Walnut green seedcase extract as well as preparation method and application thereof

Abstract

The invention discloses a walnut green seedcase extract as well as a preparation method and application thereof. Relates to the technical field of agricultural weeding. The invention provides a preparation method of a walnut green seedcase extract, the extract and application thereof. The walnut green seedcase extract disclosed by the invention has a remarkable growth inhibition effect on various common farmland weeds, including but not limited to barnyard grass, green bristlegrass, digitaria sanguinalis, purslane, amaranthus retroflexus and the like. During application, the walnut green seedcase extract (concentrated solution) can be diluted and then uniformly sprayed on the surfaces of farmland weeds through a sprayer, or applied to soil around the roots of the weeds in a root irrigation manner. And the dilution ratio is determined according to weed types, growth stages and environmental conditions, and is generally 10-50 times.

Description

Technical Field

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

[0002] In modern agricultural production, weed control is a key link in ensuring crop yield and quality. Although long-term reliance on chemical herbicides can effectively control weed growth in the short term, many disadvantages are becoming increasingly prominent. On the one hand, the abuse of chemical herbicides has caused an imbalance in soil ecology, destroyed beneficial microbial communities, and caused soil compaction and decreased fertility; on the other hand, its residue problem not only pollutes surface water and groundwater, but also causes the risk of excessive pesticides in agricultural products, seriously threatening human health. In addition, weed resistance is increasing year by year, forcing farmers to continuously increase the dosage of drugs, further deteriorating the environment and raising production costs.

[0003] Walnuts are widely planted as economic fruits, and their green peels are mostly treated as waste during the picking and processing process, which not only causes idle resources and waste, but also may breed harmful pathogens due to natural accumulation and rotting, which has a negative impact on the surrounding environment. However, basic research in recent years has gradually revealed that walnut green peels are rich in a variety of secondary metabolites with potential biological activity, such as phenols, flavonoids, and terpenoid compounds. These components have unique functions in plant defense and allelopathic effects, providing a new material basis for the development of new, green, and environmentally friendly natural herbicides, which is expected to break the dilemma of traditional weed control.

[0004] Therefore, whether it is possible to provide a walnut green peel extract and a preparation method and application thereof 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 solution:

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

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

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

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

[0011] (4) Extraction: Using ethanol aqueous solution as solvent, adding walnut green peel coarse powder into the solvent, and using ultrasound-assisted extraction under water bath conditions;

[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 0.08MPa to 0.1MPa for 8 to 12 hours.

[0015] Preferably, step (3) specifically comprises: the sieving: 40-60 mesh sieve.

[0016] Preferably, step (4) is specifically as follows: using 70% to 80% by volume ethanol aqueous solution as solvent, adding walnut green peel coarse powder to the solvent at a solid-liquid ratio of 1:10 to 1 to 15 g / mL, and extracting by ultrasound-assisted extraction for 30 to 60 minutes at a water bath temperature of 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, and the dilution multiple is 10 to 50 times.

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

[0021] Preferred: 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, a wettable powder, a granule or a nano dosage form.

[0023] It can be seen from the above technical scheme that, compared with the prior art, the present invention discloses a walnut peel extract and a preparation method and application thereof, 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: After diluting, the walnut peel extract (concentrate) can be evenly sprayed on the surface of weeds in the farmland 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. 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 drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying 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 be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. 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 creative work 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: fresh, pest-free walnut green peels are selected, and immediately rinsed with clean water after picking to remove surface impurities, and the water is drained for later use;

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

[0036] (3) crushing: using a universal crusher to crush the dried walnut green peel into powder, and passing it through a 40-mesh sieve to obtain walnut green peel coarse powder;

[0037] (4) Extraction: Using 70% ethanol aqueous solution by volume as solvent, the 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 for 30 minutes in a water bath at 55°C 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 peel (5 kg) was selected, and immediately rinsed with running water (rinsed 3 times in this embodiment) to remove surface impurities, and the water was drained for later use;

[0042] (2) Drying: Using a low-temperature vacuum drying method, the washed walnut green peel is placed in a vacuum drying oven and dried for 10 hours at a temperature of 45° C. and a vacuum degree of 0.09 MPa, until the green peel becomes brittle and hard 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), and ultrasonic-assisted extraction was performed for 45 minutes at a water bath temperature of 60°C 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 away from light 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: fresh, pest-free walnut green peels are selected, and immediately rinsed with clean water after picking to remove surface impurities, and the water is drained for later use;

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

[0050] (3) crushing: using a universal crusher to crush the dried walnut green peel into powder, and passing it through a 60-mesh sieve to obtain walnut green peel coarse powder;

[0051] (4) Extraction: Using 80% ethanol aqueous solution by volume as solvent, the 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 for 60 minutes at a water bath temperature of 65°C with an ultrasonic power of 300 W;

[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 Seed Germination of Echinochloa crusgalli

[0055] Experimental setup: Select full, uniform-sized barnyard grass seeds, disinfect them with 0.5% sodium hypochlorite solution for 10 minutes, and rinse them with sterile water three times. Set up 5 treatment groups, namely:

[0056] A blank control group (CK, sprayed with an equal amount of sterile water), a positive control group (PC, sprayed with commercially available common chemical herbicides diluted at recommended doses, 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 3 replicates, with 50 seeds in each replicate.

[0058] Experimental operation: 5 mL of each treatment solution was added to a culture dish covered with double-layer filter paper to fully moisten the filter paper, and then the sterilized barnyard grass seeds were evenly placed on the filter paper and placed in a light incubator at 25°C, 2000 lux, 12 hours / day, and 70% humidity. The seed germination was observed and recorded every day, and the germination standard was when the radicle broke through the seed coat by 2 mm. The observation was continued for 7 days, and the seed 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 calculated to be 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 viridis seedlings

[0065] Experimental setup: Select Setaria viridis seedlings with consistent growth and 2 to 3 true leaves and transplant them 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 preparation of the nanoformulation in the nanoformulation treatment group was a conventional process, 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 operation: After the seedlings have been 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 leaves just forming a uniform water film, about 20mL / pot. After treatment, the flower pots are placed in an intelligent greenhouse, and the light supplement is automatically adjusted according to the changes in natural light outside. The temperature is 22℃~28℃ and the humidity is 60%~80%. Treat once every 7 days, for a total of 3 times. Ten days after the last treatment, the plant height, stem thickness, fresh weight and dry weight of the Setaria seedlings in each treatment group were measured, and the growth inhibition rate was 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-dosage form 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 dosage form 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 nano dosage form 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 nano dosage form 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 nano dosage form 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 nano dosage form treatment group.

[0074] The data showed that walnut peel extract had a strong inhibitory effect on the growth of Setaria seedlings. The nano dosage form had an outstanding long-term inhibitory effect after multiple applications, and the higher the concentration, the more obvious the inhibitory effect.

[0075] Field plot test

[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, Amaranthus retroflexus, etc., which are relatively evenly distributed.

[0077] Experimental design: The experimental field was divided into 15 plots, each with an area of ​​40m 2 , randomized block arrangement, set up 5 treatment groups, and experimented on the inhibition of barnyard grass seed germination. Each treatment group was repeated 3 times. A 1m wide isolation zone was set between the cells to prevent the drugs from interfering with each other.

[0078] Test operation: During the vigorous growth period of weeds (plant height 10cm-20cm), use a backpack sprayer to spray each treatment solution evenly on the weed surface at a spray volume of 30L / mu to ensure uniform coverage of the agent. The weather was sunny and breezy on the day of application, and the temperature was 25℃-28℃. After application, the growth of weeds was observed, and the number and fresh weight of weeds in each plot were investigated 7 days, 14 days, and 21 days after application, and the control effect of the number and fresh weight were calculated.

[0079] Test results:

[0080] Plant number control effect: 7 days after application, the average plant number of 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 protective effect = (fresh weight of control area - fresh weight of treatment area) / fresh weight of control area × 100%, it was calculated that the fresh weight protective effect of the low concentration treatment group was 33.33%, the fresh weight protective effect of the medium concentration treatment group was 66.67%, and the fresh weight protective effect of the high concentration treatment group was 76.67%.

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

[0087] 21 days after application, the fresh weight protection efficiency of the low concentration treatment group was about 28%, the fresh weight protection efficiency of the medium concentration treatment group was about 55%, and the fresh weight protection 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 enables one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be 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 will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a walnut green peel extract, characterized in that: The following steps are involved: (1) Raw material collection: Select walnut green skin and rinse it; (2) Drying: Drying the washed walnut green skin; (3) crushing: crushing the dried walnut green peel and sieving to obtain walnut green peel coarse powder; (4) Extraction: Using ethanol aqueous solution as solvent, adding walnut green peel coarse powder into the solvent, and using ultrasound-assisted extraction under water bath conditions; After the extraction is completed, the filtrate is filtered, collected, and concentrated under reduced pressure to obtain the walnut peel extract.

2. The preparation method according to claim 1, characterized in that 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.

3. The preparation method 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 0.08 MPa to 0.1 MPa for 8 to 12 hours.

4. The preparation method according to claim 3, characterized in that: Step (3) specifically includes: the sieving: 40-60 mesh sieve.

5. The preparation method 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 solid-liquid ratio of 1:10 to 1 to 15 g / mL, and extracting by ultrasound-assisted extraction for 30 to 60 minutes at a water bath temperature of 55 to 65° C., with an ultrasound 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 walnut green peel extract prepared by the preparation method according to any one of claims 1 to 5.

7. The method for using the walnut green peel extract according to claim 6, characterized in that: The method of use is as follows: the walnut green peel extract is diluted and sprayed or rooted, and the dilution multiple is 10 to 50 times.

8. Use of the walnut green peel extract according to claim 6 in the preparation of herbicides.

9. The use according to claim 8, characterized in that The herbicide is used for inhibiting the growth of barnyard grass, foxtail grass, crabgrass, purslane or Amaranthus retroflexus.

10. The use according to claim 9, characterized in that The herbicide is in the form of a suspension, a wettable powder, a granule or a nano dosage form.

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