CN115486533A - Stable insoluble solid particle suspension system - Google Patents

Stable insoluble solid particle suspension system Download PDF

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Publication number
CN115486533A
CN115486533A CN202211194990.8A CN202211194990A CN115486533A CN 115486533 A CN115486533 A CN 115486533A CN 202211194990 A CN202211194990 A CN 202211194990A CN 115486533 A CN115486533 A CN 115486533A
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China
Prior art keywords
oil
liquid composition
aqueous liquid
solid particles
insoluble solid
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CN202211194990.8A
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Chinese (zh)
Inventor
许丹芸
陈文荣
方素琼
纪丹燕
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Xianle Health Technology Anhui Co ltd
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Xianle Health Technology Anhui Co ltd
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Priority to CN202211194990.8A priority Critical patent/CN115486533A/en
Publication of CN115486533A publication Critical patent/CN115486533A/en
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    • 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
    • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/14—Esters of carboxylic acids, e.g. fatty acid monoglycerides, medium-chain triglycerides, parabens or PEG fatty acid esters
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/22—Heterocyclic compounds, e.g. ascorbic acid, tocopherol or pyrrolidones
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/44—Oils, fats or waxes according to two or more groups of A61K47/02-A61K47/42; Natural or modified natural oils, fats or waxes, e.g. castor oil, polyethoxylated castor oil, montan wax, lignite, shellac, rosin, beeswax or lanolin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/044—Suspensions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/67—Vitamins
    • A61K8/676—Ascorbic acid, i.e. vitamin C
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/927—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of insects, e.g. shellac
    • 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
    • A61K9/10—Dispersions; Emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • 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
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use

Abstract

The present invention relates to a stable suspension system of insoluble solid particles. Specifically, the invention relates to a stable aqueous liquid composition which is characterized by comprising the following components in percentage by weight: (ii) from 0.1% to 29.9% insoluble solid particles, (ii) from 0.5% to 15% ascorbyl palmitate, (iii) from 0.1% to 19% liquid oil, (iv) from 0.1% to 19% solid oil, (v) from 0.5% to 10% emulsifier, and (vi) water.

Description

Stable suspension system of insoluble solid particles
Technical Field
The invention relates to the fields of emulsification, oil-in-water emulsion and the like in foods, health products and medicines. In particular, the present invention relates to a stable suspension system of insoluble solid particles.
Background
Insoluble particles such as mineral salts and oxides are easy to precipitate in a conventional liquid system, and a common stable mode is to use colloid for system thickening. Although the colloid can play a certain stabilizing role, the colloid in the system is easily damaged and degraded in the processes of high-temperature sterilization, accelerated stability investigation or long-term storage, so that the viscosity of the system is reduced, and insoluble particles such as mineral salts and oxides precipitate, and the like.
Insoluble particles such as mineral salts and oxides are also difficult to stably suspend in a liquid environment, and the prior art provides some solutions for realizing stable suspension. For example, CN114732092A discloses an active calcium and magnesium microemulsion and a preparation method thereof, which converts inorganic calcium, magnesium and trace elements into organic calcium lactate, calcium citrate, magnesium lactate and the like by related technologies such as microbial fermentation and metal ion chelation, and prepares the organic calcium microemulsion into a suspended organic calcium microemulsion for breeding animals to supplement calcium. However, CN114732092A has no subsequent sterilization step, and can not ensure the uniformity and stability of the system after high-temperature sterilization.
CN114158720A discloses a suspension with high solid content and a preparation method thereof, wherein the suspension comprises 52-75% of solid active ingredients, 10-45% of oil dispersant, 0.5-5% of solubilizer, 0.1-5% of surfactant and 0.1-3% of glidant, and a grinding preparation method is adopted to enable feed liquid to form stable suspension. However, this patent application mainly addresses the suspension dispersion of solid components in oil-based dispersants, and does not address the stable suspension dispersion of solid components in water.
CN103141649B discloses a method for preparing a pectin nutritional soft candy containing high calcium salt, which comprises adding buffer salt to form pectin which is easily affected by high calcium ion content (25-350 parts) and can be rapidly formed into pectin which is not affected by calcium ion and does not coagulate, thereby facilitating the pouring and forming of soft candy. CN103141649B mainly solves the problem of soft candy formation after calcium salt addition by controlling pH value, but cannot solve the problem of stable suspension dispersion of solid components in water.
Thus, there remains a need for products and methods that can achieve stable suspension of insoluble particles such as mineral salts and oxides in liquid systems.
Disclosure of Invention
The invention provides a composition formula for realizing stable suspension of insoluble particles such as mineral salts, oxides and the like in a liquid system, and the insoluble particles such as the mineral salts, the oxides and the like can be stably suspended for a long time in high-temperature sterilization, accelerated stability investigation and/or shelf life of products.
In a first aspect, the present invention relates to a stable aqueous liquid composition characterized by comprising, in weight percent:
(i) 0.1% -29.9% of insoluble solid particles,
(ii) 0.5% -15% of ascorbyl palmitate,
(iii) 0.1% -19% of liquid oil,
(iv) 0.1 to 19 percent of solid grease,
(v) 0.5-10% of an emulsifier, and
(vi) And (3) water.
In some embodiments, the weight ratio of ascorbyl palmitate to liquid oil is 1. In some embodiments, the weight ratio of liquid oil to solid grease is from 1 to 8 to 6; preferably, the weight ratio of the liquid oil to the solid grease is 8. In some embodiments, the insoluble solid particles are solid particles selected from the group consisting of: calcium salts such as calcium citrate, calcium hydrogen phosphate, calcium pyrophosphate, tricalcium phosphate, or any combination thereof; magnesium salts such as magnesium citrate, magnesium hydrogen phosphate, magnesium pyrophosphate, magnesium phosphate, or any combination thereof; calcium oxide; magnesium oxide; or any combination thereof. In some embodiments, the liquid oil is selected from: sunflower seed oil, soybean oil, olive oil, corn oil, medium chain triglycerides or any combination thereof. In some embodiments, the solid oil is selected from: mono-, diglycerol fatty acid esters, citric acid esters, succinic acid esters, beeswax, or any combination thereof. In some embodiments, the emulsifying agent is selected from sodium starch octenyl succinate, gum arabic, whey protein, gellan gum, or any combination thereof. In some embodiments, the aqueous liquid composition is a suspension.
In a second aspect, the present invention relates to a process for preparing an aqueous liquid composition as defined in the first aspect, characterized by comprising the steps of:
(1) Heating and compounding ascorbyl palmitate, solid oil and liquid oil at 50-120 ℃ to form an oil phase;
(2) Stirring and dissolving the emulsifier to prepare a water phase;
(3) Slowly adding the oil phase into the water phase to prepare primary emulsion under the condition that the shearing speed of the water phase is kept between 5000rpm and 30000 rpm/min; and
(4) Adding insoluble solid particles into the colostrum system, and mixing well.
In a third aspect, the present invention relates to a method for the stable suspension of insoluble solid particles in water, characterized in that the insoluble solid particles are added to a colostrum system comprising an oil phase comprising ascorbyl palmitate, solid lipids and liquid oil and an aqueous phase comprising emulsifier, wherein the insoluble solid particles, ascorbyl palmitate, solid lipids, liquid oil and emulsifier are as defined in the first aspect.
In a fourth aspect, the present invention relates to a product comprising an aqueous liquid composition as defined in the first aspect. In some embodiments, the product is selected from the group consisting of a food product, a pharmaceutical product, a nutraceutical product, and a cosmetic product.
Detailed Description
Several aspects of the invention are described below with reference to example applications for illustration. It should be understood that numerous specific details, relationships, and methods are set forth to provide a full understanding of the invention. One skilled in the relevant art will readily recognize, however, that the invention can be practiced without one or more of the specific details, or with other methods.
Definition of
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. Furthermore, the open-ended expressions "comprising" and "comprises" are to be interpreted as meaning that structural elements or method steps not mentioned can also be present, but it is to be noted that the open-ended expressions also cover the case of consisting only of the stated components and method steps (i.e. the closed-ended expression "consisting of 8230; \8230; consists of).
As used throughout, ranges are used as shorthand for describing each and every value that is within the range. Any number within a range, such as an integer value, a value that increments by one tenth (when the end of the range is one digit after the decimal point), or a value that increments by one hundredth (when the end of the range is two digits after the decimal point) may be selected as the terminus of the range. For example, a range of 0.1% -29.9% is used to describe all values within that range, e.g., 0.1%, 0.2%, 0.3%, 0.4%, 0.5%. 29.4%, 29.5%, 29.6%, 29.7%, 29.8%, and 29.9% (all values to the nearest decimal place), and includes all subranges defined between any two of the preceding values, e.g., 0.1% -25%, 1% -20%, 5% -15%, 0.1% -12.5%, 10% -12.5%, etc.
The phrase "in any range defined between any two of the preceding values," as used herein, literally means that any range can be selected from any two values listed before such phrase, regardless of whether the values are in the lower portion of the list or the upper portion of the list. For example, a pair of values may be selected from two lower values, two higher values, or one lower value and one higher value.
All parts and percentages used herein are by weight unless otherwise indicated.
Unless defined otherwise, all 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.
Aqueous liquid composition
The invention provides a stable aqueous liquid composition, which comprises the following components in percentage by weight:
(i) 0.1% -29.9% of insoluble solid particles,
(ii) 0.5% -15% of ascorbyl palmitate,
(iii) 0.1 to 19 percent of liquid oil,
(iv) 0.1 to 19 percent of solid grease,
(v) 0.5-10% of an emulsifier, and
(vi) And (3) water.
The components contained in the aqueous liquid composition of the present invention will be described in detail below.
(i) Insoluble solid particles
In the present application, insoluble solid particles refer to solid substances that are poorly soluble or slightly soluble in water at normal temperature. Herein, the normal temperature is also referred to as room temperature, and means a temperature in the range of 20 to 25 ℃. Such insoluble solid particles are not particularly limited. For example, in a preferred embodiment, the insoluble solid particles are mineral salts and oxides, and the like. In a more preferred embodiment, the insoluble mineral salt or insoluble oxide is a calcium salt such as calcium citrate, calcium hydrogen phosphate, calcium pyrophosphate, tricalcium phosphate, or any combination thereof; magnesium salts such as magnesium citrate, magnesium hydrogen phosphate, magnesium pyrophosphate, magnesium phosphate, or any combination thereof; calcium oxide; magnesium oxide; or any combination thereof.
The insoluble solid particles are generally present in an amount of from 0.1% to 29.9% by weight based on the total weight of the aqueous liquid composition. When the content of the insoluble solid particles is less than 0.1%, the content of the insoluble solid particles in the aqueous liquid composition thus obtained is too low, and there is a fear that it is difficult to apply it to an intended purpose; when the content of insoluble solid particles is more than 29.9%, the aqueous liquid composition is easily delaminated, and it is difficult to obtain a stable suspension. In one embodiment, the insoluble solid particles are present in an amount of 0.1%, 0.2%, 0.3%, 0.4%, 0.5%. 29.4%, 29.5%, 29.6%, 29.7%, 29.8%, or 29.9% (all to the nearest decimal value), or all subranges defined between any two of the foregoing values, e.g., 0.1% -25%, 0.5% -25%, 1% -20%, 2% -18%, 3% -21%, 4% -16%, 5% -15%, 6% -14%, 7% -13%, 8% -12%, 9% -11%, 0.1% -12.5%, 10% -12.5%, 5% -25%, 15% -25%, etc.
The particle size of the insoluble solid particles is not particularly limited as long as it can be stably suspended. In some embodiments, the insoluble solid particles may be nanoparticles (particle size of 1-100 nm), submicron particles (particle size of 0.1-1 μm), microparticles and micropowder (particle size of 1-100 μm), fines and fines (particle size of 100-1000 μm), or coarse particles (particle size greater than 1 mm). In some embodiments, the D50 (median or median particle diameter) of the insoluble solid particles may be from 1 to 100 nm, from 0.1 to 1 μm, from 1 to 100 μm, from 100 to 1000 μm, or greater than 1 mm.
(ii) Ascorbyl palmitate
The ascorbyl palmitate is prepared by esterifying palmitic acid and ascorbic acid with natural components of chemical formula C 22 H 38 O 7 The antioxidant is a high-efficiency oxygen scavenger and synergist, is a nutritional, non-toxic, high-efficiency and safe-to-use food additive evaluated by the World Health Organization (WHO) food additive committee, and is the only antioxidant which can be used for infant food in China. It can be used in food for resisting oxidation, protecting food (oil) color, and enhancing nutrition.
The ascorbyl palmitate is generally present in an amount of from 0.5% to 15% by weight, based on the total weight of the aqueous liquid composition. In one embodiment, the ascorbyl palmitate is present in an amount of 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%. 14.5%, 14.6%, 14.7%, 14.8%, 14.9%, or 15.0% (all numerical values to the nearest decimal place), or all subranges defined between any two of the foregoing values, e.g., 0.5% -12.5%, 1.0% -10.0%, 1.5% -7.5%, 2.0% -5.0%, 2.2% -2.5%, 3.0% -9.0%, 4.0% -8.0%, 5.0% -6.0%, 7% -13%, 8% -12%, 9% -11%, 1.0% -12.5%, 10% -12.5%, 2.2% -10.0%, 1.5% -2.5%, etc.
In some embodiments, the weight ratio of ascorbyl palmitate to liquid oil is 1.
(iii) Liquid oil
Liquid oil refers to a fat or oil that is liquid at ordinary temperature, and may be of plant or animal origin, for example.
The liquid oil that can be used in the present application is not particularly limited. In a preferred embodiment, the liquid oil is sunflower oil, soybean oil, olive oil, corn oil, medium chain triglycerides or any combination thereof. These may be used alone or as a mixture of two or more.
The liquid oil content is generally from 0.1% to 19% by weight, based on the total weight of the aqueous liquid composition. In one embodiment, the liquid oil is present in an amount of 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%. 18.5%, 18.6%, 18.7%, 18.8%, 18.9%, or 19.0% (all to the nearest decimal point), or all subranges defined between any two of the foregoing values, e.g., 0.1% -18%, 1.0% -17%, 1.5% -16%, 2.0% -15%, 2.5% -14%, 3.0% -13%, 4.0% -12%, 5.0% -11%, 6.0% -10%, 7% -13%, 8% -12%, 9% -11%, 1.0% -12.5%, 10% -12.5%, 2% -4.5%, 1.5% -2.5%, 4.0% -4.5%, etc.
In some embodiments, the weight ratio of liquid oil to solid grease is 1.
(iv) Solid oil and fat
Here, the solid oil and fat means an oil and fat that is solid at ordinary temperature, and for example, it may be of a plant origin or an animal origin.
The solid fat and oil usable in the present application is not particularly limited. In one embodiment, the solid fat is preferably selected from mono-, di-glycerol fatty acid esters, citric acid esters, succinic acid esters, beeswax or any combination thereof. These may be used alone or as a mixture of two or more. In some embodiments, the fatty acid in the mono-diglycerol fatty acid ester is selected from any one or more of oleic acid, linoleic acid, palmitic acid, behenic acid, stearic acid, lauric acid, and linolenic acid.
The content of the solid oil is usually 0.1% to 19% by weight based on the total weight of the aqueous liquid composition. In one embodiment, the solid fat is present at 0.1%, 0.2%, 0.3%, 0.4%, 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%. 18.5%, 18.6%, 18.7%, 18.8%, 18.9%, or 19.0% (all to the nearest decimal point), or all subranges defined between any two of the foregoing values, e.g., 0.1% -18%, 1.0% -17%, 1.5% -16%, 2.0% -15%, 2.5% -14%, 3.0% -13%, 4.0% -12%, 5.0% -11%, 6.0% -10%, 7% -13%, 8% -12%, 9% -11%, 1.0% -12.5%, 10% -12.5%, 2% -4.5%, 1.5% -2.5%, 1.0% -3.0%, 1.0% -5.0%, and the like.
(v) Emulsifying agent
The emulsifier is a substance capable of improving the surface tension between various constituent phases in an emulsification system to form a uniform dispersion or emulsion.
The emulsifier that can be used in the present application is not particularly limited. In a preferred embodiment, the emulsifying agent is selected from sodium starch octenyl succinate, gum arabic, whey protein, gellan gum, or any combination thereof. These may be used alone or as a mixture of two or more.
The content of the emulsifier is usually 0.5 to 10% by weight based on the total weight of the aqueous liquid composition. In one embodiment, the emulsifier is present in an amount of 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1.0%. 9.5%, 9.6%, 9.7%, 9.8%, 9.9%, or 10.0% (all numerical values to the nearest decimal place), or all subranges defined between any two of the foregoing values, e.g., 0.5% to 9.5%, 1.0% to 9.0%, 1.5% to 8.5%, 2.0% to 8.0%, 2.5% to 7.5%, 3.0% to 7.0%, 3.5% to 6.5%, 4.0% to 6.0%, 5.0% to 5.5%, 4% to 8%, 6% to 10%, 3% to 6%, etc.
In some embodiments, the weight ratio of liquid oil to emulsifier is from 2 to 3, for example 2.
(vi) Water (I)
The content of water is not particularly limited; typically from 50% to 90% by weight of the total aqueous liquid composition. In one embodiment, the aqueous liquid composition of the present invention comprises, in addition to the above components, a balance of water. In one embodiment, the water is present in an amount of 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, or 90%, or all subranges defined between any two of the foregoing values, e.g., 50% to 85%, 55% to 80%, 60% to 75%, 65% to 80%, etc.
In a preferred embodiment, the aqueous liquid composition of the invention is a suspension. It is known to those skilled in the art that the aqueous liquid composition of the present invention may further comprise other components commonly used in aqueous liquid compositions, such as sweetener, essence, acidity regulator, etc., in addition to the above components, without impairing the effects of the present invention.
The aqueous liquid compositions of the present invention are stable in that insoluble particles of mineral salts and oxides are stably suspended for long periods of time without delamination or precipitation during high temperature sterilization, accelerated stability studies and/or shelf life. In addition, the aqueous liquid composition can meet the requirements of safe product quality, stable system and fine mouthfeel.
Although the components of the aqueous liquid composition of the present invention are described separately above, it will be understood by those skilled in the art that the embodiments described separately for each component may be combined with each other to form further embodiments. Such embodiments are also encompassed within the disclosure of the present specification and fall within the scope of the invention.
Preparation of aqueous liquid composition
The aqueous liquid composition of the present invention can be prepared by a conventional method known in the art, and a specific preparation method is not particularly limited.
In one embodiment, the aqueous liquid composition of the present invention is prepared as follows:
(1) heating and compounding ascorbyl palmitate, solid oil and liquid oil at 50-120 ℃ to form an oil phase;
(2) stirring and dissolving the emulsifier to prepare a water phase;
(3) adding the oil phase into the water phase to prepare colostrum under the condition that the shearing speed of the water phase is kept between 5000rpm and 30000 rpm/min; and
(4) adding insoluble solid particles into the colostrum system, mixing, and optionally sterilizing at 80-100 deg.C for 0.5-2h.
In the present invention, the colostrum to be prepared is not particularly limited. In some embodiments, the colostrum is an oil-in-water emulsion. In some embodiments, the colostrum may be a nanoemulsion or a microemulsion. In some embodiments, the droplets of colostrum have a particle size of 1-100 nm, 0.1-1 μm, 1-100 μm, or 100-1000 μm.
Product comprising an aqueous liquid composition
The invention also provides a product comprising an aqueous liquid composition of the invention. It will be understood by those skilled in the art that there is no limitation as to the particular type of product, as long as it is a product suitable for containing an aqueous liquid composition.
In one embodiment, the product is any one selected from the group consisting of: food, medicine, health product and cosmetic. In a preferred embodiment, the product is a functional beverage. In another preferred embodiment, the product is a functional food.
Method for stably suspending insoluble solid particles in water
The invention also provides a method of stably suspending insoluble solid particles in water which comprises adding the insoluble solid particles to a colostrum system which comprises an oil phase comprising ascorbyl palmitate, solid lipids, and liquid oil, and an aqueous phase comprising emulsifier. In some embodiments, the oil phase is formed by heat compounding ascorbyl palmitate, solid fats and oils, liquid oils at 50-120 ℃. In some embodiments, the aqueous phase is prepared by dissolving the emulsifier with agitation. In some embodiments, the colostrum is prepared by adding the oil phase to the aqueous phase while maintaining the shear rate of the aqueous phase at 5000rpm to 30000 rpm/min. In some embodiments, insoluble solid particles are added to the colostrum system, mixed well, optionally followed by sterilization at 80-100 ℃ for 0.5-2h.
In addition, in the method of the present invention, a step of forming an oil phase and an aqueous phase, and an addition step of insoluble solid particles, ascorbyl palmitate, solid fat and oil, liquid oil, sodium starch octenyl succinate and the like may be further included.
For the insoluble solid particles, ascorbyl palmitate, solid fats and oils, liquid oils, sodium starch octenyl succinate and the like involved in the methods of the aspects of the present invention, reference is made to the details as described above in the section "aqueous liquid composition".
While various embodiments of the present invention have been described above, it should be understood that they have been presented by way of example only, and not limitation. Many modifications to the disclosed embodiments may be made in accordance with the disclosure herein without departing from the spirit or scope of the invention. Thus, the breadth and scope of the present invention should not be limited by any of the above-described embodiments.
Examples
Unless otherwise indicated, the materials used in the examples herein are commercially available and the various specific experimental procedures used to carry out the experiments are either routine in the art or according to procedures and conditions suggested by the manufacturer and can be routinely determined by those skilled in the art as desired.
1. Materials (all commercially available)
Ascorbyl palmitate, tea polyphenol palmitate, vitamin a palmitate;
xanthan gum, guar gum, pectin;
emulsifier: sodium starch octenyl succinate, acacia, lactalbumin, gellan gum;
solid grease: mono-diglycerol fatty acid ester, citric acid ester, succinic acid ester, and beeswax;
liquid oil: sunflower seed oil, soybean oil, olive oil, corn oil, medium chain triglycerides;
insoluble solid particles: calcium citrate (particle size: 10 μm), calcium hydrogen phosphate (particle size: 75 μm), calcium pyrophosphate (particle size: 100 μm), tricalcium phosphate (particle size: 15 μm).
2. Preparation method
(1) Heating and compounding ascorbyl palmitate, solid grease and liquid oil at 95 ℃ to form an oil phase;
(2) stirring to dissolve starch sodium octenyl succinate to prepare water phase;
(3) slowly adding the oil phase into the water phase to prepare primary emulsion under the condition that the shearing speed of the water phase is kept at 15000 rpm/min;
(4) adding insoluble solid particles into the colostrum system, mixing well, and sterilizing at 90 deg.C for 1h.
3. Test method
The adopted instrument is as follows: appearance evaluation, viscometer, high speed centrifuge;
(1) Appearance evaluation: the prepared composition was sterilized at 90 ℃ for 1 hour and then cooled to room temperature, and the delamination severity was evaluated. The evaluation indexes are as follows: and observing the appearance by naked eyes, wherein no obvious liquid level layering is no layering.
(3) And (3) centrifugal evaluation: and (4) placing the sterilized sample in a centrifugal tube, centrifuging at 25 ℃ and 4000rpm for 10min, then sucking out the supernatant by using a liquid transfer gun, and testing the quality to obtain the water yield.
Water yield = (water yield/sample addition) × 100%
In the following examples, "/" in each table indicates no delamination and no water discharge for the water discharge rate.
(3) The sterilized sample was added to the sample tube, tested using a rotary viscometer (ROTAVIC lo-vi II Complete, ika), the instrument was leveled, and the sample viscosity was measured using a SP-3 rotor at 25 ℃.
4. Working examples
(1) Example 1 ascorbyl palmitate thickening validation
Samples 1-5 were prepared as described above and tested and evaluated as described above. The result shows that the sunflower seed oil can not be emulsified only by adding the ascorbyl palmitate, the system can not be stable, and the layering is obvious, which shows that the emulsification effect of the ascorbyl palmitate is not obvious; under the condition of not adding ascorbyl palmitate, the octenyl succinic acid starch sodium can emulsify the sunflower seed oil, an emulsification system is not layered, but the viscosity of the system is lower; after the ascorbyl palmitate and sodium starch octenyl succinate are added, the system is stable and does not delaminate, the viscosity is obviously improved, and the ascorbyl palmitate has an obvious thickening effect. The results of samples 4 and 5, however, demonstrate that neither tea polyphenol palmitate nor vitamin A palmitate have significant thickening effects.
Figure 838792DEST_PATH_IMAGE001
(2) EXAMPLE 2 ascorbyl palmitate thickening Range examination
Samples 6-23 were prepared as described above and tested and evaluated as described above. The results show that in the condition of no addition of ascorbyl palmitate, the viscosity of the system is increased to a certain extent with the increase of the dosage of the starch sodium octenyl succinate, but the system is not layered stably; under the condition of no addition of ascorbyl palmitate, the viscosity of the system is basically unchanged along with the increase of the content of the sunflower seed oil, and the system is layered and unstable, which indicates that the viscosity of the system is not obviously affected by the increase of the liquid oil dosage; samples 14-23 the viscosity of the system increased gradually with increasing ascorbyl palmitate content, with the system going from delamination to no delamination and then to delamination. Therefore, the addition range of the ascorbyl palmitate is 0.5-15%, so that the system is not layered after centrifugation, and the water yield is obviously reduced.
Figure 173958DEST_PATH_IMAGE002
(3) Example 3 stabilization of calcium citrate by different colloidal thickening
Preparing colloid: heating purified water to 50 ℃, adding colloidal powder, stirring and dissolving until no colloidal particle is formed, and determining the final solution viscosity to be 10000cp, namely the end point. The viscosity of different colloids before sterilization is controlled to be 10000cp, and the colloids are uniformly mixed after calcium citrate is added, and are heated for sterilization. The results show that the viscosity of the system is reduced to different degrees after the ordinary colloid is sterilized, and the calcium citrate can not be supported to be stably suspended. The appearance of different colloid samples is obviously layered, and the colloid samples do not meet the requirements after centrifugation.
Figure 840563DEST_PATH_IMAGE003
(4) Example 4 examination of different emulsifiers
Samples 28-31 were prepared as described above and tested and evaluated as described above. The result shows that the replacement of sodium starch octenylsuccinate by other emulsifying agents, such as Arabic gum, lactalbumin and gellan gum, can stabilize and homogenize the system after sterilization, and the water yield is obviously improved.
Figure 106328DEST_PATH_IMAGE004
(5) Example 5 examination of different solid hard ester types
Samples 32-35 were prepared as described above and tested and evaluated as described above. The results show that other solid oils, such as citrate, succinate and beeswax, do not delaminate after sterilization and the centrifuge stability is acceptable.
Figure 604306DEST_PATH_IMAGE005
(6) Example 6 investigation of different liquid oils
Samples 36-40 were prepared as described above and tested and evaluated as described above. The results show that the system is thickened and is uniform after sterilization instead of other types of liquid oil, and the centrifugal stability is qualified when being examined.
Figure 313636DEST_PATH_IMAGE006
(7) Example 7 dosage examination of calcium citrate salt
Samples 41-45 were prepared as described above and tested and evaluated as described above. The result shows that the viscosity is increased along with the gradual increase of the content of the calcium citrate between 5 and 25 percent, the appearance is not layered after sterilization, and the centrifugal stability is qualified. When the content of the calcium citrate reaches 30 percent, the appearance of the system is layered, and excessive calcium citrate is at the bottom and cannot be completely suspended in the system.
Figure 264274DEST_PATH_IMAGE007
(8) Example 8 examination of the type of insoluble particles
Samples 46-49 were prepared as described above and tested and evaluated as described above. The results show that the mineral salts in the table are stably suspended in the system.
Figure 351308DEST_PATH_IMAGE008

Claims (10)

1. A stable aqueous liquid composition characterized by comprising in weight percent:
(i) 0.1% -29.9% of insoluble solid particles,
(ii) 0.5% -15% of ascorbyl palmitate,
(iii) 0.1 to 19 percent of liquid oil,
(iv) 0.1 to 19 percent of solid grease,
(v) 0.5-10% of an emulsifier, and
(vi) And (3) water.
2. The aqueous liquid composition according to claim 1, characterized in that the weight ratio of ascorbyl palmitate to liquid oil is from 1.
3. The aqueous liquid composition according to claim 1 or 2, characterized in that the weight ratio of liquid oil to solid fat is from 1.
4. The aqueous liquid composition according to claim 1 or 2, characterized in that the insoluble solid particles are solid particles selected from the group consisting of: calcium salts such as calcium citrate, calcium hydrogen phosphate, calcium pyrophosphate, tricalcium phosphate, or any combination thereof; magnesium salts such as magnesium citrate, magnesium hydrogen phosphate, magnesium pyrophosphate, magnesium phosphate, or any combination thereof; calcium oxide; magnesium oxide; or any combination thereof.
5. Aqueous liquid composition according to claim 1 or 2, characterized in that the liquid oil is selected from: sunflower seed oil, soybean oil, olive oil, corn oil, medium chain triglycerides, or any combination thereof.
6. Aqueous liquid composition according to claim 1 or 2, characterized in that the solid fat is selected from: mono-, diglycerol fatty acid esters, citric acid esters, succinic acid esters, beeswax, or any combination thereof.
7. Aqueous liquid composition according to claim 1 or 2, characterized in that the emulsifier is selected from sodium starch octenylsuccinate, gum arabic, whey protein, gellan gum or any combination thereof.
8. The aqueous liquid composition according to claim 1 or 2, characterized in that the aqueous liquid composition is a suspension.
9. A process for the preparation of an aqueous liquid composition according to any one of claims 1 to 8, characterized in that it comprises the steps of:
(1) Heating and compounding ascorbyl palmitate, solid oil and liquid oil at 50-120 ℃ to form an oil phase;
(2) Stirring and dissolving the emulsifier to prepare a water phase;
(3) Slowly adding the oil phase into the water phase to prepare primary emulsion under the condition that the shearing speed of the water phase is kept between 5000rpm and 30000 rpm/min; and
(4) Adding insoluble solid particles into the colostrum system, and mixing well.
10. A method of stably suspending insoluble solid particles in water, which comprises adding the insoluble solid particles to a colostrum system, which includes an oil phase containing ascorbyl palmitate, solid oil and liquid oil, and an aqueous phase containing emulsifier, wherein the insoluble solid particles, ascorbyl palmitate, solid oil and liquid oil and emulsifier are as defined in any one of claims 1 to 8.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104981170A (en) * 2012-11-14 2015-10-14 雅培制药有限公司 Stabilized liquid nutritionals including insoluble calcium salts
CN109198045A (en) * 2018-10-09 2019-01-15 嘉必优生物技术（武汉）股份有限公司 A kind of grease microcapsule and preparation method thereof
CN111194912A (en) * 2019-07-09 2020-05-26 北京市营养源研究所 Stable medical liquid enteral nutrition composition and preparation method thereof
CN114468063A (en) * 2021-12-28 2022-05-13 上海交通大学医学院 Fatty acid balanced type formula food with special medical application and preparation method thereof
CN114680197A (en) * 2020-12-29 2022-07-01 丰益(上海)生物技术研发中心有限公司 Structured emulsion

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104981170A (en) * 2012-11-14 2015-10-14 雅培制药有限公司 Stabilized liquid nutritionals including insoluble calcium salts
CN109198045A (en) * 2018-10-09 2019-01-15 嘉必优生物技术（武汉）股份有限公司 A kind of grease microcapsule and preparation method thereof
CN111194912A (en) * 2019-07-09 2020-05-26 北京市营养源研究所 Stable medical liquid enteral nutrition composition and preparation method thereof
CN114680197A (en) * 2020-12-29 2022-07-01 丰益(上海)生物技术研发中心有限公司 Structured emulsion
CN114468063A (en) * 2021-12-28 2022-05-13 上海交通大学医学院 Fatty acid balanced type formula food with special medical application and preparation method thereof

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