CN114680332A - Water-in-oil type high internal phase emulsion for carrying bitter substances and preparation method thereof - Google Patents
Water-in-oil type high internal phase emulsion for carrying bitter substances and preparation method thereof Download PDFInfo
- Publication number
- CN114680332A CN114680332A CN202210242175.8A CN202210242175A CN114680332A CN 114680332 A CN114680332 A CN 114680332A CN 202210242175 A CN202210242175 A CN 202210242175A CN 114680332 A CN114680332 A CN 114680332A
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- Prior art keywords
- oil
- water
- phase
- bitter
- high internal
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Links
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Images
Classifications
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
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- A—HUMAN NECESSITIES
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- A—HUMAN NECESSITIES
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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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
- A23L33/18—Peptides; Protein hydrolysates
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention provides a water-in-oil type high internal phase emulsion for carrying bitter substances and a preparation method thereof, and relates to the field of nutrient substance embedding and carrying. The water-in-oil type high internal phase emulsion carrying bitter substances comprises raw materials including a water phase and an oil phase, wherein the water phase comprises the bitter substances and a solvent; the oil phase comprises liquid oil, solid oil and polyglycerol ricinoleate. The bitter substance solution formed by the bitter substance and the solvent is used as an internal water phase, and the lipid network structure is constructed in a mode of combining liquid oil and solid oil to be an external oil phase, so that high internal phase emulsion with good stability is favorably formed, the encapsulation rate of the bitter substance and the content of the bitter substance in the emulsion are improved, the bad flavor of the bitter substance is covered, and the gastrointestinal digestion stability of the bitter substance is improved.
Description
Technical Field
The invention relates to the field of nutrient substance embedding and carrying, in particular to a water-in-oil type high internal phase emulsion for carrying bitter substances and a preparation method thereof.
Background
Flavors affecting consumer acceptance, such as astringency, bitterness, etc., are present in many food products, and bitter substances such as protein hydrolysates, peptides, herbal extracts, etc., have limited their use in the food industry due to the presence of undesirable flavors. For example, proteins are hydrolyzed by acid and base enzymes, and most of the polypeptides produced during the hydrolysis process have certain biological activity, but many animal and vegetable proteins exhibit bitter taste due to exposure of hydrophobic amino acids during the enzymatic hydrolysis process to form polypeptides, thereby greatly reducing the consumer acceptance (consumption of protein hydrolysates from animal by products: consumption on bits and deletion methods: economic w.international Journal of Food Science & Technology,2018,54(4), 978-. Such polypeptides that cause bitter taste in protein hydrolysates are commonly referred to as bitter peptides. Bitter peptides have attracted much attention as nutrients having physiological activities such as antibacterial, hypotensive, antioxidant, immunoregulatory, etc.
Because polypeptides are sensitive to the digestive environment of the gastrointestinal tract, degradation and loss of the physiological activity of the original structure may occur when exposed to the acidic environment of the stomach and digestive enzymes (Controlled release of viral-derived peptides in the gastric environment by side encapsulation in water-in-oil-in-water double expression. Lwt-Food Science and Technology,2016,69, 225-. Currently, most of the polypeptide powders obtained by spray drying in the food industry have strong hygroscopicity, which makes storage difficult. The bitter taste characteristics, gastrointestinal sensitivity and strong hygroscopicity of polypeptides have prevented their use in the food industry.
In order to obtain a consumer acceptable product, food practitioners have taken a series of measures to eliminate, mask, and improve the unpleasant taste of bitter flavors. The bitter taste masking methods generally used at present include additive methods, separation methods, enzyme treatment methods, maillard reaction methods, protein-like reaction methods, and encapsulation methods. The additive method is generally limited by additives and is limited in use, the separation method often causes polypeptide loss, the enzyme treatment debittering method has the defects of complex operation, high cost, strict experimental conditions and the like, the encapsulation can avoid the bitter substance from being directly exposed to the bitter receptor so that the bitter substance does not show bitter taste, can improve the gastrointestinal tract digestion sensitivity of the bitter substance and improve the biological utilization of the bitter substance, and simultaneously, the encapsulation can reduce the hygroscopicity of the bitter substance and improve the storage stability of the bitter substance.
Carriers for encapsulating water-soluble substances have been disclosed, mainly using carrier matrices of polysaccharides, proteins and lipids, and carrier types including liposomes, microcapsules, emulsions and the like (Encapsulation of food protein hydrosaltes and peptides: a review [ J ]. RSC Advances,2015,5(97): 79270-79278.). Some application problems of bitter tasting substances such as peptides and protein hydrolysates, including prevention of aggregation, controlled delivery and increased biostability, may be addressed by encapsulation. The liposome-encapsulated polypeptide faces the challenges of low encapsulation amount, thermodynamic instability, high cholesterol content and the like, and the microcapsule-encapsulated polypeptide also has the problem that the structure of the polypeptide is changed due to the Maillard reaction generated in the high-temperature spraying process of the wall material and the core material.
At present, the technology of carrying bitter substances by adopting emulsion encapsulation is mostly focused on double emulsions, for example, the Chinese non-patent document 'soybean oligopeptide decompression function, structure analysis and double emulsion bitterness masking technical research' discloses a method for preparing double emulsions to mask the bitterness of soybean oligopeptide: w is a group of1/O/W2The emulsion is prepared by a two-step homogenization method, and the first step is to prepare W stabilized by PGPR1The emulsion is prepared by dissolving soybean oligopeptide in water to obtain inner water phase, dissolving PGPR in MCT oil as oil phase, adding the water phase into the oil phase, and dispersing and homogenizing to obtain W1an/O emulsion; in a second step, OSA starch and maltodextrin are mixed and dissolved until the starch is completely gelatinized, and the solution is used as an external water phase (W)2). W is to be1W is slowly added into the/O emulsion2Phase, high speed shearing to obtain final W1/O/W2An emulsion. However, double emulsion encapsulation of delivery bitter peptides has the following limitations: internal phase material migration in double emulsionThe problem of low encapsulation efficiency caused by the migration to the external phase, the encapsulation efficiency is about 80%, and the storage stability is poor; double emulsions, due to the small volume fraction of the internal aqueous phase, typically have an encapsulated peptide content of less than 10% of the total emulsion; the preparation method of the double emulsion is complicated and has high process requirement.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of low encapsulation rate, poor storage stability, low bitter substance content, complex preparation process and the like of the double emulsion for encapsulating and carrying the bitter substance in the prior art, thereby providing the water-in-oil type high internal phase emulsion for carrying the bitter substance and the preparation method thereof.
In order to achieve the purpose, the invention provides the following technical scheme:
in a first aspect, the present invention provides a water-in-oil high internal phase emulsion for carrying bitter substances, which comprises a water phase and an oil phase as raw materials,
the aqueous phase comprises a bitter tasting substance and a solvent;
the oil phase comprises liquid oil, solid oil and polyglycerol ricinoleate.
Further, the mass concentration of the bitter substance in the water phase is 0.1-50%, preferably 5-50%.
Further, the mass concentration of the polyglycerol ricinoleate in the oil phase is 2-10%, preferably 4-6%; the mass ratio of the liquid grease to the solid grease is 0.5-10: 1, preferably 0.7-2.9: 1.
further, the mass fraction of the oil phase is 10-90%, preferably 12-25%.
Further, the bitter substance comprises at least one of wheat peptide, collagen peptide, soybean peptide, casein peptide, rice protein peptide, protein hydrolysate, Chinese medicinal decoction, and Chinese medicinal extract.
Further, the solvent comprises at least one of distilled water, PBS buffer solution with the concentration of 5-500 mM and citrate buffer solution with the concentration of 5-500 mM, and the PBS buffer solution with the concentration of 5mM is preferred.
Further, the liquid oil comprises at least one of camellia oil, corn oil, olive oil, medium chain triglyceride, linseed oil, castor oil, walnut oil, algae oil, peony seed oil, peanut oil, rapeseed oil, soybean oil, perilla seed oil and sunflower seed oil.
Further, the solid oil and fat comprises at least one of palm oil, coconut oil, shortening, butter and animal oil.
In a second aspect, the present invention provides a method for preparing the water-in-oil high internal phase emulsion carrying bitter substances, comprising the steps of:
(1) dissolving bitter substance in solvent to obtain water phase;
(2) heating and mixing liquid oil, solid oil and polyglycerol ricinoleate to obtain an oil phase;
(3) and adding the water phase into the heated oil phase for homogeneous dispersion to obtain the water-in-oil high internal phase emulsion carrying the bitter substances.
Further, in the step (3), the homogeneously dispersing includes: and in the process of adding the water phase into the oil phase, gradually increasing the rotating speed from 6000rpm to 8000rpm to 10000rpm to 14000rpm at the speed of 500rpm to 1000rpm per minute, and continuously dispersing for 1 min to 3min under 10000 to 14000 after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion carrying the bitter substances.
Further, in the step (2), heating and mixing are carried out at 35-85 ℃.
The technical scheme of the invention has the following advantages:
1. according to the water-in-oil type high internal phase emulsion for carrying the bitter substances, the bitter substance solution formed by the bitter substances and the solvent is used as an internal water phase, the lipid network structure is constructed in a mode of combining the liquid oil and the solid oil to be used as an external oil phase, the liquid oil and the solid oil are mixed for use, the gel condition of the lipid phase can be improved, the viscosity of the external oil phase is adjusted, the high internal phase emulsion with good stability can be formed, and the encapsulation rate of the bitter substances and the content of the bitter substances in the emulsion are improved. Meanwhile, the bitter substance solution of the internal water phase presents a closely packed structure due to the higher volume fraction of the internal phase, and the lipid network structure of the external oil phase and the closely packed internal phase structure limit the movement of internal liquid drops, thereby further ensuring the stability of the emulsion.
2. According to the water-in-oil type high internal phase emulsion carrying the bitter substances, the outer lipid layer provides a physical barrier, the combination of molecules of the bitter substances in the oil-in-oil type high internal phase emulsion and bitter receptors in oral cavities is blocked, the bad flavor of the bitter substances is effectively masked, the acceptable degree of consumers is improved, and meanwhile, the application of hydrophilic nutrient substances in oil-based foods can be expanded.
3. According to the water-in-oil type high internal phase emulsion carrying the bitter substances, the outer lipid layer prevents the internal bitter substances from being distributed and exposed in the stomach environment, the activity of the bitter substances is protected, and the bitter substances are ensured to have higher physiological activity before reaching the absorption site of the small intestine. During the digestion process of the small intestine, the outer lipid layer is gradually broken under the action of lipase and pancreatin, and the bitter substances in the inner part are slowly released.
4. The water-in-oil type high internal phase emulsion carrying the bitter substances, provided by the invention, can effectively slow down the oxidation process of lipid in the emulsion when the bitter substances in the water-in-oil type high internal phase emulsion are bitter peptides, and prolongs the shelf life of products.
5. The preparation method of the water-in-oil type high internal phase emulsion carrying the bitter substances, provided by the invention, can be used for preparing the water-in-oil type high internal phase emulsion carrying the bitter substances, which is high in encapsulation content, free of bitter taste and stable in gastric digestion activity, by only one step, and is simple and easy to operate. The method is mainly used in the field of food raw materials with strong pungent flavor, and can effectively improve sensory attributes of the food raw materials and improve consumer acceptance.
6. According to the preparation method of the water-in-oil type high internal phase emulsion for carrying bitter substances, the oil phase is heated, the internal water phase is slowly added into the system, the temperature of the system is gradually reduced to form a lipid phase network structure, the migration rate of liquid drops is reduced, the dispersion rotating speed is gradually increased in the process, so that stable emulsion is favorably formed, and after the internal water phase is completely rolled in, the stable emulsion is continuously dispersed, so that complete emulsification is ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a graph showing the appearance of freshly prepared emulsions of examples 1 to 3 of the present invention and emulsions after storage for 3 weeks at room temperature;
FIG. 2 is a graph showing the appearance of freshly prepared emulsion and inverted emulsion after preparation in example 4 of the present invention;
FIG. 3 is a graph of the appearance of freshly prepared emulsion and of the emulsion after it has been made according to example 5 of the present invention;
FIG. 4 is a graph showing the appearance of freshly prepared and inverted emulsions after preparation in example 6 of the present invention;
FIG. 5 is a graph of the appearance of a freshly prepared emulsion of example 1 of the invention and the emulsion after inversion and storage at room temperature for 1 week;
FIG. 6 is a graph showing the appearance of freshly prepared emulsion and inverted and prepared emulsion of comparative example 1 of the present invention after 10 min;
FIG. 7 is a graph showing the appearance of a freshly prepared emulsion and an inverted emulsion of comparative example 2 in accordance with the present invention;
FIG. 8 is a graph showing the effect of masking bitterness of a bitter substance in high internal phase emulsions obtained in examples 1 to 6 of the present invention;
FIG. 9 is a graph showing the evaluation of lipid oxidation effects of the high internal phase emulsions obtained in examples 1 to 3 of the present invention during storage;
FIG. 10 is a pictorial representation of a simulated in vitro digestion of the high internal phase emulsion obtained in example 3 of the present invention and a microstructure of the emulsion at the end of each digestion stage under a confocal laser microscope.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The preparation raw materials in the examples and comparative examples are as follows:
tea oil (green sea tea oil, Jiangxi Nanchang), palm oil (food grade, Guangzhou Langfeng), polyglycerol polyricinoleate (Dahe food, Henan Zhengzhou), wheat peptide (Jiangzhong, Jiangxi Nanchang, molecular weight below 1000 Da), coconut oil (sunshine coconut oil, Guangdong Guangzhou), linseed oil (flax public corporation, China inner Mongolia), olive oil (Betty, Spain), shortening (American flag, China Shanghai), collagen peptide (Jiangsu peptide Toyobo, Jiangsu Nanjing), coptis chinensis extract (Fufeng Si Nute, Shaanxi Bao chicken), traditional Chinese medicine liquid (Jiangxi province, traditional Chinese medicine, Jiangxi Nanchang).
The PBS buffer in the examples and comparative examples had a concentration of 5mM and a pH of 7.0 and was prepared as follows:
5mM Na was prepared separately2HPO4Solution and 5mM NaH2PO4Solution, 610mL Na2HPO4Solution with 390mL NaH2PO4The solutions were mixed and the pH was adjusted to 7.0 to prepare 5mM PBS buffer.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The raw materials or equipment used are all conventional products which can be obtained commercially, including but not limited to the raw materials or equipment used in the examples of the present application.
Example 1
This example provides a water-in-oil high internal phase emulsion carrying wheat peptide prepared as follows:
(1) dissolving 20g of wheat peptide powder in 380g of PBS buffer solution to obtain 400g of water phase (the mass concentration of the wheat peptide is 5%);
(2) heating 47.5g camellia oil, 47.5g food-grade palm oil and 5g polyglycerol ricinoleate at 70 ℃ and mixing uniformly to obtain 100g oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 8000rpm to 11000rpm at the speed of 1000rpm per minute in the process of adding the water phase into the oil phase, and continuously dispersing for 2min at 11000rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion for carrying the wheat peptide.
Example 2
This example provides a water-in-oil high internal phase emulsion carrying wheat peptide prepared as follows:
(1) dissolving 60g of wheat peptide powder in 340g of PBS buffer solution to obtain 400g of water phase (the mass concentration of the wheat peptide is 15%);
(2) heating and mixing 47.5g camellia oil, 47.5g food-grade palm oil and 5g polyglycerol ricinoleate at 70 ℃ to obtain 100g oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 8000rpm to 11000rpm at the speed of 1000rpm per minute in the process of adding the water phase into the oil phase, and continuing dispersing for 2min at 11000rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion carrying the wheat peptide.
Example 3
This example provides a wheat peptide-carrying water-in-oil high internal phase emulsion prepared as follows:
(1) dissolving 120g of wheat peptide powder in 280g of PBS buffer solution to obtain 400g of water phase (the mass concentration of the wheat peptide is 30%);
(2) heating and mixing 47.5g camellia oil, 47.5g food-grade palm oil and 5g polyglycerol ricinoleate at 70 ℃ to obtain 100g oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 8000rpm to 11000rpm at the speed of 1000rpm per minute in the process of adding the water phase into the oil phase, and continuing dispersing for 2min at 11000rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion carrying the wheat peptide.
Example 4
This example provides a collagen peptide-carrying water-in-oil high internal phase emulsion prepared as follows:
(1) dissolving 225g of collagen peptide powder in 225g of PBS buffer to obtain 440g of an aqueous phase (collagen peptide mass concentration is 50%);
(2) heating and mixing 34.4g soybean oil, 22g coconut oil and 3.6g polyglycerol ricinoleate at 65 deg.C to obtain 60g oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 7000rpm to 12000rpm at the speed of 800rpm per minute in the process of adding the water phase into the oil phase, and continuing dispersing at 12000rpm for 2min after the water phase is completely added to obtain the collagen peptide-carrying water-in-oil type high internal phase emulsion.
Example 5
The embodiment provides a water-in-oil type high internal phase emulsion for carrying traditional Chinese medicine decoction, which is prepared by the following steps:
(1) dissolving 150g of traditional Chinese medicine decoction in 275g of PBS buffer solution to obtain 425g of water phase (the mass concentration of the traditional Chinese medicine decoction is 35%);
(2) heating 52.5g of linseed oil, 18g of coconut oil and 4.5g of polyglycerol ricinoleate at 60 ℃ and uniformly mixing to obtain 75g of oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 6000rpm to 10000rpm at the speed of 500rpm per minute in the process of adding the water phase into the oil phase, and continuously dispersing for 2min at 10000rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion for carrying the traditional Chinese medicine decoction.
Example 6
This example provides a water-in-oil high internal phase emulsion carrying a water-soluble Coptidis rhizoma extract, which is prepared as follows:
(1) dissolving 45g of Coptidis rhizoma extract powder in 330g of PBS buffer solution to obtain 375g of water phase (the mass concentration of Coptidis rhizoma extract is 12%);
(2) heating and mixing 50g of olive oil, 70g of shortening and 5g of polyglycerol ricinoleate at 70 ℃ to obtain 125g of oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 7500rpm to 10500rpm at the speed of 1000rpm in the process of adding the water phase into the oil phase, and continuously dispersing for 2min at 10500rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion carrying the coptis chinensis extract.
Comparative example 1
The present comparative example provides a water-in-oil emulsion carrying wheat peptide prepared as follows:
(1) dissolving 20g of wheat peptide powder in 380g of PBS buffer solution to obtain 400g of water phase (the mass concentration of the wheat peptide is 5%);
(2) heating 95g camellia oil and 5g polyglycerol ricinoleate at 65 deg.C, and mixing to obtain 100g oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 8000rpm to 11000rpm at the speed of 1000rpm per minute in the process of adding the water phase into the oil phase, and continuing dispersing for 2min at 11000rpm after the water phase is completely added to obtain the water-in-oil type emulsion for carrying the wheat peptide.
Comparative example 2
The present comparative example provides a water-in-oil emulsion carrying wheat peptide prepared as follows:
(1) dissolving 20g of wheat peptide powder in 380g of PBS buffer solution to obtain 400g of water phase (the mass concentration of the wheat peptide is 5%);
(2) heating and mixing 95g of food-grade palm oil and 5g of polyglycerol ricinoleate at 65 ℃ to obtain 100g of oil phase;
(3) and (3) transferring the heated oil phase obtained in the step (2) into a beaker, placing the beaker into a high-speed dispersion machine, gradually increasing the rotating speed from 8000rpm to 11000rpm at the speed of 1000rpm per minute in the process of adding the water phase into the oil phase, and continuing dispersing for 2min at 11000rpm after the water phase is completely added to obtain the water-in-oil type emulsion for carrying the wheat peptide.
Experimental example 1 evaluation of emulsion stability
(1) Evaluation of storage stability of emulsions obtained in examples 1 to 3
After the preparation of the emulsions of examples 1 to 3, the emulsions were stored at room temperature for 3 weeks and the appearance of the emulsions was photographed.
And (4) analyzing results:
the aqueous phase in the emulsion prepared in example 1 was loaded with wheat peptide at a mass concentration of 5%, as shown in fig. 1, and the freshly prepared emulsion had a semisolid state inherent to the high internal phase emulsion and was not flowable after inversion, which was also attributed to the close packing of droplets within the high internal phase emulsion that squeezed into polyhedrons, rendering the emulsion to have a more viscous appearance. Phase separation occurred after 3 weeks storage at room temperature.
The aqueous phase in the emulsion prepared in example 2 was loaded with wheat peptide at a mass concentration of 15%, as shown in figure 1, and the freshly prepared emulsion also exhibited the structural features inherent to high internal phase emulsions, with the emulsion having a relatively high viscosity. After 3 weeks storage at room temperature, the texture of the emulsion changed and was flowable after inversion.
The aqueous phase in the emulsion prepared in example 3 was loaded with 30% by mass of wheat peptide, as shown in fig. 1, and the freshly prepared emulsion had a high viscosity and was not flowable after inversion. After 3 weeks of storage at room temperature, the structure of the emulsion was unchanged, showed a higher viscosity, restricted the migration between droplets, and still appeared in an inverted non-flowable state, demonstrating that the wheat peptide concentrated emulsion had better storage stability.
(2) Evaluation of stability of emulsions obtained in examples 4 to 6
Examples 4-6 emulsions were prepared and inverted or tilted and the appearance of the emulsion was photographed.
And (4) analyzing results:
the aqueous phase in the emulsion prepared in example 4 was loaded with collagen peptide at a mass concentration of 50%, as shown in fig. 2, the freshly prepared emulsion also had a high system viscosity and exhibited no flowability after inversion. In this example, the water phase mass fraction is already as high as 88% and the fat content is low. After storage, the emulsion still maintains the original viscosity and does not have unstable phenomena such as phase separation and the like, which shows that the high internal phase emulsion with good stability can be formed by increasing the mass fraction of the water phase and changing the composition of the liquid grease of the solid grease.
The aqueous phase in the emulsion prepared in example 5 carries the Chinese medicinal decoction with the mass concentration of 35%, as shown in fig. 3, the freshly prepared emulsion is viscous and has a certain viscosity, and the emulsion slowly flows after being inclined, but the emulsion is still stable after storage, and unstable phenomena such as phase separation, phase inversion and the like do not occur. In the embodiment, the mass fraction of the oil phase is only 15%, and a stable high internal phase emulsion can be formed although the solid grease accounts for a small proportion in the oil phase composition.
The aqueous phase in the emulsion prepared in example 6 was loaded with the coptis chinensis extract at a mass concentration of 12%, and as shown in fig. 4, the freshly prepared emulsion had a high viscosity and exhibited an inverted non-flowable phenomenon. In the embodiment, the mass fraction of the water phase is 75%, the solid oil accounts for a relatively large amount in the oil phase composition, the oil phase has a relatively high viscosity, the migration movement of liquid drops is limited, the emulsion also has relatively good stability after storage, the emulsion still keeps a viscous appearance, and no unstable phenomena such as phase separation occur.
(3) Evaluation of stability of emulsions obtained in example 1 and comparative examples 1 to 2
After the emulsion of the example 1 and the emulsion of the comparative examples 1 to 2 are prepared, the emulsion is stored in a standing way at room temperature, and the change of the appearance is recorded by photographing.
And (4) analyzing results:
the oil phase of example 1 contains a part of solid oil palm oil, which increases the viscosity of the external oil phase and limits the migration movement of liquid droplets, as shown in fig. 5, the freshly prepared emulsion shows the phenomenon of inversion and no flowability, has the general appearance characteristics of high internal phase emulsion, is stored at room temperature for 1 week, and has better stability and no instability phenomena such as phase separation, phase inversion and the like.
The oil phase of the comparative example 1 does not contain solid grease, the overall viscosity is low, liquid drops are easy to migrate and move, as shown in fig. 6, the freshly prepared emulsion has the phenomenon of inversion and flowability, the emulsion is unstable in oil-water two-phase separation after standing for 10min, and the emulsion is poor in stability.
The oil phase composition of comparative example 2 is mainly solid oil palm oil, the temperature of the oil phase is gradually reduced along with the addition of the water phase due to the single oil phase composition, the oil phase begins to solidify, and the viscosity is increased, but because the volume fraction of the internal water phase is too large, part of the internal water phase cannot be added into the system in the solidification process of the external phase, so that part of the internal water phase is remained outside, and a high internal phase emulsion with the volume fraction of the internal water phase being more than 74% cannot be formed, as shown in fig. 7, the emulsion formed in comparative example 2 is a common water-in-oil emulsion with certain plasticity and viscosity.
Experimental example 2 evaluation of emulsion Encapsulated efficiency
Removing residual bitter peptides on the surface of the emulsion by a water washing method, and determining the protein content by a biuret method to characterize the content of the bitter peptides.
Encapsulation efficiency (1-bitter peptide content removed by washing/total bitter peptide addition in internal aqueous phase) × 100% results analysis:
the calculated encapsulation efficiency of the emulsions of examples 1-4 is shown in Table 1.
TABLE 1 encapsulation efficiency of the emulsions of examples 1-4
| Sample (I) | Example 1 | Example 2 | Example 3 | Example 4 |
| Encapsulation efficiency | 98.85％ | 98.82％ | 95.76％ | 95.32％ |
The emulsions obtained in examples 1 to 4 all have a high bitter peptide encapsulation efficiency (> 95%), which indicates that the water-in-oil high internal phase emulsion provided by the invention can efficiently encapsulate bitter peptides. Bitter peptides are encapsulated as hydrophilic nutrients inside a water-in-oil high internal phase emulsion, and the presence of an external hydrophobic oil phase also limits leakage of the internal bitter peptides.
Experimental example 3 evaluation of bitterness intensity of emulsion
The bitter strength is measured by a scale method of sensory analysis, and is referred to ISO 8589-2007. 9 sensory evaluation members in the age range of 20-28 years were screened to evaluate bitterness. Preparing wheat peptide solutions with different mass concentrations as bitter standard substances, respectively setting the bitter intensities of pure water, a 10% wheat peptide aqueous solution, a 20% wheat peptide aqueous solution and a 30% wheat peptide aqueous solution to be 0, 5, 10 and 15, and training and evaluating members to score the standard substances so that the evaluating members can distinguish samples with different bitter intensities after training and the evaluation standards are relatively consistent. Sensory evaluation panelists rinsed their mouth with distilled water before evaluation, 1.0g of the evaluation sample was contained in the oral cavity for 10s, fully experienced bitterness, and rinsed with distilled water after spitting and scored. Rinse with distilled water between each two samples and leave a rest period of 15min to keep the oral cavity clean and reduce the impact between samples. Each sample was evaluated in duplicate 3 times.
And (4) analyzing results:
as shown in fig. 8, the concentration of wheat peptide carried by the water in the emulsion of example 1 was 5%, and the evaluation results of the sensory evaluation group showed that the 5% wheat peptide aqueous solution had a more pronounced bitter taste perception, with a bitter taste intensity evaluation value close to 3, whereas the high internal phase emulsion provided in example 1 had a much lower bitter taste intensity evaluation value and did not taste bitter, which also indicates that the lipid layer outside the emulsion served to block the binding of the wheat peptide molecules to the bitter taste receptors in the oral cavity, avoiding the perception of bitter taste.
Example 2 the concentration of wheat peptide carried by the aqueous phase in the emulsion was increased to 15% and the results of sensory panel evaluations showed that an aqueous solution of wheat peptide at 15% concentration had a strong bitterness intensity and a high bitterness score. However, the high internal phase emulsion provided in example 2 did not exhibit significant bitterness, with a bitterness intensity rating approaching 1, effectively masking the bitterness of wheat peptides.
Example 3 the concentration of wheat peptide carried by the water phase in the emulsion is increased to 30%, and the evaluation result of sensory evaluation group obviously shows that the wheat peptide water solution with the concentration of 30% has very strong bitter taste intensity and very obvious bitter taste. However, the high internal phase emulsion provided in example 3 exhibited effective bitterness masking, with a bitterness intensity evaluation value of slightly greater than 2, which is less than the bitterness value of a 5% aqueous wheat peptide solution, significantly masking the bitterness of the wheat peptide solution and increasing consumer acceptance.
Example 4 the aqueous phase of the emulsion carried collagen peptide at a concentration of 50% gave an aqueous solution of collagen peptide having a bitterness intensity score of 15, showing an extremely pronounced bitterness, whereas the encapsulated high internal phase emulsion had a bitterness intensity score of approximately 3, with a pronounced reduction in bitterness intensity.
In embodiment 5, the concentration of the traditional Chinese medicine decoction in the inner water phase is 35.3%, the bitter intensity of the traditional Chinese medicine decoction aqueous solution with the concentration is about 3 after evaluation by sensory evaluation groups, and meanwhile, the average score of the bitter intensity of the encapsulated high-inner phase emulsion is lower than 1, so that the bitter taste of the traditional Chinese medicine decoction is also obviously reduced, and the bad flavor is covered.
In example 6 in which the internal aqueous phase is a coptis extract solution, the bitterness intensity of a 12% coptis extract aqueous solution is close to 6, while the bitterness intensity of a water-in-oil high internal phase emulsion encapsulating the coptis extract at this concentration is only close to 1, the bitterness intensity is significantly reduced, which also indicates the masking effect of the water-in-oil high internal phase emulsion on the bad flavor of the coptis extract.
Experimental example 4 evaluation of lipid Oxidation of emulsion
The emulsions prepared in examples 1-3 were each placed in an oven at 40 ℃ to accelerate lipid oxidation. The extent of lipid oxidation was characterized by measuring Peroxide (POV), one of the major reaction products of lipid oxidation. Taking 0.3g of emulsion, adding 15mL of a mixture of isooctane and isopropanol (the volume ratio of isooctane to isopropanol is 3: 1) into a small centrifuge tube, fully shaking (10s, 3 times), centrifuging (1000g, 2min), taking 200 mu L of an organic layer (supernatant), adding the organic layer into 2.8mL of a mixture of methanol and butanol (the volume ratio of methanol to butanol is 2: 1), respectively adding 15 mu L of ammonium thiocyanate (3.94M) and 15 mu L of ferrous ion solution (0.132M barium chloride and 0.144M ferrous sulfate are mixed according to the volume ratio of 1: 1, passing through a 0.22 mu M filter membrane), reacting for 20min, measuring the absorbance value at the wavelength of 510nm, and calculating the concentration of peroxide in a sample by using an isopropylbenzene hydroperoxide standard curve. The blank was a water-in-oil high internal phase emulsion with an internal aqueous phase of PBS buffer. The assay was repeated 3 times for each sample.
And (4) analyzing results:
as can be seen from fig. 9, in the absence of wheat peptide in the internal phase, the peroxide value of the emulsion gradually increased with increasing storage time, which also indicates the occurrence of lipid oxidation in the emulsion.
The inner water phase of the emulsion obtained in the examples 1 to 3 is respectively encapsulated with the wheat peptide solution with the mass concentration of 5%, 15% and 30%, and as can be seen from fig. 9, the peroxide concentration in the emulsion is obviously reduced in the examples 1 to 3. At the same time, the peroxide value in the emulsion decreased with increasing wheat peptide concentration, indicating that wheat peptide concentration affects lipid oxidation reactions in the emulsion.
Experimental example 5 evaluation of digestion protection effect of wheat peptide
The protective capacity of the emulsion obtained in example 3 for the gastric digestion of wheat peptide was determined by simulating the digestion in the gastrointestinal tract.
Experimental samples were prepared according to example 3, wherein the inner aqueous phase was stained with FITC and the oil phase was stained with Nile Red. And (3) after the samples are prepared, performing an in-vitro simulated digestion experiment, and respectively transferring the emulsion sample after the oral digestion is finished, the emulsion sample after the gastric digestion is finished and the digestive juice sample after the small intestine digestion is finished into a confocal dish to observe the microstructure of the samples.
The digestive fluid used for in vitro simulated digestion was prepared according to the following method:
1.594mg/ml sodium chloride, 0.328mg/ml ammonium nitrate, 0.636mg/ml monopotassium phosphate, 0.202mg/ml potassium chloride, 0.308mg/ml potassium citrate, 0.021mg/ml sodium dihydrogen urate, 0.198mg/ml urea and 0.146mg/ml sodium lactate are dissolved in distilled water to prepare the simulated oral digestive juice. A simulated oral working fluid (SSF) was prepared by dissolving oral mucosal protein (3mg/ml) therein in advance.
Simulated Gastric Fluid (SGF) consisted of 2mg/ml sodium chloride and hydrochloric acid (adjusting the system pH to 1.2) and pepsin was dissolved in 3.2 mg/ml.
Simulated Intestinal Fluid (SIF) consists of saline solution, enzyme solution and bile salt solution. The salt solution was formulated from 31.58mg/ml calcium chloride, 218.7mg/ml sodium chloride. Pancreatin 24mg/ml, lipase 24mg/ml, and bile salt 189mg/ml were dissolved in a phosphate buffer (5mmol/L, pH 7.0).
The operation of each stage of in vitro simulated digestion is as follows:
oral stage: a1.0 g sample of the high internal phase emulsion, 7.5mL SSF and 6.5mL PBS (5mM, pH7.0) was placed in a glass vial to adjust the pH to 6.8 and digested in a 37 ℃ constant temperature shaker water bath for 10 min.
Gastric stage: after the digestion of the oral cavity is finished, 15mL of SGF is added into a glass bottle, the pH is adjusted to 2.5, and the mixture is digested for 2 hours in a water bath of a constant temperature shaker at 37 ℃.
The small intestine stage: after the completion of the digestion, the pH of the system was adjusted to 7.0, and 1.5mL of a salt solution, 3.5mL of a bile salt solution, 2.5mL of a lipase solution, and 2.5mL of a pancreatin solution were added. And titrating by using a pH constant titrator to keep the system pH7.0 in the small intestine digestion process.
And (4) evaluating the results:
as shown in figure 10, at the end of digestion in the mouth and stomach, the emulsion still maintains the structure of the high internal phase emulsion, the outer lipid layer remains intact, and the wheat peptide in the internal aqueous phase is well protected, thereby preventing the wheat peptide from being exposed in the stomach environment to change the original physiological activity. When the emulsion reaches the digestion stage of the small intestine, the outer lipid layer is gradually broken along with the action of lipase in the small intestine, and the inner wheat peptide is released to reach the action site of the small intestine and be further absorbed and utilized by the human body. The water-in-oil type high internal phase emulsion prepared by the invention ensures that the wheat peptide still has better physiological activity and structural integrity before reaching the absorption action site.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A water-in-oil type high internal phase emulsion for carrying bitter substances is characterized in that the raw materials comprise a water phase and an oil phase,
the aqueous phase comprises a bitter tasting substance and a solvent;
the oil phase comprises liquid oil, solid oil and polyglycerol ricinoleate.
2. A water-in-oil high internal phase emulsion carrying a bitter substance according to claim 1, wherein the bitter substance has a mass concentration in the water phase of 0.1 to 50%, preferably 5 to 50%.
3. A water-in-oil high internal phase emulsion carrying bitter substances according to claim 1, characterized in that the mass concentration of polyglycerol ricinoleate in the oil phase is 2% to 10%, preferably 4% to 6%; the mass ratio of the liquid grease to the solid grease is 0.5-10: 1, preferably 0.7 to 2.9: 1.
4. the water-in-oil type high internal phase emulsion carrying a bitter substance according to claim 1, wherein the oil phase is 10 to 90% by weight, preferably 12 to 25% by weight.
5. The water-in-oil high internal phase emulsion carrying a bitter tasting substance of claim 1, wherein the bitter tasting substance comprises at least one of wheat peptide, collagen peptide, soybean peptide, casein peptide, rice protein peptide, protein hydrolysate, herbal decoction, herbal extract.
6. A water-in-oil high internal phase emulsion carrying bitter substances according to claim 1, wherein the solvent comprises at least one of distilled water, PBS buffer at a concentration of 5 to 500mM, citrate buffer at a concentration of 5 to 500mM, preferably PBS buffer at a concentration of 5 mM.
7. A water-in-oil high internal phase emulsion carrying a bitter tasting substance according to claim 1, characterized in that,
the liquid oil comprises at least one of camellia oil, corn oil, olive oil, medium chain triglyceride, linseed oil, castor oil, walnut oil, algae oil, peony seed oil, peanut oil, rapeseed oil, soybean oil, perilla seed oil and sunflower seed oil;
the solid oil comprises at least one of palm oil, coconut oil, shortening, butter and animal oil.
8. A process for preparing a water-in-oil high internal phase emulsion carrying bitter substances according to any of claims 1 to 7, comprising the steps of:
(1) dissolving bitter substance in solvent to obtain water phase;
(2) heating and mixing liquid oil, solid oil and polyglycerol ricinoleate to obtain an oil phase;
(3) and adding the water phase into the heated oil phase for homogeneous dispersion to obtain the water-in-oil high internal phase emulsion carrying the bitter substances.
9. The method of preparing a water-in-oil high internal phase emulsion carrying bitter substances of claim 8 wherein in step (3) the homogeneous dispersion comprises: and in the process of adding the water phase into the oil phase, gradually increasing the rotating speed from 6000rpm to 8000rpm to 10000rpm to 14000rpm at the speed of 500rpm to 1000rpm per minute, and continuously dispersing for 1 min to 3min at 10000rpm to 14000rpm after the water phase is completely added to obtain the water-in-oil type high internal phase emulsion carrying the bitter substances.
10. The method for preparing a water-in-oil high internal phase emulsion carrying a bitter substance according to claim 8, wherein in the step (2), the mixture is heated at 35 to 85 ℃.
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| CN115606788A (en) * | 2022-09-30 | 2023-01-17 | 江苏省农业科学院 | Preparation and detection method of burdock cellulose nanocrystalline-chitosan high internal phase emulsion |
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