Walnut green peel extract and its preparation method and application

Abstract

The present invention discloses a walnut peel extract, a preparation method and an application thereof. It relates to the technical field of agricultural weed control. A preparation method of a walnut peel extract, the extract and an application thereof are provided. The walnut peel extract of the present invention has a significant growth inhibitory effect on a variety of common farmland weeds, including but not limited to barnyard grass, foxtail grass, crabgrass, purslane, and Amaranthus retroflexus. During application: the walnut peel extract (concentrated solution) can be diluted and evenly sprayed on the surface of farmland weeds through a sprayer, or applied to the soil around the roots of the weeds by root irrigation. The dilution multiple depends on the weed species, growth stage and environmental conditions, and is generally 10 to 50 times.

Description

Technical Field

[0001] The present invention relates to the technical field of agricultural weed control, and more particularly to a walnut green peel extract, a preparation method and an application thereof. Background Art

[0002] In modern agricultural production, weed control is crucial for ensuring crop yield and quality. While long-term reliance on chemical herbicides has been effective in controlling weeds in the short term, its drawbacks are becoming increasingly apparent. On the one hand, the overuse of chemical herbicides disrupts soil ecology, destroys beneficial microbial communities, and causes soil compaction and reduced fertility. On the other hand, their residues not only pollute surface and groundwater but also pose the risk of excessive pesticide levels in agricultural products, posing a serious threat to human health. Furthermore, increasing weed resistance to pesticides forces farmers to use increasingly high pesticide dosages, further degrading the environment and raising production costs.

[0003] Walnuts, a widely cultivated economic fruit, often have their green peels disposed of as waste during harvesting and processing. This not only wastes resources but also accumulates and rots naturally, potentially breeding harmful pathogens and negatively impacting the surrounding environment. However, recent research has revealed that green walnut peels are rich in a variety of potentially bioactive secondary metabolites, such as phenols, flavonoids, and terpenoids. These compounds exhibit unique functions in plant defense and allelopathic effects, providing a novel material foundation for the development of novel, green, and environmentally friendly natural herbicides, potentially breaking the traditional weed control dilemma.

[0004] Therefore, whether a walnut green peel extract, a preparation method and application thereof can be provided is an urgent problem to be solved by those skilled in the art. Summary of the Invention

[0005] In view of this, the present invention provides a walnut green peel extract and a preparation method and application thereof.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A method for preparing a walnut green peel extract comprises the following steps:

[0008] (1) Raw material collection: Select walnut green peel and rinse it clean;

[0009] (2) Drying: Dry the washed walnut green peel;

[0010] (3) Grinding: Grinding the dried walnut green peel and sieving to obtain walnut green peel coarse powder;

[0011] (4) Extraction: Using ethanol aqueous solution as solvent, the walnut green peel coarse powder is added to the solvent and ultrasonic-assisted extraction is performed in a water bath;

[0012] After the extraction is completed, the filtrate is filtered, collected, and concentrated under reduced pressure to obtain the walnut peel extract.

[0013] Preferably, step (1) specifically comprises: selecting fresh, disease- and insect-free walnut green peels, rinsing them after picking, removing surface impurities, and draining the water for later use.

[0014] Preferably, step (2) is specifically as follows: drying the washed walnut green peel at a temperature of 40° C. to 50° C. and a vacuum degree of 0.08 MPa to 0.1 MPa for 8 to 12 hours.

[0015] Preferably, step (3) is specifically as follows: the sieving is through a 40-60 mesh sieve.

[0016] Preferably, step (4) is specifically as follows: using 70% to 80% by volume of ethanol aqueous solution as solvent, adding walnut green peel coarse powder to the solvent according to a material-liquid ratio of 1:10 to 1 to 15 g / mL, and performing ultrasonic-assisted extraction for 30 to 60 minutes in a water bath at 55 to 65° C., with an ultrasonic power of 200 to 300 W;

[0017] After the extraction is completed, filter through double-layer gauze while hot, collect the filtrate, and concentrate under reduced pressure to 1 / 3 to 1 / 5 of the original volume to obtain the walnut peel extract.

[0018] The present invention also provides a walnut green peel extract prepared by any of the above preparation methods.

[0019] The present invention also provides a method for using the walnut green peel extract. The method of use is as follows: the walnut green peel extract is diluted and then sprayed or rooted, with the dilution ratio being 10 to 50 times.

[0020] The present invention also provides application of the walnut green peel extract in preparing a herbicide.

[0021] Preferably, the herbicide is used to inhibit the growth of barnyard grass, foxtail grass, crabgrass, purslane or Amaranthus retroflexus.

[0022] Preferably, the herbicide is in the form of a suspension concentrate, a wettable powder, a granule or a nano dosage form.

[0023] It can be seen from the above technical solution that compared with the prior art, the present invention discloses a walnut peel extract and its preparation method and application, and the technical effect achieved is that the walnut peel extract of the present invention has a significant growth inhibitory effect on a variety of common farmland weeds, including but not limited to barnyard grass, foxtail grass, crabgrass, purslane, Amaranthus retroflexus, etc.

[0024] Application: Dilute the walnut peel extract (concentrate) and evenly spray it on the surface of weeds in the field with a sprayer, or apply it to the soil around the weed roots by root irrigation. The dilution ratio depends on the weed species, growth stage, and environmental conditions, and is generally 10 to 50 times. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0026] Figure 1 The accompanying drawing is a process flow chart provided by the present invention.

[0027] Figure 2 The accompanying drawing is a schematic diagram of the inhibitory effect on germination of barnyard grass seeds provided by the present invention.

[0028] Figure 3 The accompanying drawing is a plant height influence diagram provided by the present invention.

[0029] Figure 4 The accompanying drawings are fresh weight impact diagrams provided by the present invention. DETAILED DESCRIPTION

[0030] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with the accompanying drawings. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0031] The present invention discloses a walnut green peel extract and its preparation method and application. Figure 1 .

[0032] Example 1

[0033] A method for preparing a walnut green peel extract comprises the following steps:

[0034] (1) Raw material collection: Select fresh, pest-free walnut green peels, rinse them with clean water immediately after picking, remove surface impurities, and drain the water for later use;

[0035] (2) Drying: Using a low-temperature vacuum drying method, the cleaned walnut green peel was placed in a vacuum drying oven and dried at a temperature of 40°C and a vacuum degree of 0.08 MPa for 8 hours until the green peel became brittle and easy to crush;

[0036] (3) Grinding: Use a universal grinder to grind the dried walnut green peel into powder, and pass it through a 40-mesh sieve to obtain walnut green peel coarse powder;

[0037] (4) Extraction: Using 70% ethanol aqueous solution as solvent, walnut green peel coarse powder was added to the solvent at a solid-liquid ratio of 1:10 (g / mL), and ultrasonic-assisted extraction was performed in a water bath at 55°C for 30 minutes with an ultrasonic power of 200W;

[0038] After the extraction is completed, the mixture is filtered while hot, the filtrate is collected, and concentrated under reduced pressure to 1 / 5 of the original volume to obtain a walnut peel extract (concentrated solution).

[0039] Example 2

[0040] A method for preparing a walnut green peel extract comprises the following steps:

[0041] (1) Raw material collection: fresh, pest-free walnut green peels (5 kg) were selected and immediately rinsed with running water (rinsed 3 times in this embodiment) to remove surface impurities and drain the water for later use;

[0042] (2) Drying: Using a low-temperature vacuum drying method, the cleaned walnut green peel was placed in a vacuum drying oven and dried at a temperature of 45°C and a vacuum degree of 0.09 MPa for 10 hours until the green peel became brittle and easy to crush;

[0043] (3) Grinding: Use a universal grinder to grind the dried walnut green peel into powder, pass it through a 50-mesh sieve, and obtain walnut green peel coarse powder (about 3 kg of coarse powder);

[0044] (4) Extraction: Using 75% ethanol aqueous solution as solvent, the walnut green peel coarse powder was added to the solvent at a solid-liquid ratio of 1:12 (g / mL). Ultrasonic-assisted extraction was performed in a water bath at 60°C for 45 minutes with an ultrasonic power of 250W.

[0045] After the extraction is completed, filter while hot (double-layer gauze), collect the filtrate, and concentrate under reduced pressure (rotary evaporator) to 1 / 3 to 1 / 5 of the original volume (about 2.5 L in this embodiment) to obtain walnut peel extract (concentrated solution, which can be stored in a brown glass bottle and kept in the dark at 4°C for future use).

[0046] Example 3

[0047] A method for preparing a walnut green peel extract comprises the following steps:

[0048] (1) Raw material collection: Select fresh, pest-free walnut green peels, rinse them with clean water immediately after picking, remove surface impurities, and drain the water for later use;

[0049] (2) Drying: Using a low-temperature vacuum drying method, the cleaned walnut green peel was placed in a vacuum drying oven and dried at a temperature of 50°C and a vacuum degree of 0.1 MPa for 12 hours until the green peel became brittle and easy to crush;

[0050] (3) Grinding: Use a universal grinder to grind the dried walnut green peel into powder, and pass it through a 60-mesh sieve to obtain walnut green peel coarse powder;

[0051] (4) Extraction: Using 80% ethanol aqueous solution as solvent, walnut green peel coarse powder was added to the solvent at a solid-liquid ratio of 1:15 (g / mL), and ultrasonic-assisted extraction was performed in a water bath at 65°C for 60 minutes with an ultrasonic power of 300W;

[0052] After the extraction is completed, the mixture is filtered while hot, the filtrate is collected, and concentrated under reduced pressure to 1 / 3 of the original volume to obtain a walnut peel extract (concentrated solution).

[0053] Technical effect verification:

[0054] Experiment on the Inhibition of Echinochloa crusgalli Seed Germination

[0055] Experimental setup: Select plump, uniform-sized barnyardgrass seeds, disinfect them with 0.5% sodium hypochlorite solution for 10 minutes, and rinse them three times with sterile water. Set up five treatment groups:

[0056] A blank control group (CK, sprayed with an equal amount of sterile water), a positive control group (PC, sprayed with a commercially available common chemical herbicide diluted at a recommended dose, such as glyphosate diluted 50 times), a low-concentration treatment group (T1, the walnut green peel extract concentrate prepared in Example 2 was diluted 50 times), a medium-concentration treatment group (T2, the walnut green peel extract concentrate prepared in Example 2 was diluted 30 times), and a high-concentration treatment group (T3, the walnut green peel extract concentrate prepared in Example 2 was diluted 10 times).

[0057] Each treatment group had three replicates, with 50 seeds in each replicate.

[0058] Experimental Procedure: 5 mL of each treatment solution was added to a Petri dish lined with double-layer filter paper to thoroughly moisten the filter paper. Disinfected barnyardgrass seeds were then evenly distributed on the filter paper and placed in a light incubator at 25°C, 2000 lux, 12 hours per day, and 70% humidity. Seed germination was observed daily, with germination defined as the radicle breaking through the seed coat by 2 mm. Observation was continued for 7 consecutive days, and the germination rate, germination index, and inhibition rate were calculated.

[0059] Experimental results:

[0060] Germination rate: The germination rate of the blank control group was 92%, the germination rate of the positive control group was 12%, the germination rate of the low concentration treatment group was 68%, the germination rate of the medium concentration treatment group was 35%, and the germination rate of the high concentration treatment group was 17%.

[0061] Germination index: the germination index of the blank control group was 7.36, the germination index of the positive control group was 0.98, the germination index of the low concentration treatment group was 5.44, the germination index of the medium concentration treatment group was 2.8, and the germination index of the high concentration treatment group was 1.44.

[0062] Inhibition rate: According to the formula inhibition rate = (control germination rate - treatment germination rate) / control germination rate × 100%, the inhibition rate of the low concentration treatment group was 26.09%, the inhibition rate of the medium concentration treatment group was 62.07%, and the inhibition rate of the high concentration treatment group was 80.43%. Figure 2 .

[0063] The results showed that walnut peel extract had a significant inhibitory effect on the germination of barnyard grass seeds, and the inhibitory effect increased with increasing concentration.

[0064] Experiment on the Inhibitory Effect on the Growth of Setaria Seedlings

[0065] Experimental setup: Selected Setaria viridis seedlings with uniform growth and 2-3 true leaves were transplanted into plastic pots (15 cm in diameter) filled with standard nutrient soil, with 6 plants per pot. Six treatment groups were set up, of which 5 treatment groups were the same as the experiment on the inhibition of barnyard grass seed germination. In addition, the nanoformulation in the nanoformulation treatment group was prepared using conventional technology. See Zhai Jing, Zhao Liwen, Gao Dana, et al. Preliminary study on the effect of nanopesticides on the control of rice stem borer [J]. China Rice, 2024, 30(02): 95-97+101.

[0066] Each treatment group had 3 replicates, with a total of 18 pots.

[0067] Experimental procedure: After the seedlings have grown for 3 days, use a precisely calibrated handheld sprayer to evenly spray each treatment solution on the leaves and stems of the seedlings. The spray amount is based on the formation of a uniform water film on the leaves, about 20 mL per pot. After treatment, the flower pots are placed in an intelligent greenhouse, which automatically adjusts the light supplement according to the changes in external natural light. The temperature is 22°C to 28°C and the humidity is 60% to 80%. Treatment is carried out every 7 days, for a total of 3 treatments. 10 days after the last treatment, the plant height, stem diameter, fresh weight and dry weight of the Setaria viridis seedlings in each treatment group are measured, and the growth inhibition rate is calculated by comparing with the data before treatment.

[0068] Experimental results: Plant height: The average plant height of the blank control group increased from 10cm before treatment to 35cm, the average plant height of the positive control group was 9cm, the average plant height of the low concentration treatment group was 25cm, the average plant height of the medium concentration treatment group was 18cm, the average plant height of the high concentration treatment group was 12cm, and the average plant height of the nano dosage form treatment group was 15cm. Figure 3 ;

[0069] Stem thickness: The average stem thickness of the blank control group increased from 2mm before treatment to 3mm, the average stem thickness of the positive control group was 1.2mm, the average stem thickness of the low-concentration treatment group was 2.2mm, the average stem thickness of the medium-concentration treatment group was 1.8mm, the average stem thickness of the high-concentration treatment group was 1.4mm, and the average stem thickness of the nano-formulation treatment group was 1.6mm.

[0070] Fresh weight: The average fresh weight of the blank control group increased from 3g before treatment to 6g, the average fresh weight of the positive control group was 1.2g, the average fresh weight of the low-concentration treatment group was 2.2g, the average fresh weight of the medium-concentration treatment group was 1.8g, the average fresh weight of the high-concentration treatment group was 1.4g, and the average fresh weight of the nano-formulation treatment group was 1.6g. Figure 4 .

[0071] Dry weight: The average dry weight of the blank control group increased from 0.5g before treatment to 1g, the average dry weight of the positive control group was 0.2g, the average dry weight of the low-concentration treatment group was 0.6g, the average dry weight of the medium-concentration treatment group was 0.4g, the average dry weight of the high-concentration treatment group was 0.3g, and the average dry weight of the nanoformulation treatment group was 0.35g.

[0072] Growth inhibition rate = (control group - treatment group) / control group × 100%

[0073] The growth inhibition rates of plant height, stem diameter, fresh weight and dry weight were calculated. The plant height growth inhibition rate was 28.57% in the low concentration treatment group, 48.57% in the medium concentration treatment group, 65.71% in the high concentration treatment group, and 57.14% in the nanoformulation treatment group; the stem diameter growth inhibition rate was 26.67% in the low concentration treatment group, 40% in the medium concentration treatment group, 53.33% in the high concentration treatment group, and 46.67% in the nanoformulation treatment group; the fresh weight growth inhibition rate was 33.33% in the low concentration treatment group, 58.33% in the medium concentration treatment group, 70% in the high concentration treatment group, and 63.33% in the nanoformulation treatment group; the dry weight growth inhibition rate was 40% in the low concentration treatment group, 60% in the medium concentration treatment group, 70% in the high concentration treatment group, and 65% in the nanoformulation treatment group.

[0074] Data show that walnut peel extract has a strong inhibitory effect on the growth of foxtail grass seedlings. The nano dosage form has an outstanding long-term inhibitory effect after multiple applications, and the higher the concentration, the more obvious the inhibitory effect.

[0075] Field plot trials

[0076] Test site: Select an area of ​​about 600m 2 The farmland has medium soil fertility and flat terrain. The previous crop is corn. There are many kinds of weeds, mainly barnyard grass, foxtail grass, purslane, and Amaranthus retroflexus, which are distributed relatively evenly.

[0077] Experimental design: The experimental field was divided into 15 plots, each with an area of ​​40m 2 Five treatment groups were randomly arranged in blocks to investigate the inhibitory effect on Echinochloa crus-galli seed germination. Each treatment group was replicated three times. A 1-meter-wide isolation zone was set between plots to prevent cross-interference between the agents.

[0078] Experimental Procedure: During the weed's peak growth period (plant height 10-20 cm), each treatment solution was evenly sprayed onto the weed surface using a knapsack sprayer at a rate of 30 L / mu to ensure uniform coverage. Application was conducted on sunny, breezy days with temperatures between 25°C and 28°C. Weed growth was observed after application. The number and fresh weight of weeds in each plot were measured 7, 14, and 21 days after application, and the control efficacy was calculated based on the number of weeds and fresh weight.

[0079] Test results:

[0080] Plant number control effect: 7 days after application, the average number of plants in the blank control group was 120 plants / m 2 The average number of plants in the positive control group was 20 plants / m 2 The average number of plants in the low concentration treatment group was 80 plants / m 2 The average number of plants in the medium concentration treatment group was 45 plants / m 2 The average number of plants in the high concentration treatment group was 30 plants / m 2 .

[0081] According to the formula plant number control effect = (number of plants in the control area - number of plants in the treatment area) / number of plants in the control area × 100%, it is calculated that the plant number control effect of the low concentration treatment group is 33.33%, the plant number control effect of the medium concentration treatment group is 62.5%, and the plant number control effect of the high concentration treatment group is 75%.

[0082] 14 days after application, the control efficiency of each treatment group fluctuated. The control efficiency of the low-concentration treatment group was about 30%, the medium-concentration treatment group was about 60%, and the high-concentration treatment group was about 70%.

[0083] 21 days after application, the control efficiency of the low-concentration treatment group was 25%, the control efficiency of the medium-concentration treatment group was 55%, and the control efficiency of the high-concentration treatment group was 65%.

[0084] Fresh weight control effect: 7 days after application, the average fresh weight of the blank control group was 300g / m 2The average fresh weight of the positive control group was 50g / m 2 The average fresh weight of the low concentration treatment group was 200g / m 2 The average fresh weight of the medium concentration treatment group was 100g / m 2 The average fresh weight of the high concentration treatment group was 70g / m 2 .

[0085] According to the formula fresh weight control effect = (fresh weight of control area - fresh weight of treatment area) / fresh weight of control area × 100%, it was calculated that the fresh weight control effect of the low concentration treatment group was 33.33%, the fresh weight control effect of the medium concentration treatment group was 66.67%, and the fresh weight control effect of the high concentration treatment group was 76.67%.

[0086] 14 days after application, the fresh weight control efficiency of the low concentration treatment group was about 32%, the fresh weight control efficiency of the medium concentration treatment group was about 61%, and the fresh weight control efficiency of the high concentration treatment group was about 70%.

[0087] 21 days after application, the fresh weight control efficiency of the low concentration treatment group was about 28%, the fresh weight control efficiency of the medium concentration treatment group was about 55%, and the fresh weight control efficiency of the high concentration treatment group was about 65%.

[0088] The results showed that walnut peel extract had a good comprehensive control effect on a variety of weeds in the field. The control effect of the medium and high concentration treatment groups was close to or reached the level of chemical herbicides. Although the control effect decreased over time, it could still maintain a certain weed control ability.

[0089] The various embodiments in this specification are described in a progressive manner, and each embodiment focuses on the differences from other embodiments. The same or similar parts between the various embodiments can be referenced to each other.

[0090] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. The application of walnut green peel extract in the preparation of herbicides, characterized in that: The following steps are involved: (1) Raw material collection: Select walnut green skin and rinse it clean; (2) Drying: Dry the washed walnut green skin; (3) Grinding: Grind the dried walnut green peel and sieve to obtain walnut green peel coarse powder; (4) Extraction: Using ethanol-water solution as solvent, add walnut green peel coarse powder into the solvent and use ultrasound-assisted extraction in a water bath; After the extraction is completed, the filtrate is filtered, collected, and concentrated under reduced pressure to obtain the walnut peel extract; The herbicide is used for inhibiting the growth of barnyard grass, foxtail grass, crabgrass, purslane or Amaranthus retroflexus; Usage: Dilute the walnut peel extract and spray or irrigate the roots with a dilution ratio of 10 to 50 times.

2. The use according to claim 1, characterized in that Step (1) is specifically as follows: fresh, pest-free walnut green peels are selected, rinsed clean after picking, surface impurities are removed, and the water is drained for later use.

3. The use according to claim 2, characterized in that Step (2) is specifically as follows: drying the washed walnut green peel at a temperature of 40°C to 50°C and a vacuum degree of 0.08MPa to 0.1MPa for 8 to 12 hours.

4. The use according to claim 3, characterized in that Step (3) is specifically as follows: the sieving: 40-60 mesh sieve.

5. The use according to claim 4, characterized in that Step (4) is specifically as follows: using 70% to 80% by volume of ethanol aqueous solution as solvent, adding walnut green peel coarse powder to the solvent at a material-liquid ratio of 1:10 to 1 to 15 g / mL, and performing ultrasonic-assisted extraction for 30 to 60 minutes in a water bath at 55 to 65°C with an ultrasonic power of 200 to 300 W; After the extraction is completed, filter through double-layer gauze while hot, collect the filtrate, and concentrate under reduced pressure to 1 / 3 to 1 / 5 of the original volume to obtain the walnut peel extract.

6. The use according to claim 5, characterized in that The herbicide is in the form of a suspension concentrate, a wettable powder, a granule or a nano dosage form.

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