Preparation method and application of peanut shell extract
Peanut shell extract was prepared by ethanol reflux method and activated carbon adsorption, which was used to prepare water-free hand sanitizer, which solved the problem of low utilization rate of peanut shells and achieved efficient utilization of peanut shells and environmental protection.
Patent Information
- Application Number
- CN202410152237.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-02-03
- Publication Date
- 2025-08-05
AI Technical Summary
The low utilization rate of peanut shell by-products leads to waste accumulation and polluting the environment. The prior art fails to effectively utilize resveratrol and flavonoids in peanut shells.
Resveratrol and flavonoids in peanut shells were extracted by ethanol reflux method and activated carbon adsorbent, and peanut shell extract was prepared, and used to prepare water-free hand sanitizer. By measuring its content and performance, it ensures its effect as an antioxidant.
The prepared peanut shell extract water-free hand sanitizer has good heat resistance and cold resistance, and its antibacterial effect is comparable to that of commercially available products. It solves the problem of peanut shell waste pollution and improves the utilization rate of peanut shells.
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Abstract
Description
Technical Field
[0001] The present application belongs to the field of peanut shell extraction technology, and in particular relates to a preparation method of peanut shell extract and its application. Background Art
[0002] Resveratrol is mainly found in plants such as peanuts, grape skins (red wine), Japanese knotweed, mulberries, pistachios, blueberries, and pineapples. The highest content of resveratrol is found in grape skins, peanut shells, and Japanese knotweed roots.
[0003] Grapes from different regions and varieties grow in different environments, resulting in varying resveratrol content. Pesticide use significantly reduces the amount of resveratrol synthesized by the grapes themselves. Compared to peanut shells, grape skins contain far less resveratrol, making extraction expensive. Furthermore, resveratrol extraction from grape skins is primarily a French method, where winemaking produces a significant amount of grape skins left over after pressing the juice, which are then reused to extract resveratrol. However, my country's grape planting area is far smaller than its peanut planting area. Data shows that my country's grape production is 14.31 million tons, while peanut production is 17.9929 million tons. Furthermore, my country's annual per capita wine consumption is only 0.5 liters, representing only 6% of the global average. Both domestic and international demand for wine is far less than that for peanuts.
[0004] Polygonum cuspidatum itself is a traditional Chinese medicine. It contains a large amount of resveratrol and has an extremely simple extraction process. However, Polygonum cuspidatum contains emodin, tannins and various phenolic compounds, which are toxic to the human body. Therefore, Polygonum cuspidatum cannot be used as a raw material for resveratrol extraction.
[0005] my country's peanut breeding and cultivation technology is currently at the forefront of the world, with 6,000 varieties and yields far exceeding those of other oil and fat crops. Peanut consumption in my country is primarily concentrated in Shandong and Henan provinces, with distribution across the country. Peanut consumption increased from 9.74 million tons in 2009 to 12.05 million tons in 2019, a 23.7% increase. This large amount of peanuts is consumed or extracted for oil, resulting in tens of thousands of tons of peanut shells. Summary of the Invention
[0006] The present application provides a preparation method of peanut shell extract and its application, which solves the problem of low utilization rate of peanut shell by-products and reduces the accumulation of peanut shell waste to pollute the environment.
[0007] The present invention provides a method for preparing a peanut shell extract and its application, which specifically comprises the following steps:
[0008] Step (1): preparing peanut shells into powder, adding the powder into a solvent, refluxing, and collecting reflux liquid 1;
[0009] Step (2): adding a solvent to the reflux solution 1 in step (1), and refluxing to obtain a reflux solution 2;
[0010] Step (3): adding the reflux liquid 2 of step (2) to an adsorbent, and performing rotary evaporation and drying to obtain a peanut shell extract.
[0011] In one embodiment,
[0012] The solvent in step (1) is 70% ethanol, and the amount used is 200 mL.
[0013] In one embodiment,
[0014] The reflux temperature in step (1) is 50°C.
[0015] In one embodiment,
[0016] The reflux time in step (1) is 2 h.
[0017] In one embodiment,
[0018] The solvent in step (2) is 70% ethanol, and the amount used is 200 mL.
[0019] In one embodiment,
[0020] The reflux temperature in step (2) is 50°C.
[0021] In one embodiment,
[0022] The reflux time in step (2) is 2 h.
[0023] In one embodiment,
[0024] The adsorbent in step (3) is activated carbon.
[0025] The present application also provides an application of peanut shell extract, and a peanut shell extract water-free hand sanitizer prepared according to the preparation method of peanut shell extract in the above embodiment.
[0026] In one embodiment,
[0027] The components of the peanut shell extract water-free hand sanitizer, calculated by mass fraction, specifically include: 15% anhydrous ethanol, 5% propylene glycol, 10% triethanolamine, 2% carbomer resin, 4-9% peanut shell extract, 1% methylparaben, and distilled water to 100%.
[0028] The present application provides a preparation method and application of peanut shell extract, wherein resveratrol and flavonoids in peanut shells are extracted by ethanol, and the contents of resveratrol and flavonoids are determined, and resveratrol and flavonoids are used as antioxidants to prepare a new waterless hand sanitizer, thereby preparing a waterless hand sanitizer containing peanut shell extract, and evaluating the performance of the waterless hand sanitizer. The waterless hand sanitizer has good heat and cold resistance, a suitable pH value, and an antibacterial degree comparable to that of commercially available waterless hand sanitizers; the present application solves the problems of low utilization rate of peanut shell by-products, reduces the accumulation of peanut shell waste polluting the environment, and solves the problem of helping rural areas. DETAILED DESCRIPTION
[0029] In order to make the technical problems, technical solutions and beneficial effects to be solved by this application more clear and understandable, this application is further described in detail. It should be understood that the specific embodiments described herein are only used to explain this application and are not used to limit this application.
[0030] Example 1 Preparation of extract
[0031] 1-1 Preparation of peanut shell extract
[0032] Weigh 10 g of peanut shells, grind them into powder, add 200 mL of 70% ethanol, heat and reflux in a 50°C water bath for 2 h, collect the ethanol solution, add 200 mL of 70% ethanol and repeat the above extraction steps, collect and combine the filtrate, add an appropriate amount of activated carbon, let it stand, filter, remove the ethanol solvent on a rotary evaporator, and obtain the peanut shell extract after drying.
[0033] 1-2 Results
[0034] 1-2-1 Peanut Shell Extract Extraction Rate
[0035] As shown in Table 1, different extraction methods have a certain influence on the extraction rate. Among them, Soxhlet extraction yields less product than condensation reflux extraction.
[0036] Table 1 Peanut shell extraction rate
[0037]
[0038] 2 Determination of peanut shell extract content
[0039] 2-1 Determination of resveratrol content in peanut shells
[0040] 2-1-1 Determination of the standard curve equation
[0041] Ten portions of 5 mg resveratrol standard were weighed and placed in different volumetric flasks. Standard solutions of different concentrations were prepared according to a gradient. The absorbance was measured at a wavelength of 306 nm. The linear equation of the standard curve was obtained by fitting, with the concentration C of the resveratrol standard solution as the abscissa and the absorbance value A as the ordinate: y = 0.1316x + 0.0072, R 2 =0.9999.
[0042] 2-1-2 Determination of resveratrol content
[0043] Weigh 1.0 g of powder, add 60% ethanol at a solid-liquid ratio of 1:20 g / mL, extract at 40°C for 90 min to obtain a crude resveratrol extract, centrifuge, take the supernatant, measure its absorbance A at a wavelength of 306 nm, calculate the tannin concentration in the sample according to the standard curve, and convert it into the resveratrol content in peanut shells.
[0044] 2-2 Determination of total flavonoids in peanut shells
[0045] 2-2-1 Determination of the standard curve equation
[0046] Accurately weigh 10 mg of rutin standard (dried to constant weight at 105°C) and place it in a 50 mL volumetric flask. Dissolve it with 60% ethanol at room temperature and dilute to 50 mL with distilled water (i.e., the rutin concentration is 0.1 mol / mL). Pipette 0 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL and 5.0 mL of the above rutin standard solution into a 10 mL volumetric flask, respectively, add 0.3 mL of 0.05 mol / mL NaNO2 aqueous solution, shake well and let it stand for 6 minutes, add 0.3 mL of 0.1 mol / mL Al(NO3)3 and let it stand for another 6 minutes, then add 4 mL of 0.04 mol / mL NaOH aqueous solution, dilute to 10 mL with distilled water, shake well and let it stand for 10-20 minutes. At a wavelength of 510 nm, the first tube of solution was used as a blank to measure the absorbance values at different concentrations. A standard curve was drawn with the absorbance value as the ordinate and the concentration as the abscissa, and the regression equation was obtained: y = 4.35x - 0.0059, R2 = 0.9991.
[0047] Determination of 2-2-2 flavonoid content
[0048] 5.0 g of peanut shell powder was weighed and ethanol reflux extraction was performed. The effects of extraction temperature of 40-90 ° C, ethanol volume fraction of 40-90%, extraction time of 30-150 min, extraction times of 1-3 times, and solid-liquid ratio of 1:6-14 (g / mL) on the extraction of total flavonoids were investigated respectively. The extract was collected and diluted to 500 mL with distilled water as the peanut shell flavonoid test solution. The absorbance was determined according to the rutin standard curve method, and the peanut shell flavonoid content and flavonoid yield were calculated.
[0049] 2-3 Results
[0050] (1) Analysis of optimal measurement conditions
[0051] The absorption spectrum of the resveratrol sample has a maximum absorption peak at λ=306 nm, so the product with a wavelength near 306 nm was selected using a UV-1800 ultraviolet spectrophotometer.
[0052] The absorption spectrum of the rutin sample has a maximum absorption peak at λ=510 nm. Therefore, 510 nm was selected as the detection wavelength in the NaNO2-Al(NO3)3-NaOH color reaction experiment.
[0053] (2) Standard curve and regression equation
[0054] The regression equation of the resveratrol standard curve is A(y)=0.8167x+0.1896, R 2 =0.9985, the linear range is 0.06-0.3 mg / mL; the regression equation of the rutin standard curve is A(y)=26.57x+0.01325, R 2 =0.9995, and the linear range is 0.01-0.05 mg / mL.
[0055] (3) Sample component content
[0056] The experiment showed that the absorption wavelength of resveratrol was 306 nm, and the resveratrol content in the sample was calculated to be 18.2%. The absorbance of flavonoids was 0.543, and the flavonoids content in the sample was calculated to be 3.0%.
[0057] 2-3 Scavenging rate of peanut shell flavonoids on DPPH free radicals
[0058] The scavenging rates of peanut shell flavonoids at different mass concentrations on DPPH free radicals were measured, and the results are shown in Table 2.
[0059] Table 2 Scavenging rate of flavonoids on DPPH free radicals
[0060]
[0061] The DPPH free radical has a single electron, a strong absorption at 517nm, and its alcohol solution appears purple. When TBHQ reagent is present, its absorption gradually disappears due to pairing with its single electron, thus causing the free radical to fall off and taking away other harmful free radicals.
[0062] The scavenging rate of 1.00 mg / mL TBHQ against DPPH free radicals was 91.3%. As shown in Table 2, the peanut shell flavonoid sample solution had a good scavenging effect on DPPH free radicals. The scavenging effect increased with increasing sample solution concentration, but the scavenging rate no longer increased with increasing sample solution concentration after reaching a certain concentration. In this experiment, the scavenging rate reached a maximum of 92.0% at a sample solution concentration of 1.00 mg / mL. The scavenging rate of 1.00 mg / mL TBHQ against DPPH free radicals was 91.3%, which is close to the scavenging rate at the same sample solution concentration. This indicates that flavonoids extracted from peanut shells can replace TBHQ as free radical scavengers.
[0063] The ethanol volume fraction was 62%, the extraction temperature was 41°C, the extraction time was 91 min, and the solid-liquid ratio was 1:20 g / mL. At this time, the resveratrol extraction amount was 1.054 mg / g, which was basically consistent with the model prediction value of 1.041 mg / g. The antioxidant activity of resveratrol in peanut shell crude extract was evaluated by scavenging DPPH free radicals and hydroxyl free radicals. IC 50 The results showed that resveratrol in peanut shell crude extract has good scavenging ability for DPPH free radicals and hydroxyl free radicals, and can be used as a new source of antioxidants.
[0064] Example 2 Application of Peanut Shell Extract
[0065] 1. Hand sanitizer ingredients
[0066] See Table 3.
[0067] Table 3 Hand sanitizer ingredients
[0068]
[0069] In the prescription, propylene glycol is a moisturizer, triethanolamine, anhydrous ethanol is a bactericidal agent, anhydrous ethanol and distilled water are solvents, methyl paraben is a preservative, carbomer resin is a modified thickener, and peanut shell extract is an antioxidant.
[0070] We prepared peanut shell extracts containing 4%, 5%, 6%, 7%, 8% and 9% by mass (concentration 1 mol / mL) respectively. Accurately weigh 0.039g of DPPH and dilute to 50mL with 95% ethanol, i.e. 6mmol / L DPPH. After diluting 10 times, 0.6mmol / L DPPH was obtained for use. To 2mL of 0.6mmol / L DPPH solution, 1mL of the sample with different concentrations was added (the blank control was replaced with an equal amount of distilled water), the total volume was 3mL, and the mixture was mixed. After standing at room temperature for 15 minutes, the absorbance of the DPPH mixed solution at 517nm was measured in a cuvette. Each absorbance was measured in parallel 3 times, and the average value was taken. The clearance rate was calculated as follows:
[0071] Clearance % = [1-(Ai-Aj) / A0]*100%
[0072] Where A0 is the absorbance of a mixture of 1 mL of distilled water and 2 mL of 0.6 mmol / L DPPH at 517 nm; Ai is the absorbance of a mixture of 2 mL of 0.6 mmol / L DPPH ethanol solution and 1 mL of sample at 517 nm; and A is the absorbance of a mixture of 2 mL of 95% ethanol and 1 mL of sample at 517 nm.
[0073] 2 Evaluation of physical and chemical indicators of hand sanitizer
[0074] 2-1 Heat and cold resistance test
[0075] The test was conducted in accordance with the national standard QB / T34855-2017 for facial masks. Specifically, for the heat resistance test, the sample was placed in two test tubes, approximately 8 cm high, plugged with rubber stoppers, and one tube was placed in a constant-temperature incubator pre-set at 40°C. After 24 hours, the tube was removed and allowed to return to room temperature before visual comparison with the sample in the other tube. If there was no significant difference between the post-test sample and the pre-test sample, the sample passed.
[0076] For the cold resistance test, the samples were placed in two test tubes, each about 8 cm high, plugged with rubber stoppers, and one of them was placed in a constant temperature incubator pre-adjusted to -8°C. After 24 hours, it was taken out and returned to room temperature. Visual comparison was made with the sample in the other test tube. If there was no obvious difference between the sample and the one before the test, it was qualified.
[0077] 2-2 pH determination
[0078] Dissolve 5g of peanut shell hand sanitizer in 100mL of purified water, bring to a slight boil, cool to room temperature, and measure the pH of the suspension with pH test paper. The ideal pH range is 4.0-10.0.
[0079] 2-3 Antibacterial assay
[0080] The antibacterial performance test was divided into a peanut shell extract antibacterial hand sanitizer group, a regular hand sanitizer group (without peanut shell extract), and a positive control group (commercially available hand sanitizer), with each group tested three times. The specific procedure was: paper slips dipped in the three groups of hand sanitizers were placed on culture media inoculated with Escherichia coli, Staphylococcus aureus, and Candida albicans, respectively. After 24 hours, the size of the inhibition zone was observed. Based on the determination of the inhibition zone size of the three parallel groups, the average value of the three groups was taken. If the number of bacteria in the peanut shell extract antibacterial hand sanitizer group was significantly reduced after the test compared to before the test, the sample passed the test.
[0081] The present application provides a preparation method and application of peanut shell extract, wherein resveratrol and flavonoids in peanut shells are extracted by ethanol, and the contents of resveratrol and flavonoids are determined, and resveratrol and flavonoids are used as antioxidants to prepare a new waterless hand sanitizer, thereby preparing a waterless hand sanitizer containing peanut shell extract, and evaluating the performance of the waterless hand sanitizer. The waterless hand sanitizer has good heat and cold resistance, a suitable pH value, and an antibacterial degree comparable to that of commercially available waterless hand sanitizers; the present application solves the problems of low utilization rate of peanut shell by-products, reduces the accumulation of peanut shell waste polluting the environment, and solves the problem of helping rural areas.
[0082] The above description is only a preferred embodiment of the present application and is not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application should be included in the scope of protection of the present application.
Claims
1. A method for preparing peanut shell extract, characterized in that: The specific steps include: Step (1): preparing peanut shells into powder, adding the powder into a solvent, refluxing, and collecting reflux liquid 1; Step (2): adding a solvent to the reflux solution 1 in step (1), and refluxing to obtain a reflux solution 2; Step (3): adding the reflux liquid 2 of step (2) to an adsorbent, and performing rotary evaporation and drying to obtain a peanut shell extract.
2. The method for preparing peanut shell extract according to claim 1, wherein: The solvent in step (1) is 70% ethanol, and the amount used is 200 mL.
3. The method for preparing peanut shell extract according to claim 1, wherein: The reflux temperature in step (1) is 50°C.
4. The method for preparing a peanut shell extract according to claim 1, wherein: The reflux time in step (1) is 2 h.
5. The method for preparing peanut shell extract according to claim 1, wherein: The solvent in step (2) is 70% ethanol, and the amount used is 200 mL.
6. The method for preparing a peanut shell extract according to claim 1, characterized in that: The reflux temperature in step (2) is 50°C.
7. The method for preparing peanut shell extract according to claim 1, characterized in that: The reflux time in step (2) is 2h.
8. The method for preparing peanut shell extract according to claim 1, characterized in that: The adsorbent in step (3) is activated carbon.
9. An application of peanut shell extract, characterized in that: A peanut shell extract water-free hand sanitizer prepared according to the preparation method of a peanut shell extract according to any one of claims 1-8.
10. The use of a peanut shell extract according to claim 9, characterized in that: The components of the peanut shell extract water-free hand sanitizer, calculated by mass fraction, specifically include: 15% anhydrous ethanol, 5% propylene glycol, 10% triethanolamine, 2% carbomer resin, 4-9% peanut shell extract, 1% methylparaben, and distilled water to 100%.