A composition, its preparation and use

Abstract

The present application belongs to the technical field of food or medicine, and provides a composition, a preparation method and application thereof, the composition comprising oil, phospholipid and nutritional ingredients, wherein the beta crystal form accounts for 50% to 90% in the fat crystal formed by the oil, the average diameter of the fat crystal aggregate is 10 to 100 mu m, and the content of phosphatidylcholine in the phospholipid is 10 wt% to 55 wt%. The composition has good dispersion effect and high flowability, and has low production difficulty, low oil leakage rate and stable nutritional ingredient content when being made into soft capsules or gummy candies.

Description

Technical Field

[0001] This invention relates to the field of food or pharmaceutical technology, and in particular to a composition, its preparation method, and its application. Background Technology

[0002] Many functional factors in food, such as probiotics, polyphenols, flavonoids, and vitamins, are easily affected by the environment, resulting in structural changes and reduced efficacy. The mechanisms of structural changes mainly include the following aspects: (1) Microphase separation: Hydrogen bonding causes changes in the conformation of molecular chains, leading to exposure of active sites (such as isomerization of polyphenol quinone structures); (2) Interfacial inactivation: Water molecule penetration causes functional factors to expand and break down (such as a decrease in the survival rate of probiotics > 2 log CFU / g); (3) Oxidative degradation: Water-mediated free radical chain reactions accelerate the loss of photosensitive components such as vitamin C (half-life shortened by 50%~70%).

[0003] To prevent changes in the structure of functional factors, the commonly used solution is to construct an oil-based core-shell delivery system to protect the functional factors: (1) Core layer structure: Disperse the solid functional factors in an oil carrier and use hydrophobic interactions to inhibit water molecule penetration; (2) Shell engineering: Through ionic crosslinking (such as sodium alginate-Ca... 2+ A dense barrier layer with a thickness of 50~200μm can be constructed by thermo-induced gelation (such as colloidal technology) or interfacial polymerization (W / O / W emulsion).

[0004] However, oil-based core-shell delivery systems also face some challenges, the most significant being the technical limitations caused by density gradients. During core layer construction, due to the density difference between the functional components and the oil phase, there is a significant difference in sedimentation coefficient (Δρ≥0.3 g / cm³). 3 ), which can easily lead to: (1) Stokes sedimentation: Powder with larger particle size settles quickly in the oil phase in a short time; (2) Marangoni convection: The tension gradient of the oil-solid interface induces eddies, causing local aggregation of functional factors (CV value > 15%), increasing the difficulty of production, such as affecting the pelleting effect of soft capsules, which can easily lead to poor sealing of the capsule seams and cause quality problems such as leakage; (3) Loading volume fluctuation: The uneven dispersion during the filling process causes the single-agent functional factor content deviation > ±20% (exceeding the maximum ±10% limit of the 2025 edition of the Chinese Pharmacopoeia).

[0005] To address the aforementioned issues, related technologies employ suspending agents such as phospholipids and mono- and diglycerides to suspend active ingredients like probiotic powder, followed by grinding and shearing processes to prepare soft capsule contents. The particle size of the contents is controlled by adjusting grinding or homogenization parameters to prevent solid-oil phase stratification and sedimentation. Alternatively, suspending agents and specific suspension processes are used to increase the viscosity of the contents, preventing the sedimentation of solid powder in the oil phase. The core technology of these solutions is the use of suspending agents or thickeners to increase the viscosity of the suspension for a suspending effect. However, in practical applications, simply increasing viscosity usually fails to maintain uniform dispersion throughout the product's shelf life. Over time, powder often settles, ultimately reducing powder retention. Furthermore, increased viscosity restricts the fluidity of the suspension, hindering material flow, increasing the difficulty of producing pressed products, and increasing the risk of oil leakage from gaps. It is also detrimental to the production of drip-type products, potentially causing issues such as inability to drip, capsule breakage, irregular capsule formation, or tailing. Summary of the Invention

[0006] The present invention aims to at least solve one of the aforementioned technical problems existing in the prior art. Therefore, the object of the present invention is to provide a composition, a method for preparing the same, and its application.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0008] In a first aspect, the present invention provides a composition comprising oils, phospholipids and nutrients, wherein, by mass percentage of the composition, the β-crystal form of the fat crystals formed by the oils accounts for 50% to 90%, the average diameter of the fat crystal aggregates is 10 to 100 μm, and the phospholipids contain 10 wt% to 55 wt% of phosphatidylcholine.

[0009] In some embodiments, the oil is a semi-solid to solid processed oil; the composition comprises 0.1-0.5% phospholipids, 69-99% processed oil, and 1-30% nutrients by mass percentage; the mass ratio of phospholipids to processed oil is 1:150-1000.

[0010] In some embodiments, the oil is a combination of semi-solid to solid processed oil and liquid oil; the composition comprises 0.5-3.0% phospholipids, 5-30% processed oil, 50-90% liquid oil and 1-30% nutrients by mass percentage; the mass ratio of phospholipids to processed oil is 1:5-15.

[0011] In some embodiments, the liquid fats include edible animal fats, vegetable oils, and / or related products thereof.

[0012] In some embodiments, the semi-solid to solid processed fats include wax fats, higher fatty acid glycerides, palm oil extracts, edible hydrogenated oils, margarine, shortening, cocoa butter substitutes, vegetable fat cream, and powdered fats.

[0013] In some embodiments, the nutrients include at least one of plant extracts, animal extracts, protein, amino acids, probiotics, vitamins, fermented nutrients, chemically synthesized nutrients, functional sugars, food-medicine homologous substances, and minerals.

[0014] A second aspect of the present invention provides a method for preparing the composition of the first aspect of the present invention, comprising the following steps:

[0015] The oil is melted and mixed with phospholipids, and then nutrients are added to obtain the composition described above.

[0016] A third aspect of the present invention provides a soft capsule or gel candy comprising a shell and a core, the core comprising the composition of the first aspect of the present invention.

[0017] A fourth aspect of the present invention provides a method for preparing soft capsules or gel candies according to the third aspect of the present invention, comprising the following steps:

[0018] The capsule core is injected into the capsule shell and then pressed or dripped into soft capsules or gel candies.

[0019] A fifth aspect of the invention provides the use of the composition of the first aspect of the invention or the soft capsule or gel candy of the third aspect of the invention in food, health food, pharmaceutical or cosmetic.

[0020] The beneficial effects of this invention are:

[0021] The composition of the present invention has good dispersion effect and high fluidity, resulting in low oil leakage rate and stable nutrient content in soft capsules or gel candies, and the production of soft capsules or gel candies is easy.

[0022] The preparation method of the composition of the present invention is simple and suitable for industrial production. Attached Figure Description

[0023] Figure 1 This is the XRD pattern of Example 12.

[0024] Figure 2 The image shows a microscope image (left) and a size distribution diagram (right) of the crystal aggregates in Example 12. Detailed Implementation

[0025] The present invention will be further described in detail below through specific embodiments. Unless otherwise specified, the raw materials, reagents, or apparatus used in the embodiments and comparative examples are all available from conventional commercial sources or can be obtained by existing technical methods. Unless otherwise specified, the test or experimental methods are conventional methods in the art.

[0026] In a first aspect, the present invention provides a composition comprising oils, phospholipids and nutrients, wherein, by mass percentage of the composition, the β-crystal form of the fat crystals formed by the oils accounts for 50% to 90%, the average diameter of the fat crystal aggregates is 10 to 100 μm, and the phospholipids contain 10 wt% to 55 wt% of phosphatidylcholine.

[0027] In some embodiments, the composition comprises composition one (excluding liquid oils) and composition two (containing liquid oils). Composition one (excluding liquid oils) comprises, by weight percentage, 0.1–0.5% phospholipids, 69–99% processed oils, and 1%–30% nutrients; the ratio of phospholipids to processed oils is 1:150–1000. The phospholipids contain 10 wt%–55 wt% phosphatidylcholine.

[0028] The second composition (containing liquid oil) comprises 0.5-3.0% phospholipids, 5-30% processed oils, 50-90% liquid oils, and 1-30% nutrients; the ratio of phospholipids to processed oils is 1:5-15. The phospholipids contain 10wt%-55wt% phosphatidylcholine.

[0029] Processed fats crystallize to form fat crystals (β-type, β'-type). In the composition of this invention, the phosphatidylcholines (PC) in the phospholipids have hydrophobic interactions and hydrogen bonds with the fatty chains and hydroxyl groups of processed fats, such as monoglycerides and cocoa butter substitutes. The phospholipids with the above-mentioned phosphatidylcholine content enable the processed fats to act as the dominant crystallizer, forming fat crystals with a predominantly tightly ordered β-type crystal, resulting in a moderate composition texture and improved fluidity. Controlling the mass ratio of phospholipids to processed fats can regulate the growth rate and nucleation rate of β-type fat crystals, thereby controlling the size of the three-dimensional network structure aggregates formed by the accumulation of fat crystals. The dynamically balanced crystal nucleation and growth rate ensures a moderate proportion of β-type nucleus formation and growth, resulting in a moderate size of the aggregated fat crystals. This provides a supporting framework for the dispersion of nutrients and improves the rheological properties of the composition, ensuring uniform dispersion of nutrients.

[0030] To further expand the application scope of the technology, a certain amount of liquid oil is added to the above composition. When unsaturated liquid oil is introduced, the regulatory effect of phospholipids on processed oils is significantly weakened, resulting in a decrease in the nucleation efficiency of β-crystals, a slowdown in the crystal nucleation rate, and an inability to form a dominant β-crystal network. In addition, abnormal proliferation of crystal aggregates and non-directional crystal growth lead to uncontrolled size distribution and structural collapse. Furthermore, the introduction of liquid oil dilutes the density of the fatty crystals in the composition, weakens the carrying capacity of the fatty crystals, and macroscopic defects manifest as dispersed phase instability (such as stratification), uneven distribution of nutrients, and decreased rheological properties.

[0031] The negative effects of liquid oils can be offset by the following strategies: First, increasing the phospholipid content of the aforementioned phosphatidylcholine-containing compounds enhances the supramolecular association ability between phospholipids and processed oils, preferentially forming stable spatial conformations. Second, optimizing the mass ratio of phospholipids to processed oils allows for precise control of the nucleation rate (preferential nucleation) and growth rate (size control) of the β-crystal form, maintaining a suitable size distribution of crystal aggregates. Based on these strategies, the rheological properties of the contents of the liquid oil system are significantly improved, and nutrients are uniformly dispersed.

[0032] In some embodiments, the proportion of β-type crystals in the adipose crystals is 50% to 90%, such as 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, etc. In this invention, X-ray diffractometer is used to test the crystal form of the adipose crystals, and the proportion of β-type crystals is calculated as: (integrated area of ​​β-type crystals / sum of integrated areas of β-type and β'-type crystals) × 100%. In this invention, if the proportion of β-crystal form in the fat crystals is too high, the network structure formed by the accumulation of fat crystals will be brittle and prone to cracking and collapse when carrying nutrients; if the proportion of β-crystal form in the fat crystals is too low, the network structure formed by the accumulation of fat crystals will lack rigidity and will be prone to structural changes when carrying functional powders, affecting the dispersion effect.

[0033] In some embodiments, the fat crystals aggregate to form fat crystal aggregates; the average diameter of the fat crystal aggregates is 10~100μm, such as 10μm, 15μm, 20µm, 25µm, 30µm, 35µm, 40µm, 45µm, 50µm, 55µm, 60µm, 65µm, 70µm, 75µm, 80µm, 85µm, 90µm, 95µm, 100µm, etc. In this invention, the average diameter of the fat crystal aggregates is obtained by polarized light microscopy, with at least 20 fat crystals tested for each sample, and the average value is taken. In this invention, when the average diameter of the fat crystal aggregates is too small, crystal nucleation is intensified, crystal growth is limited, the structure tends to be microcrystalline or disordered, and the nutrient components are unevenly dispersed and unstable; when the average diameter of the fat crystal aggregates is too large, crystal nucleation is inhibited, crystal growth is rapid, resulting in the lack of crystalline structure in some positions, and the nutrient components cannot be fully supported in the system, affecting its dispersibility and stability.

[0034] In some embodiments, the phospholipid contains 10wt% to 55wt% phosphatidylcholine, such as 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, and 55%. In this invention, if the phosphatidylcholine content in the phospholipid is too low, the interaction between the linear structure in the processed oil and the phosphoric acid choline-containing group of phosphatidylcholine is weakened, resulting in a low content of β crystals, a low density of the crystal structure, and insufficient carrying capacity of the liquid for solid powder, which is not conducive to the uniform dispersion of nutrients in the system. If the phosphatidylcholine content in the phospholipid is too high, the content of the β crystal-type fat crystals formed by regulation is too high, the texture of the composition is hard and brittle, the fluidity is significantly reduced, which is not conducive to formulation.

[0035] In some embodiments, the nutrient content, by mass percentage, that enables the achievement of the present invention is 1% to 30%, such as 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, etc. In this invention, when the proportion of nutrient content is too high, its density in the oil phase is too high, hindering the interaction of fat crystal nuclei, making crystal growth difficult, and preventing the formation of a three-dimensional network gel structure. This results in a solid-liquid stratification phenomenon, with nutrient components agglomerating in the oil phase, leading to an uneven system.

[0036] In some embodiments, the processed oil that enables the present invention to be realized by weight percentage is 69-99%, such as 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, 91%, 92%, 93%, 94%, 95%, 96%, 97%, 98%, 99%, etc.

[0037] In some embodiments of composition one (excluding liquid oils), the phospholipids are present in a mass ratio of 1:1 to the processed oils. (150~1000), such as 1:150, 1:175, 1:200, 1:225, 1:250, 1:275, 1:300, 1:325, 1:350, 1:375, 1:400, 1:425, 1:450, 1:475, 1:500, 1:525, 1:550, 1:575, 1:600, 1:625, 1:650, 1:675, 1:700, 1:725, 1:750, 1:775, 1:800, 1:825, 1:850, 1:875, 1:900, 1:925, 1:950, 1:975, 1:1000, etc. In this invention, phospholipids regulate the growth and nucleation rate of β-crystalline fatty acid crystals. When the proportion of phospholipids is too high, it easily leads to excessively high nucleus density, hindering nucleus growth space and resulting in poor fluidity of the composition. This makes it difficult to evenly disperse nutrients, making it difficult to form soft capsules and causing a high oil leakage rate. When the proportion of phospholipids is too low, the nucleation and growth rates become unbalanced, inhibiting the formation of β-crystalline fatty acid crystals, increasing the crystal growth rate, reducing the number of nuclei per unit volume, and increasing the crystal size. This results in significantly weaker structural rigidity of the oil phase, macroscopically manifesting as uneven solid-liquid dispersion or even stratification. This easily leads to oil leakage when the composition is formed into soft capsules.

[0038] Composition 2 (containing liquid grease), in some embodiments, the processed grease capable of achieving the purpose of the present invention is 5-30% by mass percentage, such as 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, etc.

[0039] In Composition Two (containing liquid oil), in some embodiments, the phospholipid to processed oil mass ratio is 1:(5~15), such as 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:11, 1:12, 1:13, 1:14, 1:15, etc. In this invention, the ratio of phospholipid to processed oil is a key parameter for controlling the β-crystal content and fat aggregate size of the system. When the phospholipid ratio is too high, the interaction between the two is too strong, the β-crystal density is high, and the fluidity of the liquid is weakened, which is not conducive to soft capsule formation. When the phospholipid ratio is too low, the interaction between the two is weakened, the β-crystal density is low, the carrying capacity of the liquid is weak, and the nutrients cannot be evenly dispersed.

[0040] Composition 2 (containing liquid oil), in some embodiments, comprises, by weight percentage, 50% to 90% of the liquid oil capable of achieving the purpose of this invention, such as 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%, etc. In this invention, the liquid oil affects the regulatory effect of phospholipids on processed oils. When the proportion of liquid oil in the system is too high, it hinders the molecular interaction between phospholipids and processed oils, which is not conducive to the formation of β crystals. At the same time, it dilutes the structural density of fat crystals in the system, resulting in fewer crystal nuclei and significantly weaker cohesive forces of the crystal nuclei. The composition exhibits a flexible structure and macroscopically shows a tendency for solid-liquid phase separation. When the proportion of liquid oil is too low, the number of processed oil crystal nuclei in the system is high at the beginning. The crystal growth space per unit volume is limited, resulting in dense accumulation of crystal nuclei. Macroscopically, it shows a rapid solidification state, poor fluidity of the composition, high viscosity of the system, and difficulty in dispersing nutrients in the system, causing nutrients to agglomerate in local areas.

[0041] In some embodiments, the liquid oils include edible animal oils, vegetable oils, and / or related products thereof; the animal oils include fish oil, cod liver oil, etc.; the vegetable oils include soybean oil, corn oil, sunflower seed oil, peanut oil, flaxseed oil, safflower seed oil, perilla oil, maple seed oil, walnut oil, rapeseed oil, wheat germ oil, pumpkin seed oil, coconut oil (containing medium-chain triglycerides MCT), cocoa butter, sea buckthorn fruit oil, grape seed oil, rice bran oil, borage oil, hemp seed oil, palm oil, olive oil, camellia seed oil, wolfberry oil, palm kernel oil, algae oil, and at least one of medium-chain triglycerides MCT; the edible animal oil and vegetable oil related products are obtained by further separation, extraction, concentration, esterification, hydrogenation, and other related processes from edible animal oils and vegetable oils, and the edible animal oil and vegetable oil related products include at least one of palm oil extract, concentrated fish oil, ethyl ester type fish oil, and rTG fish oil.

[0042] In some embodiments, the semi-solid to solid processed fats include wax fats, higher fatty acid glycerides, palm oil extracts, edible hydrogenated oils, margarine, shortening, cocoa butter substitutes (including cocoa butter substitutes), vegetable fat cream, and powdered fats.

[0043] In some embodiments, the higher fatty acid glycerides include glyceryl monostearate, glyceryl distearate, and / or mixtures thereof formed by reacting higher fatty acids and glycerol; the higher fatty acids include at least one of oleic acid, linoleic acid, linolenic acid, palmitic acid, behenic acid, stearic acid, and lauric acid.

[0044] In some embodiments, the phospholipids include at least one of soybean phospholipids, sunflower phospholipids, and egg yolk phospholipids.

[0045] In some embodiments, the nutrients include liquid nutrients and / or solid nutrients.

[0046] In some embodiments, the solid nutrient component includes nutrient powder. In this invention, compared to liquid nutrient components, nutrient powder has a higher true density (e.g., higher than liquid oils), making it difficult to disperse or load effectively, and placing higher demands on the delivery system.

[0047] In some embodiments, the nutrients include at least one of plant extracts, animal extracts, protein, amino acids, probiotics, vitamins, fermented nutrients, chemically synthesized nutrients, functional sugars, food-medicine homologous substances, and minerals.

[0048] In some embodiments, the plant extract nutrients include blueberry anthocyanins, Dunaliella salina and its extract, inulin, Haematococcus pluvialis powder, Haematococcus pluvialis oil, earthworm protein, mushroom concentrate powder, lychee enzyme, brown algae powder, citrus fruit powder, dried tangerine peel powder, white kidney bean powder, green tea powder, cherry fruit powder, vine tea powder, platycodon powder, corn oligopeptide powder, epigallocatechin gallate, wheat oligopeptide, snow lotus culture, maca powder, ginseng extract, Chlorella vulgaris powder, cordyceps powder, Euglena rubescens powder, chia seed powder, Psyllium lappa husk powder, Cordyceps militaris powder, fruit and vegetable powder, tea theanine, bamboo leaf flavonoids, loquat leaf powder, basil powder, broccoli seed water extract, Nostoc commune powder, Ashitaba juice powder, loquat flower powder, ginseng powder, quercetin, potato extract, and other related ingredients. The following is a list of at least one of the following: Chlorophytum comosum powder, Chlamydomonas reinhardtii powder, sugarcane polyphenols, rye pollen, Xanthoceras sorbifolium seed kernel powder, Xanthoceras sorbifolium leaf powder, Gynostemma pentaphyllum, catechins, phosphatidylserine, broken-cell wall Ganoderma lucidum spore powder, spirulina powder, Isatis indigotica root powder, Viola yedoensis powder, guarana extract, Chinese cinnamon bark tincture extract, bergamot extract, Alpinia galanga root extract, seaweed extract, yellow mustard extract, alfalfa extract, basil extract, celery seed extract, bay leaf extract, lemon extract, sweet orange peel extract, elderberry flower extract, bay leaf extract, enzyme-treated isoquercitrin, grape seed extract, spearmint extract, Zanthoxylum bungeanum extract, catechin powder, wormwood extract, Juniperus chinensis extract, licorice extract, annatto extract, ginger extract, kola nut extract, and Rhodiola rosea extract.

[0049] In some embodiments, the animal extract nutrients include at least one of hydrolyzed egg yolk powder, whey powder, pearl peptide powder, yeast powder containing SOD, and clam polysaccharide.

[0050] In some embodiments, the protein nutrients include at least one of colostrum basic protein, milk basic protein, lactoferrin, casein, whey protein isolate, yeast protein, collagen powder, and collagen peptides.

[0051] In some embodiments, the collagen powder includes cartilage powder containing type II collagen.

[0052] In some embodiments, the amino acid nutrients include at least one of glycine, alanine, valine, leucine, isoleucine, methionine, proline, tryptophan, serine, tyrosine, cysteine, phenylalanine, asparagine, glutamine, threonine, aspartic acid, glutamic acid, arginine, histidine, selenocysteine, and lysine.

[0053] In some embodiments, the probiotic nutrients include probiotic powder, such as inactivated probiotic powder.

[0054] In some embodiments, the vitamin nutrients include at least one of vitamin B1, vitamin B2, vitamin B3 and its derivatives, vitamin B5, vitamin B6, vitamin B12, vitamin C, vitamin K1, vitamin K2, folic acid, biotin, and inositol.

[0055] In some embodiments, the fermented nutrients include at least one of coenzyme Q10, sodium hyaluronate, γ-aminobutyric acid, and human milk oligosaccharides.

[0056] In some embodiments, the chemically synthesized nutrient includes at least one of melatonin, N-acetylneuraminic acid, cis-15-tetracosenoic acid, disodium pyrroloquinoline quinone, choline, and para-aminobenzoic acid.

[0057] In some embodiments, the functional sugar includes at least one of galactooligosaccharides, fructooligosaccharides, cottonseed oligosaccharides, yeast glucan, mannose oligosaccharides, chitosan oligosaccharides, and L-arabinose.

[0058] In some embodiments, the medicinal and edible substances include at least one of the following: sea buckthorn, amla, mulberry leaf, chicken gizzard lining, Solomon's seal, licorice, angelica, ginkgo, yam, hawthorn, cassia seed, lily, kelp, monk fruit, honeysuckle, houttuynia cordata, Japanese raisin tree fruit, wolfberry, gardenia, amomum villosum, sterculia lychnophora, poria cocos, citron, mulberry leaf, lotus seed, dandelion, jujube seed, chrysanthemum, chicory, perilla, perilla seed, kudzu root, black sesame, tangerine peel, mint, raspberry, patchouli, angelica sinensis, galangal, saffron, cardamom, turmeric, long pepper, codonopsis, cistanche deserticola, dendrobium officinale, American ginseng, astragalus, ganoderma lucidum, cornus officinalis, gastrodia elata, and eucommia ulmoides leaf.

[0059] In some embodiments, the composition further includes a flavoring agent; the flavoring agent includes at least one of a sweetener, an acidity regulator, a flavoring, a fragrance, and a fruit powder.

[0060] In some embodiments, the sweetener includes at least one of neotame, granulated sugar, caster sugar, brown sugar, sucrose, glucose, lactose, sorbitol, sucralose, aspartame, alitame, sodium saccharin, acesulfame potassium, allulose, advansat, cyclamate, sematrandezine, steviol glycosides, mogrosides, isomaltulose, ammonium glycyrrhizate, monopotassium and tripotassium glycyrrhizate, D-mannitol, xylitol, erythritol, maltitol, and lactitol.

[0061] In some embodiments, the acidity regulator includes at least one of fumaric acid, metatartaric acid, citric acid, lactic acid, malic acid, tartaric acid, acetic acid, adipic acid, monosodium fumarate, sodium citrate, potassium citrate, monosodium citrate, phosphate, calcium sulfate, calcium lactate, sodium acetate, calcium hydroxide, potassium hydroxide, and sodium hydroxide.

[0062] A second aspect of the present invention provides a method for preparing the composition of the first aspect of the present invention, comprising the following steps:

[0063] The oil is melted and mixed with phospholipids, and then nutrients are added to obtain the composition described above.

[0064] In some embodiments, the preparation method of the composition includes the following steps: melting a semi-solid to solid processing oil and mixing it with phospholipids and optionally liquid oils, and then adding nutrients to obtain the composition.

[0065] In some embodiments, the processed grease is heated to melt it. Different processed greases have different melting temperatures, and those skilled in the art can adjust the heating temperature and time according to the actual melting temperature of the processed grease to bring it to a molten state.

[0066] A third aspect of the present invention provides a soft capsule or gel candy comprising a shell and a core, the core comprising the composition of the first aspect of the present invention.

[0067] In some embodiments, the core is a single-layer or double-layer structure.

[0068] In some embodiments, the core has a two-layer structure, including an intermediate protective layer and a core layer.

[0069] In some embodiments, the intermediate protective layer comprises the semi-solid to solid processing grease.

[0070] In some embodiments, the core layer includes the semi-solid to solid processed oils, phospholipids, optional liquid oils, and nutrients.

[0071] In some embodiments, the soft capsule or gel candy has a two- or three-layer structure.

[0072] In some embodiments, the mass ratio of the shell to the core is (5~50):(50~95), such as 5:95, 10:90, 20:80, 30:70, 40:60, 50:50, etc.

[0073] In some embodiments, the capsule shell includes a gelling agent, a moisture-retaining agent, and optionally, a flavoring agent, a coloring agent, or other edible additives.

[0074] In some embodiments, the capsule shell comprises 20 to 120 parts by weight of a gelling agent and 10 to 40 parts by weight of a moisture-retaining agent, as well as optionally 0.1 to 10 parts by weight of a flavoring agent and 0.1 to 10 parts by weight of a coloring agent.

[0075] In some embodiments, the gelling agent includes at least one of gelatin, agar, gellan gum, starch, fenugreek gum, carrageenan, xanthan gum, locust bean gum, sodium alginate, konjac gum, pectin, gum arabic, and guar gum.

[0076] In some embodiments, the moisture-retaining agent is selected from at least one of glycerol, sorbitol, and maltitol.

[0077] In some embodiments, the flavoring agent includes at least one of granulated sugar, powdered sugar, brown sugar, sucrose, glucose, lactose, fructose syrup, maltose syrup, sorbitol, sucralose, aspartame, alitame, sodium saccharin, acesulfame potassium, allulose, advans, cyclamate, sematrandezine, steviol glycosides, mogrosides, isomaltulose, ammonium glycyrrhizate, monopotassium and tripotassium glycyrrhizate, D-mannitol, xylitol, erythritol, maltitol, and lactitol.

[0078] In some embodiments, the pigment includes at least one of titanium dioxide, Allura Red, Brilliant Blue, Tartrazine, Sunset Yellow, Cochineal, Turmeric, Natura Orange, Gardenia Yellow, Gardenia Blue, Safflower Yellow, Vegetable Carbon Black, Carotene, Sodium Copper Chloride, Apple Concentrate Extract, Caramel Color, Wheat Extract, Cocoa Shell Color, Capsicum Red, Beetroot Red, Phycocyanin, Butterfly Pea Flower, Corn Yellow, Catechu Black, Licorice Pigment, Hematoxylin, Roselle Red, Purple Sweet Potato Pigment, Purple Yam Pigment, Grape Skin Pigment, Lithospermum, and Phycoerythrin.

[0079] In some embodiments, the edible additives include at least one of plasticizers, preservatives, stabilizers, and solubilizers.

[0080] A fourth aspect of the present invention provides a method for preparing soft capsules or gel candies according to the third aspect of the present invention, comprising the following steps:

[0081] The capsule core is injected into the capsule shell and then pressed or dripped into soft capsules or gel candies.

[0082] In some embodiments, the pressing or dripping is carried out at an ambient temperature of 18-30°C and a relative humidity of 40%-80%.

[0083] In some embodiments, the preparation method of the capsule shell includes the following steps: heating a gelling agent, a moisture-retaining agent, an optional flavoring agent, a coloring agent and other edible additives, and purified water to 60-90°C and stirring until completely dissolved, removing air bubbles, and obtaining the capsule shell.

[0084] In some embodiments, when the core is a two-layer structure, the method for preparing the intermediate protective layer includes the following steps: melting a semi-solid to solid processing grease to obtain the intermediate protective layer.

[0085] In some embodiments, the preparation method of the soft capsules or gel candies further includes shaping and drying the soft capsules or gel candies; the shaping is carried out in a rotary drum; the drying is carried out under conditions of humidity of 45%~70% and temperature of 20~30°C; and the shells of the soft capsules or gel candies are dried to a moisture content of 7%~20%. In this invention, the moisture content of the shells is detected using a halogen-based rapid moisture analyzer.

[0086] A fifth aspect of the invention provides the use of the composition of the first aspect of the invention or the soft capsule or gel candy of the third aspect of the invention in food, health food, pharmaceutical or cosmetic.

[0087] In the following examples or comparative examples, the test methods for the content of each substance and the product performance are as follows:

[0088] Crystal form determination method: The crystal form and relative proportion of the samples were evaluated using an X-ray diffractometer (Ultima IV, Rigaku, Japan). Approximately 2 g of sample was placed on a glass slide at room temperature. Cu-K-α radiation (λ = 1.5405 Å) was used, with an operating voltage of 40 kV and a current of 40 mA; the diffraction angle (2θ) ranged from 10° to 35°, and the scan rate was set to 2° / min. Data processing was performed using MDI Jade 6. The β crystal form exhibited a characteristic long-spacing peak at a 2θ diffraction angle of 19.36 ± 0.2°, indicating a bilayer packing of reactive molecules; and a characteristic short-spacing peak at a 2θ diffraction angle of 22.73 ± 0.2°, indicating a close-packed transverse packing of alkane chains. The β' crystal form exhibited a characteristic peak at a 2θ diffraction angle of 20.28 ± 0.2°, indicating a tilted packing of reactive molecules.

[0089] The relative proportion of crystal forms is calculated using the following formula:

[0090] β-crystal content = S1 / S3 × 100%

[0091] Where S1 is the integrated area of ​​the β crystal form, including the areas of long-spacing peaks and short-spacing peaks; S2 is the integrated area of ​​the β' crystal form; S3 = S1 + S2 is the sum of the integrated areas of β and β'.

[0092] In Example 12, the XRD pattern of the β-crystal form of adipose crystals is as follows: Figure 1 As shown.

[0093] Methods for testing adipose crystal aggregates: Structures were observed using a polarizing microscope (Olympus Model CX41 biological microscope, Olympus) and a 5616×3744 pixel digital camera (Canon, 10×Olympus lens). A small amount of oleogel was applied to a glass slide, diluted with MCT as needed, and immediately covered with a coverslip for observation. To estimate crystal size, images acquired using the same threshold image and 10x objective lens were used. The average crystal size of each sample (at least 20 crystals) was statistically analyzed using ImageJ to estimate the average crystal size in the images.

[0094] Product flowability: Weigh 2-3g of the prepared combined material liquid and place it at the bottom of a 10mL stoppered colorimetric tube. After turning the bottom over, tilt the tube at 45° and observe the shortest time (T) required for the liquid to just slide down to the outlet. The shorter the time, the better the flowability (flowability). The unit is minutes (min). The material temperature is controlled within the range of 40±2℃ throughout the measurement.

[0095] Dispersion uniformity: Take 25g of the sample solution using a 100mL stoppered graduated cylinder, seal it tightly, shake vigorously for 1 minute, and record the initial height (H_0). After standing for 24 hours, record the final height (H). Sedimentation volume ratio = H / H_0.

[0096] Product oil leakage rate: Collect and record the number of oil-leaking products during the molding and light inspection process / the total number of products in the batch, and determine the oil leakage rate (X = number of oil-leaking products / total number of products in the batch * 100%). When the oil leakage rate is higher than 10%, it proves that the product defect rate is high and production is not feasible.

[0097] Table 1

[0098]

[0099] Both the examples and the control examples were prepared using the capsule shells prepared according to the table below.

[0100] Table 2

[0101]

[0102] Both the example and control capsules were prepared using the following method:

[0103] Capsule shell: Heat the gelling agent and moisture retention agent to 60~90℃ and stir until completely dissolved, remove air bubbles and set aside;

[0104] Composition liquid: Solid fat is heated and mixed with liquid oil, then nutrients are added to prepare the liquid for later use.

[0105] Capsule preparation: The composition liquid is filled into the capsule shell and soft capsules are made by pressing or dripping under the conditions of ambient temperature of 18~26℃ and relative humidity of 60%.

[0106] Drying: The moisture content of the capsule shell is dried to 7%~20%, and the moisture content is detected by a halogen method rapid moisture analyzer.

[0107] The final capsule has a shell-to-content mass ratio of 3:7.

[0108] Examples 1-3, Comparative Examples 1-2

[0109] Table 3 Composition (parts by mass) and scoring of the composition liquid

[0110]

[0111] As can be seen, in Examples 1-3, the PC content in the phospholipids ranged from 10% to 55%, regulating the crystallization behavior of the composition. The content of tightly ordered β-crystals was within the range of 50% to 90%. The three-dimensional network structure formed by the accumulation of β-crystal adipose crystals provided a supporting framework for the dispersion of solid powder in the oil phase and contributed to the flowability of soft capsules. The prepared soft capsules had good molding performance, and the overall scores were all higher than 3.5. In Control Example 1, the PC content in the phospholipids was too low, the composition had a weak texture, the density of β-crystals was low, and the size of adipose crystals was too large, making it impossible to uniformly disperse the solid powder and showing a tendency for solid-liquid separation. In Control Example 2, the PC content in the phospholipids was too high, the β-crystal content was too high, the structural density of the liquid was high, the flowability of the composition was significantly weakened, which was not conducive to the preparation and molding of soft capsules / gel candies, and the overall score was significantly reduced. Therefore, phospholipids with a PC content of 10% to 55% regulate crystal structure and rheological properties, resulting in a β-crystal fatty crystal content of 50% to 90% in the composition. This leads to excellent rheological properties, promotes uniform dispersion of solid powder in the composition, and results in good soft capsule molding performance and a high overall score.

[0112] Examples 4-6, Comparative Examples 3 and 4

[0113] Table 4 Composition (parts by mass) and scoring of the composition liquid

[0114]

[0115] It can be seen that in Comparative Example 3, the mass ratio of phospholipid to processed oil was too low. Although the composition had good flowability, the weak interaction between phospholipid and processed oil resulted in weak carrying capacity of the fat crystals and weak support for the solid powder. Consequently, significant oil leakage easily occurred when this composition was prepared into soft capsules. In Comparative Example 4, the mass ratio of phospholipid to processed oil was too high, with β-crystalline fat crystals accounting for as much as 97.37% and a crystal size of 2.19 μm. The composition had a hard and brittle texture, which significantly reduced the flowability of the liquid, increased the difficulty of soft capsule molding, and resulted in a high oil leakage rate. In contrast, the mass ratio of phospholipid to processed oil in Examples 4-6 was moderate, with the proportion of β-crystalline fat crystals ranging from 54% to 90% and the crystal aggregate size ranging from 15 to 75 μm. These compositions exhibited good flowability, strong oil phase loading performance, excellent rheological properties, and the ability to uniformly disperse solid powder. The prepared soft capsules had good molding conditions and low oil leakage rates, with an overall score exceeding 3.5 points.

[0116] Examples 7-9, Comparative Example 5

[0117] Table 5 Composition (parts by mass) and scoring of the composition liquid

[0118]

[0119] It can be seen that the composition has requirements on the loading of solid powder. In Examples 7-9, when the proportion of probiotic powder increased from 1 part to 30 parts, the fat crystallization behavior was good, the proportion of β crystal form was in the range of 53% to 78%, the crystal aggregate size was 35 to 80 μm, and it exhibited good rheological properties, stably and uniformly dispersing the probiotic powder, resulting in a high overall product score. In Control Example 7, when the proportion of probiotic powder was further increased to 50 parts, the density of solid particles in the oil phase was too high, which hindered the crystallization behavior of fat and made it impossible to construct a crystal network structure to support the solid powder. It showed a solid-liquid stratification phenomenon, and the powder agglomerated in the oil phase, resulting in an uneven system and difficulty in forming during the preparation of soft capsules, leading to a low overall score.

[0120] Comparative Examples 6-8, Example 10

[0121] Table 6 Composition (parts by mass) and scoring of the composition liquid

[0122]

[0123] It can be seen that the introduction of liquid oil significantly weakens the regulatory effect of phospholipids on processed oils, which is detrimental to the formation of β crystals. Simultaneously, the addition of liquid oil dilutes the density of fat crystals in the system, altering the rheological properties of the material. In Comparative Examples 6-8, as the phospholipid content increased, the β crystal content and the carrying capacity of fat crystals improved, but the overall product scores were low, failing to meet the requirements. In Example 10, by increasing the phospholipid content in the system and increasing the ratio of phospholipids to processed oils, the rheological properties of the liquid were significantly improved, the product flowability was significantly improved, the solid powder was uniformly dispersed, the soft capsules formed well, and there was no oil leakage. This indicates that by controlling the ratio and content of phospholipids to processed oils, the negative effects brought by liquid oils can be eliminated, achieving ideal technical results. Subsequent examples will further explore the impact of the formulation composition of the liquid oil system on the technical effects.

[0124] Examples 11-13, Comparative Examples 9-11

[0125] Table 7 Composition (parts by mass) and scoring of the composition liquid

[0126]

[0127] It can be seen that in liquid oil systems, the PC content of phospholipids significantly affects the crystallization behavior of processed oils. In Examples 11-13, the PC content of phospholipids ranged from 10% to 55%, the β-crystal content was between 55% and 86%, and the size of the adipose crystal aggregates was between 24 and 80 μm; for example... Figure 2 As shown, the average size of the fat crystal aggregates in Example 12 was 39.07±3.82μm; the liquid had good crystal structure and rheological properties, could uniformly disperse solid powder, had good product flowability, low oil leakage rate, and high overall score; in Control Examples 9-11, the PC content of phospholipids was too low or too high, which was not conducive to controlling the crystallization behavior of the processed oils, the rheological properties of the liquid were poor, and the overall score was low. These test results are basically consistent with the trend of the data in Table 3.

[0128] Examples 14-16, Comparative Examples 12-13

[0129] Table 8 Composition (parts by mass) and scoring of the composition liquid

[0130]

[0131] It can be seen that the mass ratio of phospholipids to processed oils significantly affects the crystallization behavior, crystal structure, and rheological properties of the oils. In Examples 14-16, the ratio of phospholipids to processed oils was 1:5 to 1:15, with significant molecular interactions between the two. Phospholipids could regulate the formation of a β-crystal-dominated structure in the processed oils, with a content ranging from 57% to 90%. The density of the fat crystals was moderate, which could eliminate the dilution effect of the liquid oil, resulting in good macroscopic rheological properties, uniform dispersion of solid powder, and an overall score of over 4 points. In Control Examples 12-13, a ratio of phospholipids to processed oils that was too high or too low was not conducive to the formation of ideal fat crystals, and the texture of the liquid was either hard and brittle or soft and weak, which was not conducive to the preparation of soft capsules.

[0132] Examples 17-19, Comparative Examples 14-15

[0133] Table 9 Composition (parts by mass) and scoring of the composition liquid

[0134]

[0135] It can be seen that as the liquid oil content decreases, the β crystal content gradually increases, while the fat crystal size gradually decreases, thus affecting the rheological properties of the liquid and the technical performance of the product. In Examples 17-19, when the liquid oil content is between 60% and 90%, the β crystal content is between 60% and 86%, and the size of the fat aggregates is between 20 and 65 μm, the rheological properties of the liquid are good, and the overall product score is high. In Comparative Example 14, the liquid oil content is too low, the density of the fat crystals is too high, the hardness of the liquid is too high, and the flowability is poor, which is not conducive to the preparation of soft capsules. In Comparative Example 15, the liquid oil content is too high, the fat crystals are diluted, the structural density is low, the β crystal content is low, the carrying capacity for solid powder is insufficient, and the technical performance of the product is poor.

[0136] Examples 20-22, Comparative Example 16

[0137] Table 10 Composition (parts by mass) and scoring of the composition liquid

[0138]

[0139] It can be seen that solid powder also hinders the crystallization behavior of oils, affecting the formation of β crystals and the size of fat aggregates. As the solid powder content increases, the β crystal content gradually decreases, while the size of the fat aggregates increases. In Examples 20-22, the solid powder content was 1-30%, the β crystal content was 53-80%, the size of the fat aggregates was 30-78 μm, the crystal structure density was suitable, the rheological properties of the liquid were good, and the overall score was above 3.5. In Control Example 16, the solid powder content was 50%, which hindered the formation of β crystals, resulted in low crystal density, significantly reduced load-bearing capacity, and a significantly lower overall score.

[0140] Examples 23-28

[0141] Table 11 Composition (parts by mass) and scoring of the composition liquid

[0142]

[0143] As can be seen, in Examples 23-28, the content of β crystals was 60-81%, the size of the fat crystal aggregates was 23-54 μm, the rheological properties of the liquid were excellent, the product had good flowability, the solid powder could be uniformly dispersed in the system, and the prepared soft capsules showed no obvious oil leakage. These results indicate that the system can stably load solid nutrients such as plant extracts, animal extracts, vitamins, and microbial fermentation.

[0144] Examples 29-34

[0145] Table 12 Composition (parts by mass) and scoring of the composition liquid

[0146]

[0147] As can be seen, in Examples 29-34, phospholipids can regulate the formation of crystal network structures dominated by β crystal form in different types of processed oils, with the content all in the range of 70-80%, the size of fat aggregates in the range of 35-50μm, excellent rheological properties of the liquid, good product technical effect, and high comprehensive score.

[0148] Examples 35-36

[0149] Table 13 Composition (parts by mass) and scoring of the composition liquid

[0150]

[0151] It can be seen that when the soft capsule contents have a two-layer structure, namely including an intermediate protective layer and a core layer, the composition within the scope of protection of this invention is placed in the core layer. For example, in Example 35, the β crystal content is about 75%, the size of the fat crystal aggregates is about 43 μm, the rheological properties of the liquid are excellent, and the product technology is basically the same as that of Example 5. Similarly, in Example 36, the β crystal content, the size of the fat crystal aggregates, and the overall product score are basically the same as those of Example 19, indicating that the physicochemical properties and technical effects of compositions with the same formulation ratio for preparing one-layer and two-layer contents are basically the same.

[0152] The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and shall be included within the protection scope of the present invention.

Claims

1. A composition comprising oils, phospholipids, and nutrients, characterized in that: Based on the mass percentage of the composition, the β-crystal form accounts for 50% to 90% of the fatty crystals formed by the oil, the average diameter of the fatty crystal aggregates is 10 to 100 μm, and the phospholipid content is 10 wt% to 55 wt%. The oil is a semi-solid to solid processed oil; based on the mass percentage of the composition, the composition comprises 0.1-0.5% phospholipids, 69-99% semi-solid to solid processed oil, and 1-30% nutrients; the mass ratio of phospholipids to semi-solid to solid processed oil is 1:150-1000; or The oil is a combination of semi-solid to solid processed oil and liquid oil; by mass percentage of the composition, the composition includes 0.5-3.0% phospholipids, 5-30% semi-solid to solid processed oil, 50%-90% liquid oil and 1%-30% nutrients; the mass ratio of phospholipids to semi-solid to solid processed oil is 1:5-15.

2. The composition according to claim 1, characterized in that: The liquid oils include at least one of fish oil, cod liver oil, soybean oil, corn oil, peanut oil, flaxseed oil, safflower seed oil, walnut oil, rapeseed oil, pumpkin seed oil, rice bran oil, borage oil, olive oil, algae oil, and medium-chain triglycerides (MCTs).

3. The composition according to claim 1, characterized in that: The semi-solid to solid processed oils include beeswax, higher fatty acid glycerides, palm oil extracts, edible hydrogenated oils, margarine, shortening, and cocoa butter substitutes.

4. The composition according to claim 3, characterized in that: The higher fatty acid glycerides include glyceryl monostearate, glyceryl distearate, and / or mixtures thereof formed by the reaction of higher fatty acids and glycerol; the higher fatty acid is stearic acid.

5. The composition according to claim 1, characterized in that: The nutritional components include at least one of the following: probiotic powder, epigallocatechin gallate, yeast protein, vitamin B5, coenzyme Q10, and turmeric.

6. A method for preparing the composition according to any one of claims 1 to 5, characterized in that: Includes the following steps: The oil is melted and mixed with phospholipids, and then nutrients are added to obtain the composition described above.

7. A soft capsule, characterized in that: It includes a shell and a core; the core includes the composition according to any one of claims 1 to 5.

8. A method for preparing the soft capsule according to claim 7, characterized in that: Includes the following steps: The capsule core is injected into the capsule shell and then pressed or dripped into soft capsules.

9. Use of the composition according to any one of claims 1 to 5 or the soft capsule according to claim 7 in food.

10. The use according to claim 9, characterized in that: The food products mentioned include health food products.

Images