CN111481503A - Vitamin D3-loaded nano calcium carbonate pickering emulsion and preparation method and application thereof - Google Patents
Vitamin D3-loaded nano calcium carbonate pickering emulsion and preparation method and application thereof Download PDFInfo
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- CN111481503A CN111481503A CN202010273258.4A CN202010273258A CN111481503A CN 111481503 A CN111481503 A CN 111481503A CN 202010273258 A CN202010273258 A CN 202010273258A CN 111481503 A CN111481503 A CN 111481503A
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- 239000011647 vitamin D3 Substances 0.000 title claims abstract description 112
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- A—HUMAN NECESSITIES
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/15—Vitamins
- A23L33/155—Vitamins A or D
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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
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- A23L33/16—Inorganic salts, minerals or trace elements
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/59—Compounds containing 9, 10- seco- cyclopenta[a]hydrophenanthrene ring systems
- A61K31/593—9,10-Secocholestane derivatives, e.g. cholecalciferol, i.e. vitamin D3
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- 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
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Abstract
The invention discloses a vitamin D3-loaded nano calcium carbonate pickering emulsion as well as a preparation method and application thereof, belonging to the technical field of food and medicine. A preparation method of vitamin D3-loaded nano calcium carbonate pickering emulsion comprises the following steps: (1) preparing a nano calcium carbonate suspension; (2) high static pressure treatment: carrying out high static pressure treatment on the nano calcium carbonate suspension to obtain nano calcium carbonate dispersion; (3) mixing vitamin D3 with edible oil, and stirring in dark to obtain vitamin D3 oil solution; (4) mixing the nano calcium carbonate dispersion liquid with a vitamin D3 oil solution, shearing and homogenizing to obtain the nano calcium carbonate composite material. The invention disperses through high static pressure treatment, which can obviously reduce the agglomeration degree of the nano calcium carbonate and improve the dispersibility of nano calcium carbonate particles, so that the finally prepared nano calcium carbonate Pickering emulsion loaded with vitamin D3 has good stability, viscoelasticity and biological responsiveness.
Description
Technical Field
The invention belongs to the technical field of food and medicine, and particularly relates to a vitamin D3-loaded nano calcium carbonate pickering emulsion as well as a preparation method and application thereof.
Background
Pickering emulsion is a kind of emulsion stabilized by nano/micron solid particles, has the characteristics of good stability, aggregation resistance, flocculation resistance, austenitizing resistance, and the like, and has wide application in the fields of food, cosmetics, medicines, and the like. The Pickering emulsion can be used as a drug embedding and delivery carrier and can improve the stability of the loaded drug. The type of emulsifier and oil is the basis for the functional design of pickering emulsions: (1) the physical and chemical structure, the biocompatibility and the digestion characteristic of the particle emulsifier are more key factors for determining the use, the structure and the performance of the pickering emulsion; with the development of nanotechnology, various edible raw materials, inorganic and organic, including protein, polysaccharide and inorganic salt, are made into nano-scale particles and are gradually applied to Pickering emulsion; (2) the volume fraction of the oil phase can regulate and control the microstructure of the pickering emulsion, and when the volume fraction of the internal phase is more than 74 percent, the formed emulsion is called high internal phase pickering emulsion; in high internal phase "oil-in-water" emulsions, the dispersed phase of oil droplets has deformed into multi-faceted "liquid cells" divided by a thin film of continuous phase, and the oil droplets flocculate into a gel-like network structure. Therefore, the high internal phase oil-in-water pickering emulsion also has the texture of a semi-solid food, can endow the product with certain physical strength and shape, and provides convenience for processing, transportation and storage.
The nano calcium carbonate is fine particles with the particle size less than or equal to 0.1 mu m and different shapes (such as cubic, rod-shaped or spherical). Compared with the traditional calcium carbonate with the particle size of more than micron, the nano calcium carbonate is easier to be absorbed by human body, and the calcium bioavailability is high, and the calcium supplement effect is better when the particle size is smaller. In recent years, nano-sized calcium carbonate is considered to be a novel and more efficient calcium-fortified raw material, and has attracted much attention in the fields of food, medicine, and biomedicine. In terms of emulsification activity, particle size, morphology, surface wettability are key factors for solid particles as pickering emulsifiers. Studies have shown that in order to obtain a predetermined average particle size of the emulsion, the size of the solid particles used is at least an order of magnitude lower than the average particle size of the target emulsion, and the smaller the particle size of the emulsifier, the more beneficial the emulsifying capacity of the calcium carbonate particles is. However, "bare" nano calcium carbonate particles are easily agglomerated during the synthesis process, and the formation of agglomerates results in a great loss of the emulsifying properties of nano calcium carbonate. Although the surface modification strategy can slow down the aggregation of particles in the synthesis process, many chemical modifiers have toxicity, and limit the application of the modified nano calcium carbonate in food, medicines and biomedicine. Therefore, the method has important significance in reducing the aggregation degree of the nano calcium carbonate by adopting a non-chemical/non-additive physical method and further improving the emulsification stability of the nano calcium carbonate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of vitamin D3-loaded nano calcium carbonate pickering emulsion.
The invention also aims to provide the vitamin D3-loaded nano calcium carbonate pickering emulsion prepared by the preparation method.
The invention further aims to provide application of the vitamin D3 loaded nano calcium carbonate pickering emulsion.
The purpose of the invention is realized by the following technical scheme:
a preparation method of vitamin D3-loaded nano calcium carbonate pickering emulsion comprises the following steps:
(1) suspension of nano calcium carbonate: mixing nano calcium carbonate powder with water to prepare nano calcium carbonate suspension;
(2) high static pressure treatment: carrying out high static pressure treatment on the nano calcium carbonate suspension liquid obtained in the step (1) to obtain uniformly dispersed nano calcium carbonate dispersion liquid;
(3) vitamin D3 oil solution: mixing vitamin D3 with edible oil, stirring in dark condition to completely dissolve vitamin D3 to obtain vitamin D3 oil solution;
(4) and (3) mixing the nano calcium carbonate dispersion liquid obtained in the step (2) with the vitamin D3 oil solution obtained in the step (3), and shearing and homogenizing to obtain the vitamin D3-loaded nano calcium carbonate pickering emulsion.
The nano calcium carbonate powder in the step (1) is food-grade nano calcium carbonate powder.
The content of the nano calcium carbonate in the food-grade nano calcium carbonate powder is not lower than 95 percent.
The average particle size of the nano calcium carbonate is preferably 30-250 nm; more preferably 30 to 150 nm.
The concentration of the nano calcium carbonate suspension in the step (1) is preferably 10-150 mg/m L, and more preferably 20-100 mg/m L.
The water in the step (1) comprises at least one of deionized water and pure water; preferably deionized water.
The nano calcium carbonate suspension in the step (1) is preferably prepared by the following steps: adding nano calcium carbonate powder into water or adding water into nano calcium carbonate powder, and stirring at room temperature to obtain the nano calcium carbonate powder; preferably, the nano calcium carbonate powder is obtained by adding water and stirring at room temperature.
The stirring time is preferably 2-12 h; more preferably 2 to 6 hours.
The stirring speed is preferably 200-800 rpm; more preferably 200 to 500 rpm.
The room temperature is 0-40 ℃; preferably 10-35 ℃; further preferably 20-30 ℃; more preferably 24 to 27 ℃.
The high static pressure treatment in the step (2) is kept for 10-50 min at 200-600 MPa; preferably, the pressure is maintained at 250 to 400MPa for 20 to 45 min.
The high static pressure treatment is completed in a high static pressure device; and taking out the nano calcium carbonate suspension after high static pressure treatment and pressure relief.
The vitamin D3 in the step (3) is food grade vitamin D3.
The food-grade vitamin D3 is preferably solid powder obtained by sieving with a 100-mesh sieve, and the content of the solid powder is not less than 98%.
The edible oil in the step (3) is preferably at least one of medium-chain fatty acid, fish oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, sunflower seed oil, walnut oil, camellia oil, corn germ oil and olive oil; preferably at least one of medium chain fatty acids, fish oil, soybean oil and corn oil.
The concentration of the vitamin D3 in the vitamin D3 oil solution in the step (3) is 5-1000 IU/m L, and preferably 50-200 IU/m L.
The stirring time in the step (3) is preferably 0.5-3 h; more preferably 0.5 to 1 hour.
The stirring speed in the step (3) is preferably 200-800 rpm; more preferably 200 to 500 rpm.
And (3) mixing the nano calcium carbonate dispersion liquid and the vitamin D3 oil solution in the step (4) preferably according to a volume ratio of 3: 7-2: 8.
The nano calcium carbonate and the vitamin D3 are preferably mixed according to the weight ratio of 10-150 mg: mixing 5-1000 IU; more preferably, the weight ratio of 20-100 mg: mixing at a ratio of 50-200 IU.
The shearing homogenization method in the step (4) is preferably a high-speed shearing homogenization method.
The shearing homogenization condition in the step (4) is preferably that the shearing is carried out for 1-20 min at 5000-20000 rpm; more preferably: shearing at 6000-15000 rpm for 3-15 min; most preferably: shearing at 7000-12000 rpm for 5-15 min.
The vitamin D3-loaded nano calcium carbonate pickering emulsion is prepared by the preparation method.
The vitamin D3-loaded nano calcium carbonate pickering emulsion is an edible high-internal-phase pickering oil-in-water emulsion consisting of nano calcium carbonate, vitamin D3 and edible oil.
The average particle size of the vitamin D3-loaded nano calcium carbonate pickering emulsion is 30-100 mu m, the content of vitamin D3 is 3-800 IU per gram of emulsion, and the content of nano calcium carbonate is 5-45 mg per gram of emulsion; preferably, the average particle size of the vitamin D3-loaded nano calcium carbonate pickering emulsion is 56.4-80.7 mu m, the content of vitamin D3 is 23-115 IU per gram of emulsion, and the content of calcium in the nano calcium carbonate is 2.4-7.7 mg per gram of emulsion.
The vitamin D3-loaded nano calcium carbonate pickering emulsion is applied to food, cosmetics and medicines.
Compared with the prior art, the invention has the following advantages and effects:
(1) the edible high internal phase pickering oil-in-water emulsion composed of nano calcium carbonate, vitamin D3 and edible oil is prepared by the method. The Pickering emulsion system has the structural characteristic of 'core-shell', the nano calcium carbonate serves as 'shell' and is irreversibly adsorbed on the surface of oil drops, and meanwhile, the nano calcium carbonate serves as an emulsion stabilizer and a calcium supplement, and the oil drops serve as 'core' structure and contain vitamin D3. By setting the addition amount of the vitamin D3 and the nano calcium carbonate, the calcium carbonate-vitamin D3 composite emulsion with any proportion can be obtained, and the high internal phase pickering oil-in-water emulsion with the average particle size of about 50-100 mu m is prepared, so that the high internal phase pickering oil-in-water emulsion has good properties of good stability, formability, convenience in transportation and the like. After being taken orally, the calcium supplement can supplement calcium and vitamin D3 at the same time, and has wide application prospect.
(2) The edible pickering emulsion with good biological responsiveness, good calcium supplement effect, high stability and strong excipient is synthesized by using food-grade raw and auxiliary materials; the digestive characteristics of the nano calcium carbonate are regulated and controlled through material design and size optimization, so that the bioavailability of calcium can be improved, and the burden of the gastrointestinal tract is reduced; the calcium supplement effect is promoted by loading the vitamin D3 and realizing the slow release of the vitamin D in the digestive tract.
(3) The invention disperses through high static pressure treatment, which can obviously reduce the agglomeration degree of the nano calcium carbonate and improve the dispersibility of nano calcium carbonate particles, so that the finally prepared nano calcium carbonate Pickering emulsion loaded with vitamin D3 has good stability, viscoelasticity and biological responsiveness.
Drawings
Fig. 1 is a schematic structural diagram of a nano calcium carbonate-pickering high internal phase (oil-in-water) emulsion according to the present invention.
Fig. 2 is a transmission electron microscope analysis diagram of nano calcium carbonate before and after high hydrostatic pressure.
Fig. 3 is a distribution diagram of the transmission particle size of nano calcium carbonate before and after high static pressure.
FIG. 4 is a particle size distribution diagram of a nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared by example 1 and a control group.
FIG. 5 is a physical diagram of a nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention.
FIG. 6 is a diagram of the rheological analysis of the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention.
FIG. 7 is a microscopic analysis and physical representation of the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention after 30 days of storage at 25 ℃ and 4 ℃.
FIG. 8 is a graph showing the content change of vitamin D3 in the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention after being stored at 25 ℃ for 30 days.
FIG. 9 is a graph showing the results of the emulsion structure change of the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention in simulated gastric and intestinal fluids.
FIG. 10 is a graph showing the results of the release rate of calcium ions from the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention after being treated with simulated gastric fluid.
FIG. 11 is a graph showing the retention of vitamin D3 in the in vitro simulated gastrointestinal digestion of the nano calcium carbonate Pickering high internal phase (oil-in-water) emulsion prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
The starting materials and reagents used in the following examples:
raw materials:
spherical nano calcium carbonate powder is prepared by self and is food grade; the purity is more than 98 percent, and the average grain diameter is 80 nm; the nano calcium carbonate is prepared by a batch carbonization method, and comprises the following steps: 1) lime milk preparation: weighing a certain mass of CaO according to the proportion of 1:1.5 (namely CaO: H) of grey water2Adding 1g of O-1.5 m L) into water at 85-90 ℃, digesting for 4 hours under sealed stirring (the rotating speed is 250rpm), and obtaining Ca (OH)2Sieving the suspension with 200 mesh sieve, filtering to remove part of CaO particles which are not completely digested, sealing, standing and aging for 24h, 2) carbonizing, preparing 100L Ca (OH) with mass concentration of 4%2Introducing 25-30% CO2Until the pH value is reduced to 7, the carbonization temperature is 25 ℃, and CO is added2The flow rate is 30L/min, 3) centrifugation and washing are carried out, namely the carbonized serous fluid is centrifuged for 20min by a three-foot centrifuge with the rotating speed of 2000rpm, water is used for washing for 2 times, supernatant is discarded, 4) drying is carried out, the wet nano calcium carbonate is dried for 12h under vacuum at the temperature of 60 ℃, 5) crushing is carried out, the crushing is carried out by a mechanical crusher, and the nano calcium carbonate powder is obtained after 200-mesh sieving.
Vitamin D3, food grade, commercially available, purity > 98%, purchased from Wuhan Xiangdi food ingredients, Inc.;
medium chain fatty acids, food grade, available from Britz Networks sdn.
Soybean oil, food grade, purchased from yihaijiali golden dragon fish food shares, ltd;
corn oil, food grade, purchased from yihaijiali golden dragon fish food oil food products, ltd;
the fish oil is food grade and is purchased from Shaanxi Baozao biotechnology limited company.
Example 1
1. Ingredients
Preparing food-grade nano calcium carbonate powder into nano calcium carbonate suspension with the concentration of 50mg/m L by adding water for later use;
2. high hydrostatic dispersion
Placing the nano calcium carbonate suspension in the step 1 in a high static pressure device, and keeping the nano calcium carbonate suspension for 20min under the condition that the working pressure is 300MPa to obtain nano calcium carbonate dispersion liquid;
3. vitamin D3 oil solution
Vitamin D3 oil solution, adding food grade vitamin D3 into medium chain fatty acid solution, stirring at 200rpm under dark condition at room temperature for 1h to dissolve vitamin D3 completely to obtain 100IU/m L vitamin D3 oil solution;
4. pickering emulsion preparation
Mixing the nano calcium carbonate dispersion liquid obtained in the step 2 and the vitamin D3 oil solution obtained in the step 3 according to the volume ratio of 3:7, and shearing and homogenizing at a high speed of 8000rpm for 15min to obtain a vitamin D3-loaded nano calcium carbonate pickering emulsion; meanwhile, mixing the nano calcium carbonate suspension obtained in the step 1 and the vitamin D3 oil solution obtained in the step 3 according to the volume ratio of 3:7, and shearing and homogenizing at a high speed of 8000rpm for 15min to obtain a control.
5. Detection of
The structure schematic diagram of the prepared vitamin D3-loaded nano calcium carbonate pickering emulsion is shown in figure 1.
The size and the appearance of the nano calcium carbonate before and after high static pressure dispersion are changed: the size and morphology of the nano calcium carbonate are observed by a transmission electron microscope (Tecnai G2F 20, FEI company, USA), as shown in figure 2, a plurality of 50-200 nm nano calcium carbonate particles are agglomerated into aggregates with the size larger than 2 microns before high static pressure treatment, and after high static pressure treatment, the aggregates are dispersed into single or oligomers with the size of 60-150 nm and small aggregates with the size of about 300 nm. The results of fig. 2 show that the high static pressure treatment can obviously reduce the agglomeration degree of the nano calcium carbonate and improve the dispersibility of the nano calcium carbonate particles.
The evaluation particle size of the nano calcium carbonate was measured by a dynamic light scattering instrument (Zetasizer ZS90, malvern, uk), and the results of fig. 3 showed that the average particle size of the nano calcium carbonate before the high static pressure treatment was 2600 nm; after high static pressure treatment, the particle size distribution of the nano calcium carbonate is obviously reduced, and the average particle size is also reduced from 2600nm to 80 nm.
The particle size distribution of the nano calcium carbonate pickering emulsion is shown in fig. 4, and the particle size distribution of the vitamin D3-loaded nano calcium carbonate pickering emulsion is detected to be 29-224 μm by a laser diffractometer (Mastersizer 3000, Marvin, England); the particle size distribution of the control group is 37-255 mu m.
Average particle size of the nano calcium carbonate pickering emulsion containing vitamin D3: the average particle size of the nano calcium carbonate Pickering emulsion containing vitamin D3 is 64.3 mu m by static light scattering method detection; the average particle size of the control group was 70.6. mu.m.
Physical diagram of emulsion: the physical image of the emulsion taken by a digital camera is shown in fig. 5, the appearance of the nano calcium carbonate pickering (oil-in-water) emulsion is milky, and the emulsion placed in a bottle does not fall off after being inverted. However, emulsions prepared without the high hydrostatic pressure dispersed nano calcium carbonate are significantly delaminated. Therefore, the uniformity of the emulsion is improved after the nano calcium carbonate is subjected to high static pressure dispersion pretreatment.
The calcium content of the nano calcium carbonate Pickering (oil-in-water) emulsion is measured by utilizing ion chromatography to measure the calcium content in the nano calcium carbonate Pickering solution to be 5.7mg/g, the calcium content in a control group is 5.6mg/g, the chromatographic conditions are that a sample is separated by adopting an IonPac-CS12A (4 × 250mM) analysis column and an IonPac-CG12A (4 × mM) protection column, the mobile phase is 20mM methanesulfonic acid, the flow rate is 1m L/min, a detector is an electric conductivity detector, a CSRS cation inhibitor (4mM) is selected as an inhibitor, and the sample pretreatment method comprises the steps of mixing a proper amount of sample with 20mM methanesulfonic acid solution, diluting to a proper concentration, passing through a 0.22 mu m filter membrane, and taking 25 mu L filtrate for measurement.
The vitamin D3 loading capacity of the nano calcium carbonate Pickering emulsion is measured by utilizing high performance liquid chromatography to measure that the content of vitamin D3 in the nano calcium carbonate Pickering emulsion is 47IU/g, the content of vitamin D3 in a control group is 45IU/g, a detection method is modified according to the methods of Zhao Xiaoyang and the like (Zhao Xiaoyang, Qian Liang, Yu Zheng Gao, vitamin D _3 oil detection technical research [ J ]. China livestock journal, 2014,50(24):74-77+81.), the chromatographic conditions are as follows, (1) a chromatographic column is a C18 column with the inner diameter of 4.6mm and the length of 250mm and the granularity of 5 mu m, (2) a mobile phase is 100% methanol, (3) the flow rate is 1.0m L/min, (4) the column temperature is 25 ℃, (5) the detection wavelength is 254nm, (6) the sample feeding amount is 20 mu L, after 30 days of 25 ℃, the content of the vitamin D3 of the sample in the example 1 is 46IU/g, and the content in the control group is reduced to 64 IU/39 g.
Calcium content determination of nano calcium carbonate pickering (oil-in-water) emulsion viscoelasticity: the results of the modulus test of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion prepared in example 1 by a rheometer are shown in fig. 6, where the storage modulus and the loss modulus of the emulsion obtained in example 1 are 1132Pa and 173Pa, respectively, and then the storage modulus: loss modulus 6.5, indicating that the emulsion has viscoelastic properties, which is characteristic of a semi-solid food. The storage modulus and the loss modulus of the emulsion of the control group are 770Pa and 114Pa, respectively, and then the storage modulus is: loss modulus 6.8. Generally, the greater the storage modulus of a semi-solid system, the higher the viscosity and thus the more beneficial it is in sequestering oxygen in air. As can be seen, vitamin D in the high hydrostatic group prepared in example 13The retention rate of (2) is higher.
Emulsion microarchitecture diagram: the results of microscopic analysis of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion after 30 days storage at 25 ℃ and 4 ℃ respectively are shown in fig. 7. As can be seen from fig. 7, after 30 days of storage at 25 ℃ and 4 ℃ respectively, the oil droplets in the emulsion were stacked into clusters and deformed, and there was no significant difference in the microstructure of the emulsion after storage compared to the control (fresh emulsion stored for 0 days), indicating that the emulsion had good stability.
Vitamin D3 content change chart: the vitamin D3 content of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion after 30 days of storage at 25 ℃ (detected by high performance liquid chromatography, supra) is shown in fig. 8. As can be seen from fig. 8, the stability of vitamin D3 loaded in the emulsion of the experimental group was good, and the retention rate after storage was 98% or more. The emulsion obtained without high hydrostatic pressure dispersion of the control group showed a reduction in vitamin D3 retention of 89% after 30 days of storage at 25 ℃.
The biological responsiveness of the emulsion is that the preparation of simulated gastric juice is carried out by adding 2g NaCl, 7m L concentrated hydrochloric acid with mass concentration of 37% and 3.2g pig pepsin (enzyme activity is 250U/mg) into a beaker, using deionized water to fix the volume to 1L, adjusting the pH to 2.0, and dispersing under high pressure to form the emulsionDiluting the solution with deionized water to obtain dilute emulsion with oil content of 0.5% by mass, mixing 30g of dilute emulsion with simulated gastric juice at a mass ratio of 1:1, adjusting pH of the mixed solution to 2.0 with dilute hydrochloric acid (mass concentration of 1%), heating the mixture in 37 deg.C water bath for 2h at a stirring speed of 200rpm to digest the simulated gastric juice, transferring the stomach paste sample to 200m L beaker, placing the beaker in 37 deg.C water bath, maintaining the temperature for 30min, adjusting pH of the solution to 7.0, and adding 1.5m L inorganic salt solution (CaCl containing 0.25 mol/L) into the beaker2And 3.75 mol/L of NaCl), 3.5m L of bile salt solution (54mg/m L) was added, then, the pH of the above mixture was adjusted back to 7.0 with 1 mol/L of NaOH emulsion, finally, 2.5m L of pancreatic lipase solution (24mg/m L) was added to initiate fat digestion reaction, the simulated intestinal fluid digestion reaction was performed at 37 ℃ for 2 hours from the time of pancreatic lipase addition, the whole process was accompanied by mechanical stirring at a stirring speed of 200rpm, the pH of the reaction solution was measured every 2min during simulated intestinal fluid digestion, and an appropriate amount of NaOH solution (0.1 mol/L) was added to adjust the pH back to 7.0. the emulsion structure change of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion in the simulated gastrointestinal fluid was observed at excitation wavelength and emission wavelength of 540nm and 590nm, respectively, using a fluorescence microscope, as shown in FIG. 9, and the results of the decomposition of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion showed that the nano calcium carbonate biological calcium carbonate aqueous phase (oil-in-simulated gastric fluid had a biological water response pattern of calcium carbonate.
Release rate of calcium ion: the simulated gastric juice is prepared according to Chinese pharmacopoeia. The emulsion sample was mixed with simulated gastric fluid at a volume ratio of 1:1, then after adjusting the pH to 2.0, finally incubated in a 37 ℃ water bath for 2 h. After digestion is finished, the content of calcium ions in the digestive juice is detected by adopting an ion chromatography method, and the detection method is the same as the above. The release rate of calcium ion of the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion after being treated by simulated gastric fluid is shown in fig. 10. As can be seen from fig. 10, calcium ions in the nano calcium carbonate are almost completely decomposed in the simulated gastric fluid.
The retention rate of vitamin D3 after the emulsion is treated by simulated gastric juice and intestinal juice in sequence: the retention of vitamin D3 after simulated digestion of gastric and intestinal fluids by the nano calcium carbonate pickering high internal phase (oil-in-water) emulsion is shown in fig. 11. As can be seen from FIG. 11, the retention rate of vitamin D3 was 68% after simulated digestion of gastric juice and intestinal juice.
Example 2
1. Ingredients
Preparing food-grade nano calcium carbonate powder into nano calcium carbonate suspension with the concentration of 40mg/m L by adding water for later use;
2. high hydrostatic dispersion
Placing the nano calcium carbonate suspension obtained in the step 1 in a high static pressure device, and keeping the nano calcium carbonate suspension for 30min under the condition that the working pressure is 250MPa to obtain nano calcium carbonate dispersion liquid;
3. vitamin D3 oil solution
Vitamin D3 oil solution is prepared by adding food grade vitamin D3 into corn oil, stirring at 300rpm under dark condition at room temperature for 2 hr to dissolve vitamin D3 completely to obtain 200IU/m L vitamin D3 oil solution;
4. pickering emulsion preparation
Mixing the nano calcium carbonate dispersion liquid obtained in the step 2 and the vitamin D3 oil solution obtained in the step 3 according to the volume ratio of 2:8, and carrying out high-speed shearing and homogenization for 8min at the shearing speed of 7000rpm to obtain a vitamin D3-loaded nano calcium carbonate pickering emulsion;
5. detection of
Average particle size of the nano calcium carbonate pickering emulsion containing vitamin D3: the average particle size of the nano calcium carbonate Pickering emulsion detected by a static light scattering method is 80.7 mu m.
And (3) measuring the calcium content of the nano calcium carbonate pickering emulsion: the content of calcium in the nano calcium carbonate Pickering solution is measured by ion chromatography and is 3.1 mg/g.
And (3) measuring the vitamin D3 load capacity of the nano calcium carbonate pickering emulsion: the content of vitamin D3 in the nano calcium carbonate Pickering emulsion is measured by high performance liquid chromatography and is 115 IU/g.
Example 3
1. Ingredients
Preparing food-grade nano calcium carbonate powder into nano calcium carbonate suspension with the concentration of 20mg/m L by adding water for later use;
2. high hydrostatic dispersion
Placing the nano calcium carbonate suspension in the step 1 in a high static pressure device, and keeping the nano calcium carbonate suspension for 30min under the condition that the working pressure is 400 MPa;
3. vitamin D3 oil solution
Vitamin D3 oil solution, adding food grade vitamin D3 into soybean oil, stirring at 400rpm under dark condition at room temperature for 3 hr to dissolve vitamin D3 completely to obtain 50IU/m L vitamin D3 oil solution;
4. pickering emulsion preparation
Mixing the nano calcium carbonate dispersion liquid obtained in the step 2 and the vitamin D3 oil solution obtained in the step 3 according to the volume ratio of 3:7, and shearing and homogenizing at a high speed of 10000rpm for 14min to obtain a vitamin D3-loaded nano calcium carbonate pickering emulsion;
5. detection of
Average particle size of the nano calcium carbonate pickering emulsion containing vitamin D3: the average particle size of the nano calcium carbonate Pickering emulsion detected by a static light scattering method is 71.3 mu m.
And (3) measuring the calcium content of the nano calcium carbonate pickering emulsion: the content of calcium in the nano calcium carbonate Pickering solution is measured by ion chromatography and is 2.4 mg/g.
And (3) measuring the vitamin D3 load capacity of the nano calcium carbonate pickering emulsion: the content of vitamin D3 in the nano calcium carbonate Pickering emulsion is measured by high performance liquid chromatography and is 23 IU/g.
Example 4
1. Ingredients
Preparing food-grade nano calcium carbonate powder into nano calcium carbonate suspension with the concentration of 100mg/m L by adding water for later use;
2. high hydrostatic dispersion
Placing the nano calcium carbonate suspension in the step 1 in a high static pressure device, and keeping the nano calcium carbonate suspension for 45min under the condition that the working pressure is 350 MPa;
3. vitamin D3 oil solution
Vitamin D3 oil solution is prepared by adding food grade vitamin D3 into fish oil, stirring at 500rpm under dark condition at room temperature for 0.5 hr to dissolve vitamin D3 completely to obtain 150IU/m L vitamin D3 oil solution;
4. pickering emulsion preparation
Mixing the nano calcium carbonate dispersion liquid obtained in the step 2 with a vitamin D3 oil solution according to a volume ratio of 2:8, and shearing and homogenizing at a high speed of 12000rpm for 5min to obtain a vitamin D3-loaded nano calcium carbonate pickering emulsion;
5. detection of
Average particle size of the nano calcium carbonate pickering emulsion containing vitamin D3: the average particle size of the nano calcium carbonate Pickering emulsion detected by a static light scattering method is 56.4 mu m.
And (3) measuring the calcium content of the nano calcium carbonate pickering emulsion: the content of calcium in the nano calcium carbonate Pickering solution is measured by ion chromatography and is 7.7 mg/g.
And (3) measuring the vitamin D3 load capacity of the nano calcium carbonate pickering emulsion: the content of vitamin D3 in the nano calcium carbonate Pickering emulsion is measured by high performance liquid chromatography and is 92 IU/g.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A preparation method of vitamin D3-loaded nano calcium carbonate pickering emulsion is characterized by comprising the following steps:
(1) suspension of nano calcium carbonate: mixing nano calcium carbonate powder with water to prepare nano calcium carbonate suspension;
(2) high static pressure treatment: carrying out high static pressure treatment on the nano calcium carbonate suspension liquid obtained in the step (1) to obtain uniformly dispersed nano calcium carbonate dispersion liquid;
(3) vitamin D3 oil solution: mixing vitamin D3 with edible oil, stirring in dark condition to completely dissolve vitamin D3 to obtain vitamin D3 oil solution;
(4) and (3) mixing the nano calcium carbonate dispersion liquid obtained in the step (2) with the vitamin D3 oil solution obtained in the step (3), and shearing and homogenizing to obtain the vitamin D3-loaded nano calcium carbonate pickering emulsion.
2. The preparation method according to claim 1, characterized in that the nano calcium carbonate powder in step (1) is food grade nano calcium carbonate powder; the content of the nano calcium carbonate in the food-grade nano calcium carbonate powder is not lower than 95 percent; the average particle size of the nano calcium carbonate is 30-250 nm.
3. The method of claim 1, wherein the vitamin D3 in step (3) is food grade vitamin D3; the food-grade vitamin D3 is solid powder obtained by sieving with a 100-mesh sieve, and the content of the solid powder is not less than 98%.
4. The method according to claim 1, wherein the edible oil in the step (3) is at least one of medium-chain fatty acid, fish oil, soybean oil, corn oil, peanut oil, rapeseed oil, sesame oil, sunflower seed oil, walnut oil, camellia oil, corn germ oil and olive oil.
5. The preparation method according to claim 1, wherein the concentration of the nano calcium carbonate suspension in the step (1) is 10-150 mg/m L;
the concentration of the vitamin D3 in the vitamin D3 oil solution in the step (3) is 5-1000 IU/m L.
6. The preparation method according to claim 5, wherein the nano calcium carbonate dispersion liquid and the vitamin D3 oil solution in the step (4) are mixed according to a volume ratio of 3: 7-2: 8.
7. The method according to claim 1, wherein the high static pressure treatment in step (2) is performed under 200 to 600MPa for 10 to 50 min; further keeping the pressure at 250-400 MPa for 20-45 min.
8. The method according to claim 1, wherein the shearing homogenization in the step (4) is carried out under a condition of shearing at 5000 to 20000rpm for 1 to 20 min; further comprises the following steps: shearing at 6000-15000 rpm for 3-15 min; further, the method comprises the following steps: shearing at 7000-12000 rpm for 5-15 min.
9. The vitamin D3-loaded nano calcium carbonate pickering emulsion is characterized by being prepared by the preparation method of any one of claims 1-8.
10. The vitamin D3-loaded nano calcium carbonate pickering emulsion of claim 9, which is used in food, cosmetics and medicine.
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