CN113826906A - Dihydroquercetin nanoemulsion and preparation method and application thereof - Google Patents

Dihydroquercetin nanoemulsion and preparation method and application thereof Download PDF

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Publication number
CN113826906A
CN113826906A CN202111357973.7A CN202111357973A CN113826906A CN 113826906 A CN113826906 A CN 113826906A CN 202111357973 A CN202111357973 A CN 202111357973A CN 113826906 A CN113826906 A CN 113826906A
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dihydroquercetin
water
nanoemulsion
oil
emulsifier
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郑旭
于婷
穆春旭
张树刚
关莹
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Yuneng Dalian Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/15Vitamins
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/03Organic compounds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L29/00Foods or foodstuffs containing additives; Preparation or treatment thereof
    • A23L29/10Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
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Abstract

The invention discloses a dihydroquercetin nanoemulsion and a preparation method and application thereof. The dihydroquercetin nanoemulsion comprises the following raw materials in parts by weight: 1-20 parts of oil, 1-5 parts of emulsifier, 0.01-0.05 part of dihydroquercetin and 80-99 parts of water. The preparation method of the dihydroquercetin nanoemulsion comprises the following steps: s1: dividing water into two parts, mixing the first part of water and an emulsifier, and stirring; heating the second water cut to 100 ℃ to obtain boiling water; s2: preparing a primary coarse emulsion; s3: and (4) carrying out homogeneous reaction on the primary crude emulsion obtained in the step S2. Application of dihydroquercetin nanoemulsion in food structure modification base materials. The invention realizes the production of an antioxidant nano-emulsion to overcome the defects of poor water solubility and low bioavailability of the prior dihydroquercetin.

Description

Dihydroquercetin nanoemulsion and preparation method and application thereof
Technical Field
The invention relates to the field of emulsions, in particular to a dihydroquercetin nanoemulsion and a preparation method and application thereof.
Background
Dihydroquercetin is a flavanonol compound, belongs to vitamin P group, is a bioactive agent with wide application, and has various biological activities in human body like other flavonoid compounds, including antioxidation, free radical scavenging, antivirus, anti-inflammation, vasodilatation, antibacterial and other effects. At present, a great amount of dietary supplements using dihydroquercetin exist, but the solubility of dihydroquercetin in a water phase is not high, the exertion of the biological activity is limited, the bioavailability is reduced, and related emulsion products are not found at present.
In recent years, food-grade nano emulsion as a simple and effective embedding and transporting system is widely applied to embedding and transferring functional grease and various oil-soluble nutrients, can prevent functional nutrient components from being oxidized, and improves the water solubility and bioavailability of the functional nutrient components. The nano emulsion is also different from the common emulsion in that the nano emulsion can resist flocculation, coalescence and gravity separation in the storage process and is a near-thermodynamic stable system. The preparation method of the nano emulsion comprises a high-energy method and a low-energy method, and the high-pressure homogeneous emulsification technology is used as a commonly used high-energy method for preparing the nano emulsion and has the advantages of small emulsion particle size, uniform distribution, stable emulsion system, small demand of a surfactant and the like. At present, the research on preparing the nano emulsion by using a high-pressure homogeneous emulsification technology exists, but the research on the dihydroquercetin nano emulsion is not available.
Disclosure of Invention
The invention discloses a dihydroquercetin nanoemulsion and a preparation method and application thereof, aiming at producing an antioxidant nanoemulsion and solving the defects of poor water solubility and low bioavailability of the dihydroquercetin at present.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a dihydroquercetin nanoemulsion comprises the following raw materials in parts by weight: 1-20 parts of oil, 1-5 parts of emulsifier, 0.01-0.05 part of dihydroquercetin and 80-99 parts of water.
Further, the oil is at least one of olive oil, DHA algae oil, linseed oil, and krill oil.
Further, the particle size of the dihydroquercetin is 113.3-171.8 nm.
Further, the emulsifier is at least one of soybean phospholipid, octenyl succinic acid starch ester, polyoxyethylene sorbitan monooleate and sodium caseinate.
The dihydroquercetin nanoemulsion has the beneficial effects that:
1. by mixing oil, an emulsifier, dihydroquercetin and water and controlling the content of each component, the concentration of the emulsifier solution can be kept in a proper range, so that oil drops are not easy to fuse, and the diameter of the oil drops is kept in a proper range.
2. The emulsifier is controlled to be 1-5 parts by weight, so that the emulsifier can completely wrap oil drops, and the volume ratio of oil phases in the emulsion is improved.
In order to achieve the above object, the technical solution of the present invention further includes:
a preparation method of dihydroquercetin nanoemulsion comprises the following steps:
s1: dividing the water into two parts, wherein the weight ratio of the first part of water to the second part of water is (7-8.9): 1; mixing and stirring the first part of water and an emulsifier to obtain a hydrated emulsifier;
heating the second portion of water to 100 ℃ to obtain boiling water;
s2: adding dihydroquercetin into the boiling water obtained in the step S1, and uniformly mixing to obtain a dihydroquercetin solution;
s3: uniformly mixing the oil, the hydrated emulsifier obtained in the step S1 and the dihydroquercetin solution obtained in the step S2 to obtain a primary coarse emulsion;
s4: and (3) homogenizing the primary coarse emulsion obtained in the step S3 for 1-5min at the pressure of 100-150 MPa.
Further, in step S1, the first part of water and the emulsifier are mixed and stirred by magnetic stirring.
Further, the rotation speed of the magnetic stirring is 800-.
Further, in step S3, the oil, the post-hydration emulsifier obtained in step S1, and the dihydroquercetin solution obtained in step S2 are added to a high-speed disperser and sheared together.
Further, the rotating speed of the high-speed disperser is 5000-.
The preparation method of the dihydroquercetin nanoemulsion has the beneficial effects that:
1. by adopting the preparation method, the problem that dihydroquercetin is difficult to dissolve in water is solved, and the oxidation resistance of dihydroquercetin is effectively improved;
2. the oil-in-water emulsion prepared by the preparation method has small particle size, good viscoelasticity and high storage stability;
3. the preparation method has low requirement on equipment, is simple and easy to operate, and is suitable for large-scale industrial production and processing.
In order to achieve the purpose, the technical scheme of the invention is as follows:
an application of dihydroquercetin nanoemulsion, in particular to an application of dihydroquercetin nanoemulsion in a food structure modification base material.
The application of the dihydroquercetin nanoemulsion has the beneficial effects that:
1. the application of the dihydroquercetin nanoemulsion in the field of food is expanded.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The starting materials used in the present application are all commercially available.
Examples
The following examples and comparative examples a method for preparing dihydroquercetin nanoemulsion, comprising the steps of:
s1: dividing water into two parts, adding the first part of water and the emulsion into a beaker, mixing and stirring in a magnetic stirring mode at the rotating speed of 1000r/min for 2 hours to ensure that the emulsifier is fully hydrated in the first part of water to obtain a hydrated emulsifier;
heating the second part of water to 100 ℃ to obtain boiling water;
s2: adding dihydroquercetin into the boiling water obtained in step S1, and mixing to obtain dihydroquercetin solution with particle diameter of 113.3 nm;
s3: adding the oil, the hydrated emulsifier obtained in the step S1 and the dihydroquercetin solution obtained in the step S2 into a high-speed disperser for shearing, wherein the rotating speed of the high-speed disperser is 8000r/min, the reaction time is 3h, and the treatment interval is 5S, so as to prepare a primary coarse emulsion;
s4: and (4) adding the primary coarse emulsion obtained in the step (S3) into a homogenizer, wherein the homogenizing pressure is 150MPa, and the reaction time is 3 min.
Table 1: examples 1-5 raw Material composition of Dihydroquercetin nanoemulsion
Figure BDA0003358022930000041
Table 2: example 6-10 raw Material composition of Dihydroquercetin nanoemulsion
Figure BDA0003358022930000051
Comparative example
Comparative example 1: the difference from example 3 is that no dihydroquercetin was added.
Comparative example 2: a method for preparing dihydroquercetin nanoemulsion comprises heating 10ml of water to 100 deg.C to obtain boiling water; adding 0.05g dihydroquercetin into boiling water, and mixing to obtain dihydroquercetin solution.
Performance test
The following performance tests were performed on the dihydroquercetin nanoemulsion prepared in examples 1 to 10 and comparative examples 1 to 2, respectively.
Testing the particle size of the dihydroquercetin nanoemulsion: dihydroquercetin nanoemulsion prepared by the method
Diluting with ionized water by 20 times, measuring the average particle diameter of the emulsion sample by a nanometer particle size-Zeta potentiometer, and keeping the temperature of the measuring environment at 25 ℃. The results are shown in Table 3.
And (3) testing the cell antioxidant activity of the dihydroquercetin nanoemulsion:
s1: before measurement, liver cancer cells HepG-2 are subcultured, 5% fetal bovine serum, 10mmonl/L hydroxyethyl piperazine ethosulfate, 2mmo 1/LL-glutamine, 5 mu g/mL insulin, 0.05 mu g/mL cortisol, 50 mu g/mL penicillin, 50 mu g/mL streptomycin and 100 mu g/mL gentamicin are added into a VE culture medium, and the culture is carried out at 37 ℃ and under the condition of higher humidity.
S2: on a 96-well plate at 6X 104And (4) inoculating the cultured liver cancer cell HepG-2 obtained in the step S1 and the cell of the dihydroquercetin nanoemulsion prepared by the application to the density of each hole, and testing the cell antioxidant activity of the dihydroquercetin nanoemulsion prepared by the application by using a CAA method.
S3: after 24h of inoculation, the medium was removed and washed once with 100. mu.L of phosphate buffer. The mixture was treated with 100uL of different concentrations of antioxidant compound and 25. mu. mol/L of 2', 7' -dichlorofluorescein diacetate at 37 ℃ for 1 h. Then treated with 100uL of 600. mu. mol/L of 2, 2' -azobisisobutylamidine dihydrochloride, and finally fluorescence was measured every 5min at 538nm for 1h using a fluorescent microplate reader.
S4: blanks were set up and the control on each plate was treated with 2', 7' -dichlorofluorescent diacetate and 2, 2' -azobisisobutylamidine dihydrochloride, and the blank was treated with 2', 7' -dichlorofluorescent diacetate only. After blank zero adjustment and initial fluorescence value zero adjustment, a curve of the change of the fluorescence value along with time can be obtained by spectrum, and the CAA value of the antioxidant substance can be calculated according to the area under the curve.
The CAA value is calculated by the formula:
CAAunit=100-(∫SA/∫CA)×100
in the formula: SA is the integral area under the time-fluorescence value curve of the sample group;
and CA is the integral area under the time-fluorescence value curve of the control group. The results are shown in Table 3.
And (3) testing the stability of the dihydroquercetin nanoemulsion: sterilizing the dihydroquercetin nanoemulsion prepared by the method at 115 ℃ for 15min, keeping the temperature of a test environment at 37 ℃ and the relative humidity at 70%, standing for 30 days, and observing the layering condition of the dihydroquercetin nanoemulsion. The results are shown in Table 3.
Table 3: test results of examples 1 to 10 and comparative examples 1 to 2
Test items Average particle diameter (nm) CAA value (μmolQE/g) Whether or not to stratify
Example 1 156.3 331.71 Whether or not
Example 2 164.7 386.23 Whether or not
Example 3 162.1 404.19 Whether or not
Example 4 166.5 365.89 Whether or not
Example 5 171.8 401.12 Whether or not
Example 6 169.4 399.89 Whether or not
Example 7 232.5 397.28 Is that
Example 8 113.3 60.34 Whether or not
Example 9 161.8 204.75 Whether or not
Example 10 307.4 517.3 Is that
Comparative example 1 160.6 153.47 Whether or not
Comparative example 2 - 225.24 Is that
The analysis data shows that:
as can be seen from table 2, in examples 1 to 4, the emulsifier was soybean lecithin, the amount of dihydroquercetin added was 0.05g, and the amount of oil added was 10mL, comparing the cell antioxidant activity of dihydroquercetin nanoemulsion prepared from olive oil, linseed oil, DHA algal oil, and krill oil. Wherein the antioxidant activity of linseed oil is higher than that of olive oil, DHA algal oil and krill oil.
As is clear from Table 2, in examples 3 and 5-7, the amount of dihydroquercetin added was 0.05g, the amount of oil added was 10mL, and the linseed oil was selected as the oil, and the average particle size of dihydroquercetin nanoemulsion prepared by comparing soybean lecithin, starch octenylsuccinate, polyoxyethylene sorbitan monooleate, and sodium caseinate was determined. The average particle size of the nano emulsion is 50-200 nm. Soybean lecithin as emulsifier is smaller than other 3 kinds of emulsifiers, wherein the soybean lecithin is sterilized at 115 deg.C for 15min, and dihydroquercetin nanoemulsion prepared from sodium caseinate is layered.
As is clear from table 2, in example 3, the amount of the added oil was 10mL, the linseed oil was selected as the oil, the soybean lecithin was selected as the emulsifier, and the amount of the added dihydroquercetin was different from that of example 9. With the increase of the dihydroquercetin, the cell antioxidant activity of the dihydroquercetin nanoemulsion is increased.
As is clear from table 2, in example 8, the amount of dihydroquercetin added was 0.01g, linseed oil was used as the oil, soybean phospholipid was used as the emulsifier, and the amount of oil added was different from that of example 9. Example 3 compared with 10, the amount of dihydroquercetin added was 0.05g, linseed oil was selected as the oil, soybean phospholipid was selected as the emulsifier, and the amount of oil added was different. The antioxidant activity is increased with the increase of the oil amount, but the particle size is also increased. Both were sterilized at 115 ℃ for 15min, and then delamination was evident in example 10 during the standing.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.

Claims (10)

1. The dihydroquercetin nanoemulsion is characterized by comprising the following raw materials in parts by weight: 1-20 parts of oil, 1-5 parts of emulsifier, 0.01-0.05 part of dihydroquercetin and 80-99 parts of water.
2. The dihydroquercetin nanoemulsion according to claim 1, wherein the oil is at least one of olive oil, DHA algae oil, linseed oil, krill oil.
3. The dihydroquercetin nanoemulsion according to claim 1, wherein the particle size of the dihydroquercetin is 113.3-171.8 nm.
4. The dihydroquercetin nanoemulsion according to claim 1, wherein the emulsifier is at least one of soybean lecithin, starch octenyl succinate, polyoxyethylene sorbitan monooleate, and sodium caseinate.
5. A method of preparing a dihydroquercetin nanoemulsion according to any one of claims 1-4, characterized by comprising the following steps:
s1: dividing the water into two parts, wherein the weight ratio of the first part of water to the second part of water is (7-8.9): 1; mixing and stirring the first part of water and an emulsifier to obtain a hydrated emulsifier;
heating the second portion of water to 100 ℃ to obtain boiling water;
s2: adding dihydroquercetin into the boiling water obtained in the step S1, and uniformly mixing to obtain a dihydroquercetin solution;
s3: uniformly mixing the oil, the hydrated emulsifier obtained in the step S1 and the dihydroquercetin solution obtained in the step S2 to obtain a primary coarse emulsion;
s4: and (3) homogenizing the primary coarse emulsion obtained in the step S3 for 1-5min at the pressure of 100-150 MPa.
6. The method of claim 5, wherein the first portion of water and the emulsifier are mixed and stirred in step S1 by magnetic stirring.
7. The method for preparing dihydroquercetin nanoemulsion as claimed in claim 6, wherein the rotation speed of magnetic stirring is 800-1000r/min, and the stirring time is 60-120 min.
8. The method of claim 5, wherein in step S3, the oil, the post-hydration emulsifier obtained in step S1, and the dihydroquercetin solution obtained in step S2 are added together in a high-speed disperser and sheared.
9. The method of claim 8, wherein the rotating speed of the high speed disperser is 5000-8000r/min, the reaction time is 2-4min, and the treatment interval is 5 s.
10. Use of a dihydroquercetin nanoemulsion according to any one of claims 1-4, characterized in that the use of the dihydroquercetin nanoemulsion is in a food structure modification base.
CN202111357973.7A 2021-11-16 2021-11-16 Dihydroquercetin nanoemulsion and preparation method and application thereof Pending CN113826906A (en)

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CN115462529A (en) * 2022-09-16 2022-12-13 华中农业大学 Quercetin emulsion and preparation method and application thereof

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CN115462529A (en) * 2022-09-16 2022-12-13 华中农业大学 Quercetin emulsion and preparation method and application thereof

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