Preparation method of antioxidant prepared by extracting malus hallasisiana seed lipid-soluble substances
Patent Information
- Application Number
- CN202611480027.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2026-09-22
- Publication Date
- 2026-11-03
AI Technical Summary
Existing prickly pear seed extraction processes are inefficient. Room temperature extraction has low dissolution efficiency, and high temperature extraction will destroy polyunsaturated fatty acids. Existing processes cannot effectively utilize prickly pear seed resources, and most existing antioxidants are artificially synthesized, which has limitations.
Anhydrous ethanol was used as the solvent, combined with ultrasonic extraction technology, and the extraction was carried out at a low temperature of 25-80℃ in the dark. The material-to-liquid ratio was 1/5-1/20 g/mL, the ultrasonic power was 35-85%, and the extraction time was 10-80 min. The lipid-soluble substances were then obtained by saponification-acid back titration method and vacuum evaporation purification.
It improves the extraction efficiency of fat-soluble substances from prickly pear seeds, protects polyunsaturated fatty acids from oxidation, and the extract has excellent antioxidant properties, making it suitable for food, cosmetics, and health products, with the potential for large-scale production.
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Figure CN123023724A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of antioxidant production technology, specifically to a method for preparing antioxidants by extracting fat-soluble substances from prickly pear seeds. Background Technology
[0002] Prickly pear seeds are the seeds obtained after removing the pulp from the prickly pear fruit. Juicing fresh prickly pears generates a large amount of waste seeds, most of which are discarded along with the fruit pulp, resulting in extremely low resource utilization. Prickly pear seeds contain abundant esters, polyunsaturated fatty acids, and other active ingredients, possessing the potential to be developed into raw materials for natural antioxidants. Currently, the food and cosmetics industries have an increasing demand for natural antioxidants, but artificially synthesized antioxidants have certain limitations.
[0003] Existing extraction processes for prickly pear seeds have significant drawbacks: conventional room-temperature extraction has low dissolution efficiency, while high-temperature extraction destroys polyunsaturated fatty acids and esters in the seeds, resulting in unstable antioxidant properties of the extract. Currently, there is a lack of a preparation process for preparing antioxidant extracts from prickly pear seeds using anhydrous ethanol ultrasonic extraction, and the development of related product applications is insufficient. Developing this process to realize the resource utilization of prickly pear seed by-products has practical value. Summary of the Invention
[0004] To address the aforementioned problems, this invention proposes a method for extracting fat-soluble substances from prickly pear seeds to prepare antioxidants. This method improves the extraction efficiency of fat-soluble substances, protects polyunsaturated fatty acids from oxidative degradation, clarifies the application pathways of the extract as a natural antioxidant in the food, cosmetics, and health product fields, and enhances the added value of prickly pear processing by-products.
[0005] To solve the above-mentioned technical problems, the technical solution proposed by this invention is as follows: a method for preparing an antioxidant by extracting fat-soluble substances from prickly pear seeds, the steps of which are as follows: Raw material pretreatment: Separate the pulp of fresh prickly pear fruit to obtain clean, mold-free prickly pear seeds, dry and crush them, pass them through a sieve of not less than 10 mesh, and seal and store them away from light.
[0006] Ultrasonic extraction: Anhydrous ethanol is used as solvent, the material-to-liquid ratio is 1 / 5-1 / 20 g / mL, the temperature is 25-80℃, the power ratio is 35-85%, and the extraction is carried out in the dark for 10-80 min. Solid-liquid separation: The extract is filtered to remove residue, and the supernatant is collected; Volume adjustment: Transfer the supernatant to a 100mL volumetric flask and dilute to volume with anhydrous ethanol to obtain a prickly pear seed extract rich in fat-soluble substances.
[0007] During the experimental phase, the saponification-acid back titration method was used to determine the saponifiable components of each fat-soluble substance, thereby screening for the optimal extraction process. This step can be omitted if no detection is required.
[0008] Anhydrous ethanol removal: The collected supernatant is evaporated under reduced pressure to remove anhydrous ethanol, yielding a lipid-soluble substance.
[0009] Formula for detecting and calculating the saponification value of fat-soluble substances: This invention uses the saponification-acid back titration method to determine the saponification value of fat-soluble substances in a sample, as shown in the following formula: Where: X is the proportionality coefficient (sodium hydroxide and sulfuric acid); V0 is the volume of sulfuric acid consumed in the blank; V1 is the volume of sulfuric acid consumed in the sample; C is the molar concentration of the sulfuric acid standard solution; and 56.1 is the molar mass of potassium hydroxide.
[0010] Compared with existing technologies, the advantages of this invention are: the raw material is waste prickly pear seeds, which is inexpensive and solves the problem of waste pollution; the ultrasonic cavitation effect improves the extraction rate; the whole process is carried out at low temperature and in the dark, which protects the unsaturated esters well; and the DPPH free radical scavenging experiment has verified that the extract has excellent antioxidant properties.
[0011] In the food processing industry, it can be added to edible oils, pastries, and meat products to eliminate free radicals, delay oil rancidity, and extend the shelf life of food. In the skin care and cosmetics industry, it can be added to lotions, creams, serums, sunscreens, and other products to eliminate free radicals in the skin, provide antioxidant protection, and delay skin aging. In the oral health supplement processing industry, it can help eliminate free radicals in the body and play a role in the body's antioxidant regulation. The entire process is simple to operate, takes less time, and the ethanol solvent can be recovered. It is green and safe and has the potential for large-scale production. Attached Figure Description
[0012] Figure 1 This is a bar chart illustrating the effect of ultrasonic extraction time on the saponification value of fat-soluble substances according to an embodiment of the present invention. Figure 2 This is a bar chart illustrating the effect of ultrasonic extraction temperature on the saponification value of fat-soluble substances according to an embodiment of the present invention. Figure 3 This is a bar chart illustrating the effect of the ultrasonic extraction liquid-to-material ratio on the saponification value of fat-soluble substances according to an embodiment of the present invention. Figure 4 This is a bar chart illustrating the effect of ultrasonic extraction power on the saponification value of fat-soluble substances according to an embodiment of the present invention. Figure 5 This is a line graph comparing the free radical scavenging rates of prickly pear seed extract stock solution, fresh prickly pear juice stock solution, ascorbic acid (VC), and DPPH free radical scavenging rate of prickly pear seed extract in embodiments of the present invention. Detailed Implementation
[0013] The following embodiments are a further detailed description of the present invention.
[0014] Example 1: Effect of ultrasonic extraction time on the saponification value of fat-soluble substances in the extract.
[0015] Dried prickly pear seeds were pulverized and passed through an 80-mesh sieve. Five equal portions of 5g each of dried prickly pear seed powder were weighed out. The material-to-liquid ratio was fixed at 1 / 10g / mL, the temperature was 50℃, and the ultrasonic power was 50%. The mixture was ultrasonically extracted with anhydrous ethanol, with the ultrasonic time varying only to five different values: 20min, 30min, 40min, 50min, and 60min. The entire extraction process was conducted in the dark. After extraction, the residue was removed by vacuum filtration, and the volume was adjusted to 100mL with anhydrous ethanol. 10mL of each extract was transferred and analyzed according to the saponification-acid back-tipping method described earlier for determining the saponifiable value of fat-soluble substances. The saponifiable value of fat-soluble substances in each group was calculated using the formula.
[0016] The test results showed that the saponification value of fat-soluble substances in the prickly pear seed extract was the highest when the ultrasonic extraction time was 40 min, which was 103.88 mg KOH / g.
[0017] Example 2: Effect of ultrasonic extraction temperature on the saponification value of fat-soluble substances in the extract.
[0018] With a fixed material-to-liquid ratio of 1 / 10 g / mL, an ultrasonic extraction time of 40 min, and an ultrasonic power of 50%, anhydrous ethanol was used for ultrasonic extraction. Only the ultrasonic temperature was changed to five gradients: 40℃, 50℃, 60℃, 70℃, and 80℃. All other conditions and subsequent detection procedures were the same as in Example 1.
[0019] The test results showed that the saponification value of fat-soluble substances in the prickly pear seed extract was highest at an ultrasonic extraction temperature of 70℃, reaching 83.04 mg KOH / g. Example 3: Effect of ultrasonic extraction material-to-liquid ratio on the saponification value of fat-soluble substances in the extract.
[0020] The extraction was performed at a fixed time of 40 min, a temperature of 70°C, and an ultrasonic power of 50%. Anhydrous ethanol was used for ultrasonic extraction, with only the material-to-liquid ratio changed to five gradients: 1 / 5 g / mL, 1 / 8 g / mL, 1 / 10 g / mL, 1 / 12 g / mL, and 1 / 15 g / mL. All other conditions and subsequent detection procedures were the same as in Example 1.
[0021] The test results showed that when the ultrasonic extraction ratio was 1 / 10 g / mL, the saponification value of fat-soluble substances in the prickly pear seed extract was the highest, reaching 78.75 mg KOH / g.
[0022] Example 4: Effect of ultrasonic extraction power on the saponification value of fat-soluble substances in the extract.
[0023] The extraction was performed at a fixed time of 40 min, a temperature of 70°C, and a material-to-liquid ratio of 1 / 10 g / mL. Anhydrous ethanol was used for ultrasonic extraction, with only the ultrasonic extraction power varying at five gradients: 30%, 40%, 50%, 60%, and 70%. All other conditions and subsequent detection procedures were the same as in Example 1.
[0024] The test results showed that when the ultrasonic extraction power was 60%, the saponification value of fat-soluble substances in the prickly pear seed extract was the highest, at 97.51 mg KOH / g.
[0025] Example 5: Orthogonal optimization experiment + DPPH activity determination and control.
[0026] This experiment investigated four factors—ultrasonic time, ultrasonic temperature, ultrasonic power, and solid-liquid ratio—under three different levels of orthogonal experiments to determine the optimal extraction process parameters. The order of influence of the four factors on the saponifiable value of the fat-soluble substances in the extract was: extraction temperature > solid-liquid ratio > extraction power > extraction time. Considering the order of influence of the orthogonal experiments and range analysis of single factors, the optimal process of this invention yielded a saponifiable value of 120.36 mg KOH / g for the fat-soluble substances in the prickly pear seed extract.
[0027] Antioxidant activity detection and comparative experiments.
[0028] The DPPH antioxidant activity of the product from the optimal process was tested (including VC control and fresh prickly pear juice control). The in vitro antioxidant activity of the prickly pear seed fat-soluble substance extract prepared by the optimal process of this invention was evaluated by the DPPH free radical scavenging method. At the same time, ascorbic acid (VC) positive control and fresh prickly pear juice control were set up to conduct a triple activity comparison test.
[0029] Detection method: Use 0.2 mmol / L DPPH anhydrous ethanol standard solution, store in the dark for later use. Set up a blank control group, a sample reaction group, and a sample background group. After mixing the systems of each group according to the same ratio, react at room temperature in the dark for 30 min, and measure the absorbance at a wavelength of 517 nm.
[0030] Formula for calculating DPPH free radical scavenging rate: In the formula: A0 is the absorbance of the blank group; A1 is the absorbance of the sample reacting with DPPH; A2 is the absorbance of the sample background group.
[0031] All samples in this experiment were not diluted; the original extracts were used for analysis. The results are as follows: 1. The extract of fat-soluble substances from prickly pear seeds prepared by the orthogonal optimal process of this invention: direct detection of the stock solution shows that the DPPH free radical scavenging rate can reach 94.63%; 2. The oil obtained by vacuum evaporation of the extract from the optimal process of this invention: When the oil is mixed with anhydrous ethanol at a ratio of 1:1, the DPPH free radical scavenging rate can reach 89.06%; 3. Fresh prickly pear juice: Direct testing of the undiluted juice showed a DPPH free radical scavenging rate of 74%. 4. Ascorbic acid (VC) control solution: Prepare a 1.0 mg / mL standard solution for detection, and the DPPH free radical scavenging rate is 86.4%.
[0032] Comparative results show that the ultrasound-assisted anhydrous ethanol extraction of lipid-soluble substances from prickly pear seeds in this invention exhibits excellent in vitro antioxidant capacity, with free radical scavenging activity higher than the positive control VC and significantly superior to fresh prickly pear juice. This demonstrates that this process can effectively enrich antioxidant esters in prickly pear seeds, and the product has stable functional activity and high application value.
[0033] In summary, the extraction process optimized by this invention through single-factor experiments combined with orthogonal experiments is stable, reliable, and highly efficient. The resulting extract of fat-soluble substances from prickly pear seeds possesses excellent antioxidant activity and is suitable for industrial production and the development of functional antioxidant products.
[0034] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
Claims
1. A method for preparing an antioxidant by extracting fat-soluble substances from prickly pear seeds, characterized in that, Includes the following steps: S1: Raw material pretreatment: Separate the prickly pear pulp from the prickly pear seeds to obtain prickly pear seeds. Dry, crush, and sieve the prickly pear seeds with a mesh size of not less than 10 to obtain prickly pear seed powder. S2: Ultrasonic extraction: Using anhydrous ethanol as the extraction solvent, add the prickly pear seed powder for light-protected ultrasonic extraction; control the material-liquid ratio to be 1 / 5-1 / 20 g / mL, the extraction temperature to be 25-80℃, the ultrasonic power ratio to be 35-85%, and the extraction time to be 10-80 min. S3: Solid-liquid separation: The mixed system after extraction is subjected to solid-liquid separation to remove residue and collect the supernatant; S4: Solvent removal: Remove anhydrous ethanol from the supernatant to obtain the fat-soluble substance from the prickly pear seed, which is a natural antioxidant product.
2. The preparation method according to claim 1, characterized in that, Step 2 involves ultrasonic extraction, which is performed entirely in the dark to prevent the polyunsaturated fatty acids in the prickly pear seeds from undergoing oxidative degradation.
3. The preparation method according to claim 1, characterized in that, Step 3, after solid-liquid separation, also includes a volume adjustment step: the collected supernatant is transferred to a volumetric flask and adjusted to volume with anhydrous ethanol to obtain a prickly pear seed extract rich in fat-soluble substances.
4. The preparation method according to claim 1, characterized in that, Step 4 removes anhydrous ethanol by vacuum evaporation.
5. The preparation method according to claim 1, characterized in that, The optimal extraction conditions were obtained through single-factor combined orthogonal experiments: ultrasonic extraction time 40 min, extraction temperature 70℃, material-to-liquid ratio 1 / 10 g / mL, and ultrasonic power ratio 60%.
6. The application of the fat-soluble substance from prickly pear seeds prepared by the method according to any one of claims 1-5 as a natural antioxidant.
7. The preparation method according to claim 1, characterized in that, The natural antioxidants are applied in food processing systems to scavenge free radicals, delay the oxidation and spoilage of oils and cooked foods, and extend the shelf life of food.
8. The preparation method according to claim 1, characterized in that, The food products mentioned are edible oils, pastries, or meat products.
9. The preparation method according to claim 1, characterized in that, The natural antioxidants are applied to skincare and cosmetic systems, added to lotions, creams, serums, or sunscreens to eliminate free radicals in the skin, achieving antioxidant protection and delaying skin aging.
10. The preparation method according to claim 1, characterized in that, The natural antioxidants mentioned above are used in oral health supplements to eliminate free radicals in the body, thereby achieving antioxidant regulation and alleviating the damage to the body caused by oxidation.