CN115337880A - Pumpkin seed oil microcapsule and preparation method and application thereof - Google Patents
Pumpkin seed oil microcapsule and preparation method and application thereof Download PDFInfo
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- CN115337880A CN115337880A CN202210830025.9A CN202210830025A CN115337880A CN 115337880 A CN115337880 A CN 115337880A CN 202210830025 A CN202210830025 A CN 202210830025A CN 115337880 A CN115337880 A CN 115337880A
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- seed oil
- pumpkin seed
- wall material
- microcapsule
- emulsion
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 81
- 239000011162 core material Substances 0.000 claims abstract description 38
- 238000002156 mixing Methods 0.000 claims abstract description 13
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- 239000005913 Maltodextrin Substances 0.000 claims description 25
- 229940035034 maltodextrin Drugs 0.000 claims description 25
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- 239000000230 xanthan gum Substances 0.000 claims description 23
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- RZRNAYUHWVFMIP-HXUWFJFHSA-N glycerol monolinoleate Natural products CCCCCCCCC=CCCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-HXUWFJFHSA-N 0.000 claims description 20
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- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
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- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
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- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- 229940087168 alpha tocopherol Drugs 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
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- 238000009472 formulation Methods 0.000 description 1
- 235000010382 gamma-tocopherol Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 239000010931 gold Substances 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
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- 238000005286 illumination Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
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- 239000011777 magnesium Substances 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 238000000611 regression analysis Methods 0.000 description 1
- 229940092258 rosemary extract Drugs 0.000 description 1
- 235000020748 rosemary extract Nutrition 0.000 description 1
- 239000001233 rosmarinus officinalis l. extract Substances 0.000 description 1
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- QUEDXNHFTDJVIY-DQCZWYHMSA-N γ-tocopherol Chemical compound OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1 QUEDXNHFTDJVIY-DQCZWYHMSA-N 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The invention provides a pumpkin seed oil microcapsule and a preparation method and application thereof. According to the invention, by screening the types and the compounding ratio of the wall materials, the synergistic effect of the components is fully exerted, the stability of the emulsion formed by mixing the wall materials and the core materials is improved, the embedding rate of the prepared microcapsule is improved, the peroxide value is reduced, and the quality guarantee period of the pumpkin seed oil is prolonged. The microencapsulated pumpkin seed oil has better water solubility, can effectively improve the bioavailability of the pumpkin seed oil, and can widen the application field of the pumpkin seed oil.
Description
Technical Field
The invention belongs to the field of food processing, and particularly relates to a pumpkin seed oil microcapsule as well as a preparation method and application thereof.
Background
The pumpkin seed oil not only contains rich unsaturated fatty acid such as linolenic acid, linoleic acid and the like, but also contains various bioactive substances such as phytosterol, amino acid, vitamin, mineral substances and the like, and particularly has extremely high contents of zinc, magnesium, calcium and phosphorus. The pumpkin seed oil also contains an active biological activator component called male hormone, can eliminate the initial swelling of the prostate, and has good treatment and prevention effects on urinary system and prostatic hyperplasia. In addition, the pumpkin seed oil is rich in phytosterol, tocopherol and vitamin A, wherein the alpha-tocopherol and the gamma-tocopherol are respectively 2 mg/kg-91 mg/kg and 41 mg/kg-620 mg/kg, so that the pumpkin seed oil has a good antioxidant effect.
However, because the pumpkin seed oil contains rich unsaturated fatty acid, the pumpkin seed oil is very easy to be influenced by external factors such as illumination, air, water and the like to generate oxidation reaction, so that the phenomenon of oxidative rancidity of the oil is generated, original nutrient substances and flavor substances in the oil are damaged, and the quality of the oil is seriously influenced. Through microencapsulation, the core material can be protected from the external environment, the volatility is reduced, the stability is improved, the original color, aroma, performance and physiological activity can be kept to the maximum extent, the damage and loss of nutrient substances are prevented, and the transportation and the storage are facilitated.
The research on the existing patents and literature about microencapsulation finds that the product after microencapsulation has the problems of poor stability, low embedding rate, multiple types of used wall material accessories and the like, and further queries on the patent about the microencapsulation of the pumpkin seed oil find that the research on improving the oxidation resistance of the pumpkin seed oil by microencapsulating the pumpkin seed oil is not available. The prior patent discloses an oxidation-resistant pumpkin seed oil microcapsule and a preparation method thereof, which mainly adds rosemary extract into a core material and pumpkin seed polypeptide into a wall material to improve the storage performance and the preservation capacity of the pumpkin seed oil, but does not screen, simplify and optimize the wall material. Therefore, the search for a wall material suitable for the pumpkin seed oil ensures the stability of the emulsion, improves the embedding rate and improves the oxidation resistance of the pumpkin seed oil microcapsule powder, has important research significance, and is beneficial to widening the application field of the pumpkin seed oil.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. To this end, the invention provides a pumpkin seed oil microcapsule in the first aspect, can improve the embedding rate, reduce the peroxide value and prolong the quality guarantee period of the pumpkin seed oil.
The second aspect of the invention provides a preparation method of pumpkin seed oil microcapsules.
The third aspect of the invention provides an application of the pumpkin seed oil microcapsule in preparing food, health care products or medicines.
According to the first aspect of the invention, the pumpkin seed oil microcapsule comprises a core material and a wall material, wherein the core material is pumpkin seed oil, and the wall material is prepared from maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum.
In some embodiments of the invention, the microcapsules are spherical or spheroidal with an average particle size of 50 μm to 65 μm.
In some embodiments of the present invention, the ratio of the wall material to the core material is (1-2): (1-2).
In some preferred embodiments of the present invention, the ratio of the wall material to the core material is (1-2): 1.
in some preferred embodiments of the present invention, the maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are used in the following ratio (3-7): (8-12): (0.1-0.3): (0.2-0.4).
In some more preferred embodiments of the present invention, the maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are used in the ratio of (3-5): (10-12): (0.15-0.2): (0.2-0.3).
In the invention, the types of the wall material preparation raw materials and the compounding ratio of the wall material preparation raw materials are screened, and the synergistic effect of all components in the wall material and the synergistic effect between the wall material and the pumpkin seed oil are fully exerted, so that the stability of an emulsion formed by mixing the wall material and the pumpkin seed oil is improved, the embedding rate of the prepared microcapsule is improved, the peroxide value is reduced, and the quality guarantee period of the pumpkin seed oil is further prolonged.
According to the second aspect of the invention, the preparation method of the pumpkin seed oil microcapsule comprises the following steps:
the materials are added according to the mixture ratio of the first aspect,
s1: mixing the maltodextrin, the sodium starch octenyl succinate, the glycerol monooleate and the xanthan gum in a solvent to form a wall material solution;
s2: and (3) mixing the wall material solution of S1 with the pumpkin seed oil, dispersing, homogenizing and drying to obtain the pumpkin seed oil microcapsule.
In the invention, wall materials formed by mixing maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are mixed with pumpkin seed oil, the obtained mixture is dispersed to obtain emulsion, and then the emulsion is homogenized and dried to obtain the pumpkin seed oil microcapsule.
In some embodiments of the present invention, the maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are used in the ratio of (3-7): (8-12): (0.1-0.3): (0.2-0.4).
In some preferred embodiments of the present invention, the maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are used in the ratio of (3-5): (10-12): (0.15-0.2): (0.2-0.3).
In some embodiments of the present invention, the wall material and the pumpkin seed oil are used in a ratio of (1-2): (1-2).
In some preferred embodiments of the present invention, the wall material and the pumpkin seed oil are used in a ratio of (1-2): 1.
in some embodiments of the present invention, the solvent in S1 is water, and the water includes at least one of distilled water and purified water.
In some preferred embodiments of the invention, the dispersion of S2 is a shear dispersion.
In some preferred embodiments of the invention, the rotation speed of the dispersion of S2 is 8000r/min to 12000r/min.
In some more preferred embodiments of the present invention, the rotation speed of the dispersion of S2 is 9000r/min to 11000r/min.
In some more preferred embodiments of the present invention, the time for the dispersion is 1min to 5min.
In some more preferred embodiments of the present invention, the homogenization pressure of S2 is 30MPa to 50MPa.
Further, the homogenizing pressure of S2 is 35 MPa-45 MPa.
In some more preferred embodiments of the present invention, the temperature of homogenization for S2 is 50 ℃ to 60 ℃.
In some more preferred embodiments of the present invention, the number of homogenizations is 1 to 3.
In the present invention, the premixing shear dispersion time of the emulsion is an important factor affecting the stability of the emulsion, and too short or too long shear time may cause the emulsion to be unstable. This is because the time is too short, the wall material absorbs water insufficiently, and the dispersion is not uniform; the time is too long, the demulsification phenomenon is increased due to the thermal motion of molecules, and the stability index of the emulsion is reduced.
In the invention, after the crude emulsion is homogenized under high pressure, the core material and the wall material are highly dispersed and fully mixed, so that the particle size of small particle aggregates and large particles in the crude emulsion is reduced, and the formation of uniform and stable emulsion is facilitated. However, if the homogenizing pressure is too large, the surface energy and the surface area of the liquid drop are also too large, and the emulsion breaking phenomenon is easy to occur, so that the stability of the emulsion is reduced, and the embedding effect of the product is influenced.
In some more preferred embodiments of the present invention, the drying of S2 is at least one of spray drying, fluidized drying, microwave drying, preferably spray drying.
In some more preferred embodiments of the present invention, the air inlet temperature of the spray drying is 140 ℃ to 200 ℃, and the air outlet temperature is 80 ℃ to 90 ℃.
According to a third aspect of the invention, the application of the pumpkin seed oil microcapsule in preparing food, health care products or medicines is provided.
In some preferred embodiments of the invention, the food product has at least one of the following functions: has effects of preventing and promoting health, resisting oxidation, and reducing blood lipid for male prostate diseases.
In some preferred embodiments of the present invention, the health product has at least one of the following functions: relieving early stage swelling of prostate, resisting oxidation, and reducing blood lipid.
In some preferred embodiments of the invention, the pharmaceutical product has at least one of the following functions: has effects of preventing and promoting health, resisting oxidation, and reducing blood lipid for male prostate diseases.
The invention has the beneficial effects that:
1. according to the invention, by screening the types and the compounding ratio of the raw materials for preparing the wall material, the synergistic effect of the components in the wall material and the synergistic effect between the wall material and the core material are fully exerted, the stability of the emulsion formed by mixing the wall material and the core material is improved, the embedding rate of the prepared microcapsule is improved to more than 99%, the peroxide value of the microcapsule is reduced, the quality guarantee period of the pumpkin seed oil is prolonged, and the shelf life of the pumpkin seed oil crude oil is about 5 times longer.
2. The pumpkin seed oil microcapsule provided by the invention has strong oxidation resistance, so that the oxidation resistance of the embedded pumpkin seed oil is obviously improved compared with that of crude oil.
3. The preparation method of the pumpkin seed oil microcapsule is simple and feasible, has low cost and can be used for large-scale production.
4. The microencapsulated pumpkin seed oil has better water solubility, can effectively improve the bioavailability of the pumpkin seed oil, and broadens the application field of the pumpkin seed oil.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a graph comparing the DPPH radical scavenging ability of the pumpkin seed oil (crude oil) and the pumpkin seed oil microcapsules of example 1;
FIG. 2 is a graph showing the comparison of the ability of removing hydroxyl radicals of the pumpkin seed oil (crude oil) and the pumpkin seed oil microcapsules of example 1;
FIG. 3 is a graph comparing the ABTS free radical scavenging ability of the pumpkin seed oil (crude oil) and the pumpkin seed oil microcapsules of example 1;
FIG. 4 is a graph showing the comparison of the peroxide change of the pumpkin seed oil (crude oil) and the pumpkin seed oil microcapsule of example 1 stored at 60 ℃ for 18 days.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention.
Example 1
The embodiment prepares the pumpkin seed oil microcapsule, and the specific process is as follows:
(1) Respectively adding 5 parts of maltodextrin, 10 parts of sodium starch octenylsuccinate, 0.15 part of glycerol monooleate and 0.2 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the materials are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Example 2
The embodiment prepares the pumpkin seed oil microcapsule, and the specific process is as follows:
(1) Respectively adding 3 parts of maltodextrin, 12 parts of sodium starch octenyl succinate, 0.15 part of glycerol monooleate and 0.2 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the materials are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Example 3
The embodiment prepares the pumpkin seed oil microcapsule, and the specific process is as follows:
(1) Respectively adding 5 parts of maltodextrin, 10 parts of sodium starch octenyl succinate, 0.2 part of glycerol monooleate and 0.3 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the materials are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Comparative example 1
The pumpkin seed oil microcapsule prepared by the comparative example is different from the pumpkin seed oil microcapsule prepared by the example 1 in that the compounding ratio of maltodextrin to starch sodium octenyl succinate is 2:1, and the specific process is as follows:
(1) Respectively adding 10 parts of maltodextrin, 5 parts of sodium starch octenyl succinate, 0.15 part of glycerol monooleate and 0.2 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the materials are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1 in parts by weight;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (5) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Comparative example 2
The comparison example prepares a pumpkin seed oil microcapsule, and the difference from the example 1 is that maltodextrin is not added, and the specific process is as follows:
(1) Respectively adding 10 parts by weight of sodium starch octenyl succinate, 0.15 part by weight of glycerol monooleate and 0.2 part by weight of xanthan gum into distilled water, stirring for 2-3 hours until the starch octenyl succinate is completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Comparative example 3
The pumpkin seed oil microcapsule prepared by the comparative example is different from the pumpkin seed oil microcapsule prepared by the example 1 in that no starch sodium octenyl succinate is added, and the specific process is as follows:
(1) Respectively adding 5 parts of maltodextrin, 0.15 part of glycerol monooleate and 0.2 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the maltodextrin, the glycerol monooleate and the xanthan gum are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1 in parts by weight;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (5) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Comparative example 4
The pumpkin seed oil microcapsule is prepared according to the comparative example, and is different from the pumpkin seed oil microcapsule in example 1 in that glycerol monooleate is not added, and the specific process is as follows:
(1) Respectively adding 5 parts of maltodextrin, 10 parts of sodium starch octenyl succinate and 0.2 part of xanthan gum into distilled water according to parts by weight, stirring for 2-3 hours until the maltodextrin, the starch octenyl succinate and the xanthan gum are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1 in parts by weight;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Comparative example 5
The pumpkin seed oil microcapsule prepared by the comparative example is different from the pumpkin seed oil microcapsule prepared by the example 1 in that xanthan gum is not added, and the specific process is as follows:
(1) Respectively adding 5 parts of maltodextrin, 10 parts of sodium starch octenyl succinate and 0.15 part of glycerol monooleate into distilled water according to the parts by weight, stirring for 2-3 hours until the materials are completely dissolved, and standing at room temperature for full hydration to prepare a wall material solution;
(2) Heating the wall material solution to 60-70 ℃, adding the pumpkin seed oil core material preheated to 60 ℃, and fully and uniformly stirring, wherein the dosage ratio of the pumpkin seed oil core material to the wall material is 1:1;
(3) Dispersing the mixture of the core material and wall material solution obtained in the step (2) at a high speed for 3min under the condition of a rotating speed of 10000r/min to obtain an emulsion;
(4) Homogenizing the emulsion obtained in the step (3) for 2 times by a high-pressure homogenizer at the temperature of 50-60 ℃ and under the pressure of 40 MPa;
(5) And (4) carrying out spray drying on the emulsion obtained in the step (4), wherein the air inlet temperature is 160 ℃, the air outlet temperature is 85 ℃, and finally obtaining the powdery pumpkin seed oil microcapsule.
Test example 1
The test methods involved in this test example were:
(1) Stability testing of the emulsions: the stability of the emulsion is characterized by The Stability Index (TSI) of the emulsion system, and the dynamic changes of the emulsion system are monitored by the intensity of the backscattered light and the transmitted light by using a stability analyzer to vertically scan the emulsion sample before spray drying in a top-down manner. 20mL of the emulsion sample was added to a glass bottle dedicated to a Turbiscan Lab Expert multiple light scattering instrument, the temperature was set at 30 ℃ and the scan was performed 1 time every 2min for 2h, and the sample scan was recorded and the measurement was repeated 3 times. The data was analyzed using Turbi Soft based on the change in sample transmitted light and back scattered intensity to give the TSI of the emulsion.
(2) And (3) testing the embedding rate: the quality of the microcapsule surface oil was measured by the method specified in QBT 4791-2015. The total oil quality of the microcapsules was determined according to the method specified in GB 5009.6-2016. The embedding rate of the microcapsules is calculated by the following formula:
(3) Determination of peroxide number: the samples were stored in an oven at 60 ℃ for 18 days and then assayed according to the method specified in GB 5009.227-2016.
TABLE 1 results of emulsion stability (TSI), encapsulation efficiency, and microcapsule peroxide value test prepared in examples 1 to 3 and comparative examples 1 to 5
| Item | TSI | Embedding Rate (%) | Peroxide number (meq/kg) |
| Example 1 | 2.8 | 99.08 | 2.17 |
| Example 2 | 3.0 | 98.94 | 2.40 |
| Example 3 | 3.0 | 98.98 | 2.32 |
| Comparative example 1 | 5.9 | 94.09 | 5.87 |
| Comparative example 2 | 9.0 | 80.11 | 8.91 |
| Comparative example 3 | 16.5 | 63.74 | 16.86 |
| Comparative example 4 | 7.3 | 89.65 | 8.20 |
| Comparative example 5 | 6.8 | 90.06 | 7.01 |
And (4) analyzing results:
as can be seen from Table 1, the emulsions prepared by using the examples of the present invention have smaller TSI values, none of the TSI values exceeds 3, and the smaller the TSI value is, the higher the stability of the emulsion is, that is, the emulsion composed of the wall material and the core material in the examples of the present invention has good stability. It can be seen from comparison of examples 1 to 3 that, by adjusting the use ratio of the wall material in the wall material mass parts specified in the present invention, although there is a certain fluctuation in the emulsion stability, embedding rate and peroxide value of the microcapsule, there is no obvious difference change, which indicates that the wall material type and wall material formulation ratio selected in the examples of the present invention can be well fused with pumpkin seed oil to improve the stability, embedding rate and embedding effect of the microcapsule emulsion.
It can also be seen from table 1 that, compared with example 1, the microcapsule emulsion in comparative example 1 has poor stability, reduced embedding rate and improved peroxide value, which indicates that the compounding of maltodextrin and sodium starch octenyl succinate in a proper proportion can improve the emulsion stability, and further improve the embedding rate of the prepared microcapsule and reduce the peroxide value of the microcapsule; compared with example 1, in comparative examples 2 to 5, it is shown that maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum are not added, and as a result, the emulsion stability of the microcapsule is greatly reduced, the embedding rate is reduced, and the peroxide value is greatly improved, which indicates that a strong synergistic effect exists among maltodextrin, sodium starch octenyl succinate, glycerol monooleate and xanthan gum, and the lack of one of the synergistic effects causes the emulsification structure to be obviously changed, so that the embedding rate is reduced, and the embedding effect is poor. Meanwhile, the types of the wall materials are gold combinations, and the wall materials have good synergistic effect.
Test example 2
Preparing a sample solution: different amounts of the pumpkin seed oil microcapsules prepared in example 1 and the amount of the corresponding embedded pumpkin seed oil crude oil are respectively weighed, and distilled water is added to the weighed amount to obtain the required volume of the sample solution.
(1) Ability to scavenge DPPH free radicals
Determination of DPPH radical scavenging capacity: accurately weighing 0.3mL of distilled water and 0.3mL of sample solution, respectively placing in 10mL test tubes with plugs, respectively adding 2.7mL of working solution of LDPPH, mixing, dark reacting for 30min, and reacting with anhydrousMethanol as control, and the absorbance at 518nm, respectively, is recorded as A 0 、A s (ii) a Accurately weighing 0.3mL sample solution and 2.7mL anhydrous methanol in 10mL test tube with plug, mixing, dark reacting for 30min, using anhydrous methanol as control, measuring absorbance at 518nm, and recording as A r The radical clearance (Y) was calculated according to the formula, and the results are shown in FIG. 1.
(2) Ability to scavenge hydroxyl radicals
Determination of the hydroxyl radical scavenging capacity: taking 3 10mL test tubes with plugs and marking as 1, 2 and 3 respectively, adding 1mL phenanthroline, 0.5mL ferrous sulfate and 1mL PBS buffer solution into each test tube in turn, adding 7.5mL distilled water into the test tube No. 1, adding 7mL distilled water into the test tube No. 2, and adding 0.5mLH 2 O 2 Solution, 1mL of sample solution, 6mL of distilled water and 0.5mLH were added to test tube No. 3 2 O 2 Mixing the solutions, maintaining the temperature in 37 deg.C water bath for 1h, measuring absorbance at 536nm with distilled water as reference, and recording as A 0 Ar and As, the radical clearance (Y) is calculated according to the formula, and the result is shown in figure 2.
(3) Ability to scavenge ABTS free radicals
Determination of ABTS free radical scavenging ability: accurately measuring 1mL of deionized water and 1mL of sample solution, respectively placing in 10mL test tubes with plugs, respectively adding 3mL of LaBTS working solution into the test tubes, mixing, dark reacting for 6min, measuring absorbance at 734nm with 70% ethanol as reference, respectively recording as A 0 As; accurately measuring 1mL of sample solution and 3mL of 70% ethanol in a 10mL test tube with a plug, uniformly mixing, carrying out dark reaction for 6min, taking 70% ethanol as reference, and measuring the absorbance at 734nm and recording as Ar. The radical clearance (Y) was calculated according to the formula, and the results are shown in FIG. 3.
From fig. 1 to fig. 3, it can be seen that compared with pumpkin seed crude oil, the pumpkin seed oil microcapsule prepared by selecting maltodextrin, sodium starch octenyl succinate, glyceryl monooleate and xanthan gum as the wall material of the pumpkin seed oil microcapsule and appropriate microencapsulation process parameters has obviously improved capability of removing DPPH free radical, hydroxyl free radical and ABTS free radical, which indicates that the antioxidant capability of the pumpkin seed oil microcapsule can be improved by the screened wall material type and wall material compounding ratio.
Test example 3
Determination of peroxide value of microcapsules during storage
The pumpkin seed oil (crude oil) and the pumpkin seed oil microcapsule sample prepared in example 1 were stored in an oven at 60 ℃ for 18 days, and the peroxide value was measured every three days to examine the change of the peroxide value of the microcapsule sample under the accelerated oxidation condition. The peroxide number was determined according to the method specified in GB5009.227-2016, and the results are shown in FIG. 4.
As can be seen from fig. 4, the peroxide value of the pumpkin seed oil is increased continuously in the acceleration test process, wherein the value is increased slowly in 0 d-6 d, and is increased rapidly in 6 d-18 d, and is increased exponentially, while the peroxide value of the pumpkin seed oil microcapsule prepared in example 1 is also increased, but the increase amplitude is gentle, and the increase speed is gradually slow. Comparing the peroxide value of the pumpkin seed oil microcapsule after the accelerated experiment with the crude oil, the peroxide value of the microcapsule is found to be obviously lower than that of the crude oil, which shows that the microcapsule wall material has a good protection effect on the pumpkin seed oil.
Using the zero order reaction equation C = C, respectively 0 -kt and first order reaction equation lnC = ln (C) 0 -kt) performing regression analysis on peroxide value changes of the pumpkin seed oil crude oil and the pumpkin seed oil microcapsules, and obtaining that the oxidation reaction of the pumpkin seed oil crude oil belongs to a first-order oxidation kinetic reaction (ln (C) 1 )＝-0.3973+0.2431t 1 ) The oxidation reaction of the pumpkin seed oil microcapsule belongs to zero-order oxidation reactionMechanics (C) 2 ＝0.2440t 2 +3.0561). According to the limit regulation (peroxide value is less than or equal to 19.7 meq/kg) of the edible oil, the 19.7meq/kg is substituted into the corresponding kinetic equation, and the storage time of the sample can be obtained. The results obtained were as follows: the storage time of the pumpkin seed oil crude oil and the pumpkin seed oil microcapsule is 14d and 68d respectively at the temperature of 60 ℃. According to the Vant' Hoff empirical formula, the storage time of the product is shortened by 1/2 for every 10 ℃ rise of the reaction temperature, namely, the storage time of the sample at 60 ℃ for 1d is equivalent to the storage time of the sample at 20 ℃ for 16d. Therefore, the storage time of the pumpkin seed oil crude oil and the pumpkin seed oil microcapsule under the same condition of 20 ℃ is 224d and 1088d respectively. In conclusion, at normal temperature, the shelf life of the pumpkin seed oil crude oil without being embedded by the wall material system is 224 days, while the shelf life of the pumpkin seed oil microcapsule is 1088 days, and the prolonged shelf life is nearly 5 times, which shows that the oxidation stability of the pumpkin seed oil after being embedded is improved, and the shelf life of the sample is prolonged.
While the embodiments of the present invention have been described in detail, the present invention is not limited to the embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art. Furthermore, the embodiments of the present invention and the features of the embodiments may be combined with each other without conflict.
Claims (10)
1. The pumpkin seed oil microcapsule comprises a core material and a wall material, and is characterized in that the core material is pumpkin seed oil, and the wall material is prepared from maltodextrin, sodium starch octenyl succinate, glyceryl monooleate and xanthan gum.
2. The microcapsule according to claim 1, wherein the wall material and the core material are used in a ratio of (1 to 2): (1-2).
3. The microcapsule according to claim 2, wherein the maltodextrin, sodium starch octenylsuccinate, glycerol monooleate and xanthan gum are used in the ratio of (3-7): (8-12): (0.1-0.3): (0.2-0.4).
4. A preparation method of pumpkin seed oil microcapsules is characterized by comprising the following steps:
the proportioning addition according to claims 2 and 3,
s1: mixing the maltodextrin, the sodium starch octenyl succinate, the glycerol monooleate and the xanthan gum in a solvent to form a wall material solution;
s2: and (3) mixing the wall material solution of S1 with the pumpkin seed oil, dispersing, homogenizing and drying to obtain the pumpkin seed oil microcapsule powder.
5. The method according to claim 4, wherein the rotation speed of the dispersion of S2 is 8000 to 12000r/min.
6. The method according to claim 4, wherein the homogenization pressure of S2 is 30MPa to 50MPa.
7. The method of claim 6, wherein the temperature of homogenizing is 50 ℃ to 60 ℃.
8. The method according to claim 4, wherein the drying step S2 is at least one of spray drying, fluidized drying and microwave drying.
9. The preparation method of claim 8, wherein the inlet air temperature of the spray drying is 140-200 ℃, and the outlet air temperature is 80-90 ℃.
10. Use of a pumpkin seed oil microcapsule for the preparation of a food product, a nutraceutical product or a pharmaceutical product, wherein the pumpkin seed oil microcapsule is according to any one of claims 1 to 3 or according to any one of claims 4 to 9.
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