溶液。将上述维生素D3融油滴加到乳化釜中，高速剪切20min得到乳化液。将乳化液通入喷雾干燥塔中进行喷雾干燥，得到维生素D3干粉，测定各组分的含量如表1所示，计算生产过程中维生素D3保留率为96.5％。将上述维生素D3干粉放置于25℃条件下进行稳定性试验，通过6个月后检测维生素D3干粉中维生素D3的含量，可计算得到6个月后维生素D3的保留率为93.5％。
对比例三
叶黄素微胶囊及其制备
组分：
Figure PCTCN2018084596-appb-000008
将生育酚5Kg投入熔油釜中，再投入叶黄素结晶5.3Kg，升温至180℃使物料全部熔化，然后降温至90℃，得到融油；放饮用水1050L到乳化釜中，再投可凝胶化的改性淀粉190Kg、果糖60Kg、糊精250Kg，升温搅拌溶解得到水溶胶溶液。将上述叶黄素融油滴加到乳化釜中，高速剪切20min得到乳化液。将叶黄素乳液通入喷雾干燥塔中进行喷雾干燥，得到叶黄素干粉，测定各组分的含量如表1所示，计算生产过程中叶黄素保留率为75.6％。将叶黄素干粉放置于25℃条件下进行稳定性试验，通过6个月后检测叶黄素干粉中叶黄素的含量，可计算得到6个月后叶黄素的保留率为72.2％。
实施例四～十
组分配比和空化乳化器级数及压力按照表1，制备流程按照实施例二(实施例四、五、十)或实施例三(实施例六、七、八、九)，得到不同的营养素微胶囊，测定各组分的含量，计算其营养素的保留率和稳定性，结果见表1。
表1 不同配方营养素微胶囊在生产过程及25℃储存6个月后的保留率
Figure PCTCN2018084596-appb-000009
Figure PCTCN2018084596-appb-000010

Claims (10)

  1. 一种脂溶性营养素微胶囊，其特征在于，以重量百分比计，组成为：
    Figure PCTCN2018084596-appb-100001
    所述的脂溶性营养素微胶囊中保持活性的脂溶性营养素与初始添加的脂溶性营养素的比值为0.990-0.997:1。
  2. 根据权利要求1所述的脂溶性营养素微胶囊，其特征在于，所述的脂溶性营养素为维生素A衍生物、维生素E衍生物、维生素D、类胡萝卜素、辅酶Q 10中的一种或多种。
  3. 根据权利要求2所述的脂溶性营养素微胶囊，其特征在于，所述的脂溶性营养素为维生素A醋酸酯、维生素A棕榈酸脂、维生素E醋酸酯、维生素E棕榈酸脂、维生素D2、维生素D3、β-胡萝卜素、虾青素、番茄红素、斑蝥黄、叶黄素、辅酶Q 10中的一种或多种。
  4. 根据权利要求1所述的脂溶性营养素微胶囊，其特征在于，所述的抗氧化剂为没食子酸丙酯、BHT、茶多酚、α-生育酚、L-抗坏血酸-6-棕榈酸酯、茶多酚棕榈酸酯、抗坏血酸钠、抗坏血酸、硫代二丙酸二月桂酯、硫辛酸中的一种或多种；作为优选，所述的抗氧化剂为水溶性抗氧化剂，包含抗坏血酸、抗坏血酸钠、异抗坏血酸、异抗坏血酸钠中的一种或多种。
  5. 根据权利要求1所述的脂溶性营养素微胶囊，其特征在于，所述的壁材为水溶性胶体和碳水化合物。
  6. 根据权利要求5所述的脂溶性营养素微胶囊，其特征在于，所述的水溶性胶体为明胶、阿拉伯胶、可凝胶化的改性淀粉、辛烯基琥珀酸淀粉酯中的一种或多种；
    所述的碳水化合物为糊精、葡萄糖、白砂糖、果糖、麦芽糖、纤维糖、玉米淀粉中的一种或多种。
  7. 一种如权利要求1～6任一项所述的脂溶性营养素微胶囊的制备方 法，其特征在于，包括：将包含脂溶性芯材的熔融脂溶性营养素油相或预分散体和包含水溶性壁材的水相混合或者分别在高压下通入多级串联空化乳化器中进行乳化或分散，得到的乳化液或分散液进行喷雾造粒、干燥，即得到脂溶性营养素微胶囊。
  8. 根据权利要求7所述的脂溶性营养素微胶囊的制备方法，其特征在于，所述的多级串联空化乳化器为3级以上的串联空化乳化器；优选的，所述的多级串联空化乳化器为5-10级的串联空化乳化器。
  9. 根据权利要求7所述的脂溶性营养素微胶囊的制备方法，其特征在于，每一级空化乳化器由相互连通的收缩段和扩张段组成，收缩段的出口与扩张段的出口在收缩段的出口方向上不全部和不部分重叠。
  10. 根据权利要求7所述的脂溶性营养素微胶囊的制备方法，其特征在于，所述的高压压力为100-500Mpa。
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