Method for jointly preparing amino acid-containing water-soluble fertilizer by using traditional Chinese medicine residues and rape seed cakes

Abstract

The invention relates to a method for jointly preparing amino acid-containing water-soluble fertilizer by using traditional Chinese medicine residues and rape seed cakes, the traditional Chinese medicine residues and the rape seed cakes which are wide in source are adopted as raw materials, and the traditional Chinese medicine residues are effectively utilized to reduce environmental pollution; the enzymatic hydrolysate is filtered and centrifuged by adopting a membrane concentration method to obtain the plant source amino acid stock solution, the biological activity of alkaloid, flavone, volatile oil and other substances in the amino acid stock solution is effectively maintained, the final product contains various active substances such as flavonoid, coumarin, phenolic acid, terpenoid, amino acid, organic acid and the like, the content ratio of the flavonoid substance reaches 13%, and the content ratio of the volatile oil reaches 13%. The substance has the effects of bacteriostasis, sterilization and disease prevention. When the water-soluble fertilizer is applied to field crop and fruit and vegetable planting, the nutritional requirements of crop growth can be met, the crop yield can be increased, the crop quality can be improved, the occurrence of crop diseases and insect pests can be effectively inhibited, and the green and sustainable development of agriculture can be promoted.

Description

Technical Field

[0001] The invention belongs to the technical field of preparation of water-soluble fertilizer containing amino acids, and particularly relates to a method for preparing water-soluble fertilizer containing amino acids by utilizing traditional Chinese medicine residues and rapeseed cakes. Background Art

[0002] Water-soluble fertilizer is a multi-component compound fertilizer that can be completely soluble in water. It can dissolve quickly in water, is easily absorbed by crops, and has a high absorption and utilization rate. Water-soluble fertilizers can be used in drip irrigation, sprinkler irrigation and other facility agriculture to meet the needs of water-fertilizer integration. Water-soluble fertilizers mainly include macro-element water-soluble fertilizers, medium-element water-soluble fertilizers, trace element water-soluble fertilizers, humic acid-containing water-soluble fertilizers, organic water-soluble fertilizers and amino acid-containing water-soluble fertilizers. Amino acid-containing water-soluble fertilizers have gradually attracted attention due to their small molecular weight, balanced nutrition, and easy absorption and utilization. However, the amino acid-containing water-soluble fertilizers on the market currently focus on the amino acid content. With the development of precision fertilization and green agriculture in facility agriculture and the promotion of the "water-soluble fertilizer +" fertilization model, the market has put forward higher requirements for the functions of amino acid-containing water-soluble fertilizers. Single-nutrient amino acid-containing water-soluble fertilizers can no longer meet market needs. The active synergistic substances with fertilizers as carriers and the synergistic effect of fertilizers will be welcomed by the market. "Water-soluble fertilizer containing amino acids +", "water-soluble medicinal fertilizer containing amino acids" and the like will meet the new demand for water-fertilizer integration that combines functional and nutritional types, and will be conducive to promoting precision fertilization and achieving the goal of green agricultural development with high resource efficiency and good environment.

[0003] The planting area of ​​Chinese herbal medicines in my country has reached 2.4 million hectares, and the amount of drug residues produced by Chinese herbal medicines reaches 60 to 70 million tons each year. The main treatment methods for drug residues are incineration, landfill, and stacking, which not only pollute the environment but also waste resources.

[0004] The existing Chinese invention patent CN117700277A is an amino acid water-soluble fertilizer used for tomato planting, which contains sodium alginate oligosaccharides, gibberellins and sodium nitrophenolate, etc. Its preparation process and raw materials are different from those of the present invention, and it has not been confirmed that the water-soluble fertilizer contains flavonoids, coumarins, phenolic acids, terpenes, amino acids, organic acids and other active substances, as well as the effects of the active substances on tomato growth. Summary of the invention

[0005] The purpose of the present invention is to solve the above problems and propose a method for preparing amino acid-containing water-soluble fertilizer by combining traditional Chinese medicine residues and rapeseed cake. On the one hand, nutrients such as crude protein and active substances such as alkaloids and flavonoids in the traditional Chinese medicine residues are fully utilized to achieve growth-promoting, insecticidal and antibacterial effects; on the other hand, the rich plant-derived amino acids and additionally added animal-derived amino acids in rapeseed cakes can be used to meet the needs of crop growth, improve crop products, and enhance crop quality, and can also effectively inhibit the occurrence of crop diseases and insect pests, thereby promoting green and sustainable development of agriculture.

[0006] To achieve the above object, the present invention provides the following technical scheme: a method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake, wherein the raw materials are Chinese medicine residue and rapeseed cake, and the Chinese medicine residue contains coptis root, pinellia tuber, tuckahoe, ophiopogon japonicus, artemisia annua, camphor tree root and elsholtzia ciliata, and the specific preparation method comprises the following steps;

[0007] S1. Crushing and soaking: crush the Chinese medicine residue and rapeseed cake, use a 40-60 mesh screen to obtain a powder, soak the powder with distilled water at a material-liquid ratio of 1:7-1:10 at 60-80 ° C for 2-4 hours, and stir every 10-30 minutes during the soaking process;

[0008] S2. Enzymolysis: Add 2% to 5% of the total enzyme amount of proteolytic enzyme, enzymolyze in a water bath at 40 to 60 ° C for 4 to 5 hours to obtain an enzymolysis solution, and stir every 10 to 30 minutes during the enzymolysis process;

[0009] S3. The enzymatic hydrolysate in step S2 is filtered and centrifuged, and the enzymatic hydrolysate is highly concentrated into a plant-derived amino acid stock solution at a volume ratio of 1:7 to 1:10 by a membrane concentration method;

[0010] S4. Adding animal-derived amino acid stock solution to the plant-derived amino acid stock solution to obtain a mixed amino acid stock solution;

[0011] S5. Add 5% to 20% inorganic salt to the mixed amino acid stock solution to obtain amino acid-containing water-soluble fertilizer, in which the organic matter content is as high as 120g / L, and it contains a variety of active substances, including flavonoids, coumarins, phenolic acids, terpenes, amino acids and organic acids, and the content of flavonoids accounts for 13%.

[0012] Furthermore: the proteolytic enzyme added in the enzymatic hydrolysis process in step S2 is selected from one or a mixture of neutral protease, papain, cellulase, and lipase.

[0013] Further: the enzymolysis solution obtained after enzymolysis in step S2 is heated to 80-100° C. for inactivation treatment, the inactivation time is 10-30 minutes, and the enzymolysis solution is filtered and centrifuged after inactivation.

[0014] Further: the animal-derived amino acids in step S4 are one or a mixture of fish meal, meat and bone meal, and animal hair.

[0015] Further: the inorganic salt added in step S5 includes calcium nitrate, calcium chloride, magnesium chloride, and magnesium sulfate. When adding the inorganic salt, at least two of them are selected.

[0016] Furthermore: the free amino acid content in the amino acid water-soluble fertilizer is not less than 100g / L, the secondary element content is not less than 30g / L, and the water-insoluble matter content is not higher than 50g / L.

[0017] Compared with the prior art, the present invention has the following beneficial effects:

[0018] The raw materials of the invention, Chinese medicinal residues and rapeseed cakes, are widely available and rich in resources, providing a large amount of raw materials for amino acid-containing water-soluble fertilizers, and can effectively utilize the Chinese medicinal residues to reduce environmental pollution caused by traditional treatment methods such as incineration and burial.

[0019] The amino acid-containing water-soluble fertilizer adopts the membrane concentration method to filter and centrifuge the enzymatic hydrolyzate, which effectively maintains the biological activity of alkaloids, flavonoids, volatile oils and other substances in the amino acid stock solution. After non-targeted metabolomics detection and analysis, the amino acid-containing water-soluble fertilizer contains flavonoids, coumarins, phenolic acids, terpenes, amino acids and organic acids and other active substances, among which the content of flavonoids accounts for 13%. This substance has antibacterial, bactericidal and disease prevention effects, which can not only effectively reduce the occurrence of crop diseases and pests, but also promote crop growth; and plant-derived amino acids are easily absorbed by crops, which plays an important role in promoting crop root growth, increasing crop yield and improving crop quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings in the following description are only for more clearly illustrating the embodiments of the present invention or the technical solutions in the prior art. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0021] Figure 1 It is the total ion chromatogram of non-targeted metabolites of the water-soluble fertilizer containing amino acids of the present invention;

[0022] Figure 2 This is a chromatogram of targeted metabolites of flavonoids in the water-soluble fertilizer containing amino acids of the present invention. DETAILED DESCRIPTION

[0023] In order to enable those skilled in the art to better understand and implement the technical solution of the present invention, the present invention is further described below in conjunction with specific embodiments. However, the embodiments are only intended to illustrate the present invention and not to limit the present invention.

[0024] A method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake. The raw materials are Chinese medicine residue and rapeseed cake. The Chinese medicine residue contains coptis root, pinellia tuber, tuckahoe, ophiopogon japonicus, artemisia annua, camphor tree root, Elsholtzia ciliata and the like.

[0025] Traditional Chinese medicine residues contain a large amount of nutrients such as cellulose, lignin, crude protein, etc., as well as a certain amount of bioactive substances such as alkaloids, quinones, flavonoids, steroids, saponins, tannins, etc. These bioactive ingredients have medicinal value and have certain inhibitory and preventive effects on pests and diseases. The flavonoids rich in the residues of traditional Chinese medicines such as Coptis chinensis, Pinellia ternata, Poria cocos, Ophiopogon japonicus, Artemisia annua, Camphor tree roots, and Elsholtzia ciliata are a kind of plant-derived biological pesticides, which have certain insecticidal effects on aphids, whiteflies, cotton bollworms, diamondback moths, etc.; alkaloids are toxic to insects and have inhibitory effects on fungi, and can control crop diseases and pests; active substances such as artemisinin, anethole, and volatile oils have significant antibacterial and insecticidal effects. Through the secondary utilization of bioactive substances in traditional Chinese medicine residues, it is possible to reduce environmental pollution caused by the treatment of traditional Chinese medicine residues and reduce the use of pesticides.

[0026] The present invention collects a kind of compound Chinese medicine residue waste generated in the production process of a pharmaceutical company to produce amino acid-containing water-soluble fertilizer, and the specific steps are as follows:

[0027] Embodiment 1

[0028] S1. Crush the Chinese medicine residues and rapeseed cakes such as coptis root, pinellia tuber, tuckahoe, ophiopogon japonicus, artemisia annua, camphor root, and elsholtzia cava, and pass through a 40-mesh sieve, and soak them in distilled water at a material-liquid ratio of 1:8 at 60°C for 2 hours, stirring every 10 minutes during the soaking process;

[0029] S2. Add 2% of the total enzyme amount of proteolytic enzyme, enzymolysis in a 40°C water bath for 4 hours, stirring every 10 minutes during the enzymolysis process;

[0030] S3. The enzymatic hydrolysate was filtered and centrifuged, and the enzymatic hydrolysate was highly concentrated into a plant-derived amino acid stock solution at a volume ratio of 1:7 by membrane concentration;

[0031] S4. Adding animal-derived amino acid stock solution to the plant-derived amino acid stock solution to obtain a mixed amino acid stock solution;

[0032] S5. Add 5% calcium chloride and 10% magnesium chloride to the mixed amino acid stock solution to obtain a water-soluble fertilizer containing amino acids, the indicators of which meet the requirements of free amino acid content of not less than 100g / L, secondary element content (the sum of calcium and magnesium content) of not less than 30g / L, and water-insoluble matter content of not more than 50g / L.

[0033] Embodiment 2

[0034] S1. Crush the Chinese medicine residues and rapeseed cakes of Coptis chinensis, Pinellia ternata, Poria cocos, Ophiopogon japonicus, Artemisia annua, Camphor tree root, Elsholtzia ciliata, etc., pass through a 50-mesh sieve, and soak them in distilled water at a material-liquid ratio of 1:9 at 70°C for 3 hours, stirring every 20 minutes during the soaking process;

[0035] S2. Add 3% of the total enzyme amount of proteolytic enzyme, enzymolysis in a 50°C water bath for 4 hours, stirring every 20 minutes during the enzymolysis process;

[0036] S3. The enzymatic hydrolysate was filtered and centrifuged, and the enzymatic hydrolysate was highly concentrated into a plant-derived amino acid stock solution at a volume ratio of 1:8 by membrane concentration;

[0037] S4. Adding animal-derived amino acid stock solution to the plant-derived amino acid stock solution to obtain a mixed amino acid stock solution;

[0038] S5. Add 10% calcium nitrate and 11% magnesium chloride raw materials to the mixed amino acid stock solution to obtain a water-soluble fertilizer containing amino acids, the indicators of which meet the requirements of free amino acid content of not less than 100g / L, secondary element content (the sum of calcium and magnesium content) of not less than 30g / L, and water-insoluble matter content of not more than 50g / L.

[0039] Embodiment 3

[0040] S1. Crush the Chinese medicine residues and rapeseed cakes such as Coptis chinensis, Pinellia ternata, Poria cocos, Ophiopogon japonicus, Artemisia annua, Camphor tree root, Elsholtzia ciliata, etc., pass through a 60-mesh sieve, and soak them in distilled water at a material-liquid ratio of 1:10 at 80°C for 4 hours, stirring every 30 minutes during the soaking process;

[0041] S2. Add 4% of the total enzyme amount of proteolytic enzyme, enzymolysis in a 60°C water bath for 5 hours, stirring every 30 minutes during the enzymolysis process;

[0042] S3. The enzymatic hydrolysate was filtered and centrifuged, and the enzymatic hydrolysate was highly concentrated into a plant-derived amino acid stock solution at a volume ratio of 1:9 by membrane concentration;

[0043] S4. Adding animal-derived amino acid stock solution to the plant-derived amino acid stock solution to obtain a mixed amino acid stock solution;

[0044] S5. Add 11% calcium nitrate and 10% magnesium chloride raw materials to the mixed amino acid stock solution to obtain an amino acid-containing water-soluble fertilizer, which meets the indicators of free amino acid content of not less than 100g / L, medium element content (the sum of calcium and magnesium content) of not less than 30g / L, and water-insoluble matter content of not more than 50g / L.

[0045] The performance indicators of the amino acid-containing water-soluble fertilizer prepared in the above embodiment are shown in Table 1:

[0046] Table 1 Performance indexes of water-soluble fertilizer containing amino acids

[0047]

[0048] The results in Table 1 show that the amino acid-containing water-soluble fertilizers prepared in the three embodiments of the present invention all meet the national standard for amino acid-containing water-soluble fertilizers (NY1429-2010).

[0049] The three amino acid-containing water-soluble fertilizers prepared in Examples 1-3 were used to carry out field fertilizer efficiency tests. The Yanyu tomato variety was selected. A total of 5 treatments were set up, each with 3 replicates. The area of ​​each test plot was 5m 2 , 18 tomato plants in each plot, randomly distributed in the plots. Treatment 1 was sprayed with the amino acid water-soluble fertilizer prepared in Example 1; Treatment 2 was sprayed with the amino acid water-soluble fertilizer prepared in Example 2; Treatment 3 was sprayed with the amino acid water-soluble fertilizer prepared in Example 3; Treatment 4 was the control group, sprayed with a commercially available amino acid water-soluble fertilizer (indicators: free amino acid content ≥ 100 g / L, calcium + magnesium ≥ 30 g / L), and Treatment 5 was a blank control (sprayed with an equal amount of clean water).

[0050] All treatment groups applied basal fertilizer one month before planting tomatoes, and applied 100kg / mu of bio-organic fertilizer as basal fertilizer. During the entire growth period of tomatoes, amino acid water-soluble fertilizer or clean water (set according to different treatment groups) was sprayed on the leaves for a total of 5 times. The spraying amount was appropriate to have liquid dripping on the leaves. The spraying volume of each treatment group was the same. The amino acid water-soluble fertilizer was diluted 1000 times, sprayed twice in the seedling stage (after the second watering of tomatoes, amino acid water-soluble fertilizer was sprayed once every 15 days, and sprayed twice), sprayed once in the fruit setting stage (sprayed once with amino acid water-soluble fertilizer after flowering), and sprayed twice in the fruiting stage (the first spray was sprayed when the first bunch of fruits entered the rapid expansion period, and the second spray was sprayed once 15 days later with amino acid water-soluble fertilizer). The spraying time was before 10 am and after 4 pm every day.

[0051] Mature tomato samples were picked during the peak fruit-bearing period and tested for fruit quality indicators, including vitamin C content, soluble sugar content, titratable acid content, and sugar-acid ratio.

[0052] The effects of the amino acid-containing water-soluble fertilizers prepared in different embodiments on the quality of tomato fruits are shown in Table 2. The yield and disease rate of the test plots were statistically analyzed during the tomato harvest period. The effects of the amino acid-containing water-soluble fertilizers prepared in different embodiments on the tomato yield and disease rate are shown in Table 3.

[0053] Table 2 Effects of amino acid-containing water-soluble fertilizers on tomato fruit quality in three examples

[0054]

[0055]

[0056] Table 2 shows that the amino acid-containing water-soluble fertilizers prepared by the three embodiments of the present invention, compared with a certain amino acid-containing water-soluble fertilizer currently sold on the market, have an increased vitamin C content of 8.62% to 14.88%, and an increased sugar-acid ratio of 10.86% to 14.33%; compared with the water blank group, the vitamin C content is increased by 21.55% to 28.56%, and the sugar-acid ratio is increased by 21.89% to 25.70%. It shows that the amino acid-containing water-soluble fertilizers prepared by the three embodiments can improve the quality of tomato fruits.

[0057] Table 3 Effects of amino acid-containing water-soluble fertilizers on tomato yield and disease rate

[0058]

[0059] Table 3 shows that the amino acid-containing water-soluble fertilizer prepared by the three embodiments of the present invention has an increase rate of 8.77% to 16.13% and a disease rate reduction of 51.89% to 61.17% compared with a certain amino acid-containing water-soluble fertilizer currently sold on the market; compared with the blank group of clear water, the increase rate is 24.26% to 32.67%, and the disease rate is reduced by 57.83% to 65.96%. It shows that the amino acid-containing water-soluble fertilizer can increase tomato yield and reduce the occurrence of diseases.

[0060] The amino acid-containing water-soluble fertilizer prepared in Example 2 was also selected and diluted 1000 times and then sprayed on the leaves of tomatoes. During the growth process, the stem diameter, plant height, and leaf chlorophyll content were measured in detail for a total of 5 times, each time at an interval of 15 days. The measurement results are shown in Table 4.

[0061] Table 4 Changes in stem diameter, plant height and chlorophyll during tomato growth

[0062] first Second time The third time Fourth Fifth Stem diameter (mm) 40.56 71.96 96.75 113.80 147.77 Plant height(cm) 8.40 13.62 14.61 15.00 14.80 Chlorophyll (SPAD) 36.28 47.04 41.3 40.82 45.52

[0063] The data in Table 4 confirm that the amino acid-containing water-soluble fertilizer of the present invention can promote the growth of tomato plants and thicken the neck of the plants.

[0064] The amino acid-containing water-soluble fertilizer prepared by the present invention uses Chinese medicine residue and rapeseed cake as raw materials. The plant-derived amino acids are easily absorbed by crops. The enzymatic hydrolyzate is filtered and centrifuged by a membrane concentration method, which effectively maintains the biological activity of alkaloids, flavonoids, volatile oils and other substances in the amino acid stock solution. The non-targeted metabolomics detection shows that the amino acid-containing water-soluble fertilizer contains flavonoids, coumarins, phenolic acids, terpenes, amino acids, organic acids and other active substances, among which the content of flavonoids accounts for 13%. The non-targeted total ion chromatogram of the metabolites of the amino acid-containing water-soluble fertilizer is as follows: Figure 1 As shown, since flavonoids have antibacterial, bactericidal and disease-preventing effects, they can effectively reduce the occurrence of crop diseases and insect pests. During the production process of crops, the present invention provides nutrients, promotes root growth, increases crop yields, and improves crop quality.

[0065] Further targeted metabolite detection of flavonoids in amino acid-containing water-soluble fertilizers was performed, and the chromatograms were as follows: Figure 2 The quantitative results are shown in Table 5, where the top 10 substances in terms of flavonoid metabolite concentrations from high to low are kaempferol, rutin, quercetin, astragaloside, isoquercetin, luteolin, quercetin, isorhamnetin, apigenin and catechin.

[0066] Table 5 Quantitative results of targeted detection of flavonoid metabolome

[0067]

[0068]

[0069] The amino acid-containing water-soluble fertilizer prepared by the present invention contains more active substances: flavonoids, coumarins, phenolic acids, terpenes, amino acids and organic acids, among which the content of flavonoids accounts for 13%. The flavonoid active substances can not only promote the growth and development of crops, but also kill insects and prevent diseases. The amino acid-containing water-soluble fertilizer has good application value.

[0070] The contents not described in detail in the present invention are all prior art.

[0071] The above description is only a preferred embodiment of the present invention, and is not limited to the description in the specification and implementation. Therefore, any equivalent changes or modifications made according to the structure, features and principles described in the scope of the present invention should be included in the scope of the present invention.

Claims

1. A method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake, wherein the raw materials are Chinese medicine residue and rapeseed cake, and the method is characterized in that: The Chinese medicine residue contains coptis root, pinellia tuber, tuckahoe, ophiopogon japonicus, artemisia annua, camphor tree root and elsholtzia ciliata, and the specific preparation method comprises the following steps; S1. Crushing and soaking: crush the Chinese medicine residue and tea seed cake, use a 40-60 mesh screen to obtain a powder, soak the powder with distilled water at a material-liquid ratio of 1:7-1:10 at 60-80 ° C for 2-4 hours, and stir every 10-30 minutes during the soaking process; S2. Enzymolysis: Add 2% to 5% of the total enzyme amount of proteolytic enzyme, and enzymolyze in a water bath at 40 to 60 ° C for 4 to 5 hours to obtain an enzymolysis solution, stirring every 10 to 30 minutes during the enzymolysis process; S3. The enzymatic hydrolysate in step S2 is filtered and centrifuged, and the enzymatic hydrolysate is highly concentrated into a plant-derived amino acid stock solution at a volume ratio of 1:7 to 1:10 by a membrane concentration method; S4. Adding animal-derived amino acid stock solution to the plant-derived amino acid stock solution to obtain a mixed amino acid stock solution; S5. Add 5% to 20% of inorganic salts to the mixed amino acid stock solution to obtain an amino acid-containing water-soluble fertilizer, in which the organic matter content is as high as 120g / L, and it contains a variety of active substances, including flavonoids, coumarins, phenolic acids, terpenes, amino acids and organic acids, and the content of flavonoids accounts for 13%.

2. The method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake according to claim 1, characterized in that: The proteolytic enzyme added in the enzymatic hydrolysis process in step S2 is selected from one or a mixture of neutral protease, papain, cellulase, and lipase.

3. The method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake according to claim 1, characterized in that: The enzymolysis solution obtained after enzymolysis in step S2 is heated to 80-100° C. for inactivation treatment. The inactivation time is 10-30 minutes. After inactivation, the enzymolysis solution is filtered and centrifuged.

4. The method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake according to claim 1, characterized in that: The animal-derived amino acids added in step S4 are one or a mixture of fish meal, meat and bone meal, and animal hair.

5. The method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake according to claim 1, characterized in that: The inorganic salt in step S5 includes calcium nitrate, calcium chloride, magnesium chloride, and magnesium sulfate. When adding the inorganic salt, at least two of them are selected.

6. The method for preparing amino acid-containing water-soluble fertilizer by using Chinese medicine residue and rapeseed cake according to claim 1, characterized in that: The free amino acid content in the amino acid water-soluble fertilizer shall not be less than 100g / L, the secondary element content shall not be less than 30g / L, and the water-insoluble matter content shall not be higher than 50g / L.

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