Perilla oil-containing haematococcus pluvialis composition with antioxidant function and preparation method of perilla oil-containing haematococcus pluvialis composition
By combining ingredients such as Haematococcus pluvialis powder and perilla oil and performing specific process treatment, a composition with high-efficiency antioxidant activity and stability is prepared, which solves the problem of insufficient stability of antioxidant compositions in the prior art during storage.
Patent Information
- Application Number
- CN202511047133.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-29
- Publication Date
- 2025-09-26
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of preparation of Haematococcus pluvialis compositions, in particular to a Haematococcus pluvialis composition containing perilla oil and having antioxidant function and a preparation method thereof. Background Art
[0002] The human body continuously generates free radicals due to constant contact with the outside world, including through breathing, pollution, and radiation exposure. While this unavoidable free radical production occurs, the body naturally produces antioxidants to counteract the oxidative attack of free radicals on human cells. However, with aging, enzyme activity in the body decreases, and eventually, antioxidants are no longer able to eliminate the accumulated free radicals. Therefore, a combination of antioxidants is needed to effectively scavenge free radicals.
[0003] While existing research has explored the combination of multiple natural antioxidant ingredients, there are still deficiencies in improving the stability of these compositions. Some compounded products are prone to oxidation, deterioration, stratification, and precipitation during storage due to interactions between ingredients or environmental influences, leading to a decrease in antioxidant activity. Summary of the Invention
[0004] The present invention aims to provide a Haematococcus pluvialis composition containing perilla oil with antioxidant function and a preparation method thereof, wherein the stability of the Haematococcus pluvialis composition containing perilla oil is significantly improved by adding a stabilizer while ensuring high antioxidant performance.
[0005] To achieve the above object, the technical solution adopted by the present invention is: providing a Haematococcus pluvialis composition containing perilla oil with antioxidant function, which is composed of the following components by weight: 15-25 parts of Haematococcus pluvialis powder, 8-18 parts of perilla oil, 1-3 parts of coenzyme Q10, 2-5 parts of black wolfberry extract, 1-4 parts of vitamin E, 3-8 parts of a composite emulsifier, 5-10 parts of cyclodextrin and 1-5 parts of a stabilizer.
[0006] Optionally, the astaxanthin content in the Haematococcus pluvialis powder is not less than 2%, and the α-linolenic acid content in the perilla oil is not less than 55%.
[0007] Optionally, the composite emulsifier consists of monoglyceride, sucrose ester and soybean lecithin in a mass ratio of 2:1:1.
[0008] Optionally, the stabilizer is one or more combinations of sodium alginate, xanthan gum, and sodium carboxymethyl cellulose.
[0009] A method for preparing a Haematococcus pluvialis composition containing perilla oil and having antioxidant function, comprising the following steps: Pretreatment: Haematococcus pluvialis powder and cyclodextrin were mixed in a mass ratio of 1:1.2, and deionized water (8 times the total mass of the two) was added. The mixture was stirred at 50°C and 400 rpm for 30 minutes. At the same time, perilla oil was heated to 60°C under nitrogen and maintained for 15 minutes to remove trace oxygen. Emulsification stage: The composite emulsifier and vitamin E are mixed, and the treated perilla oil is added, and the mixture is stirred at 8000 rpm in a high-speed shearing machine for 10 minutes to form a stable oil phase; the inclusion Haematococcus pluvialis powder-cyclodextrin mixture, coenzyme Q10, black wolfberry extract and stabilizer are added to an appropriate amount of deionized water, and stirred at 45°C and 300 rpm for 20 minutes to form an aqueous phase; under a vacuum degree of -0.08 MPa, the oil phase is slowly added to the aqueous phase, and the high-pressure homogenizer is started at the same time, and homogenization is performed twice at a pressure of 40 MPa to form a uniform and stable emulsion; Post-processing stage: the emulsion was treated with a microfluidizer at a pressure of 120 MPa for three times; the emulsion was then dried using spray freeze drying technology to obtain the final composite powder.
[0010] Optionally, the spray freeze drying technology is to use liquid nitrogen pre-cooled to -40°C as the cooling medium, spray freezing is performed under the conditions of a liquid inlet rate of 5 mL / min and an atomization pressure of 0.3 MPa, and then freeze drying is performed under the conditions of a vacuum degree of 5 Pa and a temperature of -50°C for 48 hours.
[0011] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention achieves the synergistic effect of multiple antioxidant components by adding Haematococcus pluvialis powder, perilla oil, coenzyme Q10 and black wolfberry extract to the composition, which is beneficial for scavenging free radicals through different pathways, inhibiting lipid peroxidation, and making the composition have excellent antioxidant activity.
[0012] (2) The present invention improves the physical and chemical stability of the composition by adding a stabilizer, a composite emulsifier and a cyclodextrin to the composition. The synergistic effect of the three improves the physical and chemical stability of the composition, prevents the emulsification system from stratification and precipitation, delays the oxidative rancidity of the oil and the degradation of the active ingredients, and thus improves the retention rate of active ingredients such as astaxanthin.
[0013] (3) In the preparation method of the present invention, the emulsion is refined by using a microfluidizer, and the water solubility is improved under the combined action of cyclodextrin inclusion and composite emulsifier, so that the antioxidant components are more easily absorbed by the human body. The system is maintained stable by combining with a stabilizer, ensuring the effective release of the components in the body and improving the biological availability. DETAILED DESCRIPTION
[0014] Example 1 The raw material ratio of the composition (by weight): 15 parts of Haematococcus pluvialis powder (astaxanthin content 2.1%), 8 parts of perilla oil (α-linolenic acid content 56%), 1 part of coenzyme Q10, 2 parts of black wolfberry extract, 1 part of vitamin E, 3 parts of composite emulsifier (monoglyceride, sucrose ester and soybean lecithin mass ratio of 2:1:1), 5 parts of cyclodextrin and 1 part of sodium alginate. Preparation method: Pretreatment stage: Haematococcus pluvialis powder and cyclodextrin were mixed according to the mass ratio, and deionized water (8 times the total mass of the two) was added. The mixture was stirred at 50°C and 400 rpm for 30 minutes. At the same time, perilla oil was heated to 60°C under nitrogen protection and maintained for 15 minutes to remove trace oxygen contained therein. Emulsification stage: The composite emulsifier and vitamin E are mixed, and the treated perilla oil is added, and the mixture is stirred at 8000 rpm in a high-speed shearing machine for 10 minutes to form a stable oil phase; the inclusion Haematococcus pluvialis powder-cyclodextrin mixture, coenzyme Q10, black wolfberry extract and stabilizer are added to an appropriate amount of deionized water, and stirred at 45°C and 300 rpm for 20 minutes to form an aqueous phase; under a vacuum degree of -0.08 MPa, the oil phase is slowly added to the aqueous phase, and the high-pressure homogenizer is started at the same time, and homogenization is performed twice at a pressure of 40 MPa to form a uniform and stable emulsion; Post-processing stage: The emulsion was treated with a microfluidizer, the pressure was set to 120 MPa, and the treatment was performed three times; then the emulsion was dried using spray freeze drying technology. When performing the spray freeze drying technology, liquid nitrogen pre-cooled to -40°C was used as the cooling medium, and spray freezing was performed under the conditions of a liquid inlet rate of 5 mL / min and an atomization pressure of 0.3 MPa. Then, freeze drying was performed under the conditions of a vacuum degree of 5 Pa and a temperature of -50°C for 48 hours to obtain the final composite powder.
[0015] Example 2 The raw material ratio of the composition (by weight): 20 parts of Haematococcus pluvialis powder (astaxanthin content 2.2%), 13 parts of perilla oil (α-linolenic acid content 57%), 2 parts of coenzyme Q10, 3 parts of black wolfberry extract, 2 parts of vitamin E, 5 parts of composite emulsifier (monoglyceride, sucrose ester and soybean lecithin mass ratio of 2:1:1), 7 parts of cyclodextrin, 2 parts of xanthan gum and 1 part of sodium carboxymethyl cellulose.
[0016] Preparation method: Pretreatment stage: Haematococcus pluvialis powder and cyclodextrin were mixed according to the mass ratio, and deionized water (8 times the total mass of the two) was added. The mixture was stirred at 50°C and 400 rpm for 30 minutes. At the same time, perilla oil was heated to 60°C under nitrogen protection and maintained for 15 minutes to remove trace oxygen contained therein. Emulsification stage: The composite emulsifier and vitamin E are mixed, and the treated perilla oil is added, and the mixture is stirred at 8000 rpm in a high-speed shearing machine for 10 minutes to form a stable oil phase; the inclusion Haematococcus pluvialis powder-cyclodextrin mixture, coenzyme Q10, black wolfberry extract and stabilizer are added to an appropriate amount of deionized water, and stirred at 45°C and 300 rpm for 20 minutes to form an aqueous phase; under a vacuum degree of -0.08 MPa, the oil phase is slowly added to the aqueous phase, and the high-pressure homogenizer is started at the same time, and homogenization is performed twice at a pressure of 40 MPa to form a uniform and stable emulsion; Post-processing stage: The emulsion was treated with a microfluidizer, the pressure was set to 120 MPa, and the treatment was performed three times; then the emulsion was dried using spray freeze drying technology. When performing the spray freeze drying technology, liquid nitrogen pre-cooled to -40°C was used as the cooling medium, and spray freezing was performed under the conditions of a liquid inlet rate of 5 mL / min and an atomization pressure of 0.3 MPa. Then, freeze drying was performed under the conditions of a vacuum degree of 5 Pa and a temperature of -50°C for 48 hours to obtain the final composite powder.
[0017] Example 3 The raw material ratio of the composition (by weight): 25 parts of Haematococcus pluvialis powder (astaxanthin content 2.3%), 18 parts of perilla oil (α-linolenic acid content 58%), 3 parts of coenzyme Q10, 5 parts of black wolfberry extract, 4 parts of vitamin E, 8 parts of composite emulsifier (the mass ratio of monoglyceride, sucrose ester and soybean lecithin is 2:1:1), 10 parts of cyclodextrin, 2 parts of sodium alginate and 3 parts of xanthan gum.
[0018] Preparation method: Pretreatment stage: Haematococcus pluvialis powder and cyclodextrin were mixed according to the mass ratio, and deionized water (8 times the total mass of the two) was added. The mixture was stirred at 50°C and 400 rpm for 30 minutes. At the same time, perilla oil was heated to 60°C under nitrogen protection and maintained for 15 minutes to remove trace oxygen contained therein. Emulsification stage: The composite emulsifier and vitamin E are mixed, and the treated perilla oil is added, and the mixture is stirred at 8000 rpm in a high-speed shearing machine for 10 minutes to form a stable oil phase; the inclusion Haematococcus pluvialis powder-cyclodextrin mixture, coenzyme Q10, black wolfberry extract and stabilizer are added to an appropriate amount of deionized water, and stirred at 45°C and 300 rpm for 20 minutes to form an aqueous phase; under a vacuum degree of -0.08 MPa, the oil phase is slowly added to the aqueous phase, and the high-pressure homogenizer is started at the same time, and homogenization is performed twice at a pressure of 40 MPa to form a uniform and stable emulsion; Post-processing stage: The emulsion was treated with a microfluidizer, the pressure was set to 120 MPa, and the treatment was performed three times; then the emulsion was dried using spray freeze drying technology. When performing the spray freeze drying technology, liquid nitrogen pre-cooled to -40°C was used as the cooling medium, and spray freezing was performed under the conditions of a liquid inlet rate of 5 mL / min and an atomization pressure of 0.3 MPa. Then, freeze drying was performed under the conditions of a vacuum degree of 5 Pa and a temperature of -50°C for 48 hours to obtain the final composite powder.
[0019] Comparative Example 1 It uses only Haematococcus pluvialis powder (astaxanthin content 2.2%) without compounding with other ingredients or special processing.
[0020] Comparative Example 2 Single perilla oil (57% α-linolenic acid content) is used without compounding with other ingredients or special processing. Comparative Example 3 20 parts of Haematococcus pluvialis powder (astaxanthin content 2.2%), 13 parts of perilla oil (α-linolenic acid content 57%), 2 parts of coenzyme Q10, 3 parts of black wolfberry extract, and 2 parts of vitamin E are simply mixed without using a composite emulsifier, cyclodextrin, and stabilizer, and without adopting the preparation process of the present invention.
[0021] Antioxidant activity assay Determination of DPPH free radical scavenging rate: Referring to the Brand-Williams method, take 2 mL of sample solution (diluted to an appropriate concentration with anhydrous ethanol), add 2 mL of 0.1 mM DPPH ethanol solution, mix well and react in the dark for 30 minutes, measure the absorbance at 517 nm (A sample), and simultaneously measure the absorbance of the mixture of 2 mL of anhydrous ethanol and 2 mL of DPPH solution (A blank) and the absorbance of the mixture of 2 mL of sample solution and 2 mL of anhydrous ethanol (A control).
[0022] DPPH free radical scavenging rate (%) = [1-(A sample-A control) / A blank] × 100%.
[0023] ABTS cation radical scavenging rate determination: Referring to the Re method, equal volumes of 7 mM ABTS solution and 2.45 mM potassium persulfate solution were mixed, and the mixture was allowed to stand in the dark for 12-16 hours to obtain an ABTS cation stock solution; before use, the solution was diluted with phosphate buffered saline (PBS, pH 7.4) to an absorbance of 0.70 ± 0.02 at 734 nm; 0.1 mL of sample solution was added to 3.9 mL of ABTS cation working solution, mixed, and reacted for 6 minutes. The absorbance at 734 nm was measured (A sample), and the absorbance of the blank group (0.1 mL PBS + 3.9 mL ABTS cation working solution) was measured (A blank).
[0024] ABTS cation radical scavenging rate (%) = [1-A sample / A blank] × 100%.
[0025] Determination of antioxidant capacity by FRAP method: Referring to the Benzie method, the FRAP working solution was prepared by mixing 300 mM sodium acetate buffer (pH 3.6), 10 mM tripyridine triazine (TPTZ) solution, and 20 mM ferric chloride solution in a volume ratio of 10:1:1. It was preheated to 37°C before use. 0.1 mL of sample solution was added to 3 mL of FRAP working solution, mixed, and reacted for 4 minutes. The absorbance was measured at 593 nm, and the FRAP value of the sample was calculated based on the FeSO4 standard curve.
[0026] Table 1 shows the results of the antioxidant activity test. Table 1
[0027] According to the data in Table 1, the compositions of Examples 1 to 3 are significantly better than those of Comparative Examples 1 to 3 in terms of DPPH free radical scavenging rate, ABTS free radical scavenging rate and FRAP value, indicating that the synergistic combination of multiple ingredients effectively improves the antioxidant activity; at the same time, the addition of stabilizers in Examples 1 to 3 further optimizes the system performance without affecting the synergistic antioxidant effect.
[0028] Stability test: Store the samples at 40°C and 75% relative humidity, and regularly measure the peroxide value and astaxanthin retention rate (for samples containing astaxanthin). The peroxide value is determined according to GB5009.227-2016, and the astaxanthin content is determined by HPLC. Observe the samples for any signs of stratification or precipitation.
[0029] Astaxanthin retention rate (%) = (measured astaxanthin content at a certain time point / astaxanthin content at the initial time) × 100% Table 2 shows the stability test results Table 2
[0030] According to the data in Table 2, after 60 days of storage, the peroxide value of the compositions of Examples 1 to 3 increased slowly, the astaxanthin retention rate was high, and the appearance was uniform with no stratification or precipitation. The perilla oil of Comparative Example 2 showed slight stratification, and the peroxide value increased significantly. Comparative Example 3 showed obvious stratification and precipitation, and poor stability. Although Comparative Example 4 used a composite emulsifier and cyclodextrin, it still showed slight stratification due to the lack of a stabilizer. This fully demonstrates that the addition of the stabilizer synergizes with the composite emulsifier and cyclodextrin to significantly improve the stability of the composition and effectively prevent oxidation of the components and changes in their physical state.
[0031] In summary, the Haematococcus pluvialis composition containing perilla oil prepared by the present invention significantly improves stability while maintaining excellent antioxidant properties by adding a stabilizer.
[0032] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.
Claims
1. A Haematococcus pluvialis composition containing perilla oil having antioxidant function, characterized in that: The invention comprises the following components by weight: 15-25 parts of Haematococcus pluvialis powder, 8-18 parts of perilla oil, 1-3 parts of coenzyme Q10, 2-5 parts of black wolfberry extract, 1-4 parts of vitamin E, 3-8 parts of composite emulsifier, 5-10 parts of cyclodextrin and 1-5 parts of stabilizer.
2. The antioxidant Haematococcus pluvialis composition containing perilla oil according to claim 1, wherein: The astaxanthin content in the Haematococcus pluvialis powder is not less than 2%, and the α-linolenic acid content in the perilla oil is not less than 55%.
3. The antioxidant Haematococcus pluvialis composition containing perilla oil according to claim 1, wherein: The composite emulsifier consists of monoglyceride, sucrose ester and soybean lecithin in a mass ratio of 2:1:
1.
4. The antioxidant Haematococcus pluvialis composition containing perilla oil according to claim 1, wherein: The stabilizer is one or more combinations of sodium alginate, xanthan gum, and sodium carboxymethyl cellulose.
5. A method for preparing a Haematococcus pluvialis composition containing perilla oil having antioxidant function, characterized in that: The method for preparing the Haematococcus pluvialis composition containing perilla oil and having antioxidant function according to any one of claims 1 to 4 comprises the following steps: Pretreatment stage: Haematococcus pluvialis powder and cyclodextrin were mixed according to the mass ratio, and deionized water (8 times the total mass of the two) was added. The mixture was stirred at 50°C and 400 rpm for 30 minutes. At the same time, perilla oil was heated to 60°C under nitrogen protection and maintained for 15 minutes to remove trace oxygen contained therein. Emulsification stage: The composite emulsifier and vitamin E are mixed, and the treated perilla oil is added, and the mixture is stirred at 8000 rpm in a high-speed shearing machine for 10 minutes to form a stable oil phase; the inclusion Haematococcus pluvialis powder-cyclodextrin mixture, coenzyme Q10, black wolfberry extract and stabilizer are added to an appropriate amount of deionized water, and stirred at 45°C and 300 rpm for 20 minutes to form an aqueous phase; under a vacuum degree of -0.08 MPa, the oil phase is slowly added to the aqueous phase, and the high-pressure homogenizer is started at the same time, and homogenization is performed twice at a pressure of 40 MPa to form a uniform and stable emulsion; Post-processing stage: the emulsion was treated with a microfluidizer at a pressure of 120 MPa for three times; the emulsion was then dried using spray freeze drying technology to obtain the final composite powder.
6. The method for preparing the perilla oil-containing Haematococcus pluvialis composition having antioxidant function as claimed in claim 5, wherein: The spray freeze drying technology uses liquid nitrogen pre-cooled to -40°C as a cooling medium, spray freezing is performed under the conditions of a liquid inlet rate of 5 mL / min and an atomization pressure of 0.3 MPa, and then freeze drying is performed under the conditions of a vacuum degree of 5 Pa and a temperature of -50°C for 48 hours.