A 24-epibrassinolide soluble concentrate, its preparation method and application

Abstract

This invention provides a 24-epibrassinolide soluble concentrate, its preparation method, and its uses. Through the synergistic effect of nonionic and biosurfactants, the low-durability foaming of the formulation can be reduced, while improving the solubility and storage stability of the active ingredient. The 24-epibrassinolide soluble concentrate of this invention shows significant effects in promoting crop root growth, enhancing photosynthesis, and improving stress resistance, and is suitable for growth regulation of crops such as wheat and cucumber.

Description

Technical Field

[0001] This invention relates to the field of plant growth regulators, specifically to a soluble 24-epibrassinolide, its preparation method, and its application. Background Technology

[0002] Plant growth regulators are a class of chemical substances that influence the growth and development of plants by regulating their endogenous hormone systems. They are characterized by small dosages, rapid effects, and wide application. Currently, there are approximately 40 registered plant growth regulators worldwide, including gibberellins, ethephon, and paclobutrazol, which are widely used for increasing crop yield, enhancing stress resistance, and improving quality. However, the application of plant growth regulators still faces some prominent problems, such as insufficient formulation stability, with some regulators easily decomposing and becoming ineffective during storage or application due to environmental factors such as light and temperature; high risk of phytotoxicity, with excessive or improper use easily causing plant abnormalities; and the potential for pesticide residues to inhibit the growth of subsequent crops.

[0003] 24-epibrassinolide, chemically known as (22R,23R,24R)-2α,3α,22,23-tetrahydroxy-24-methyl-B-homo-7-oxa-5α-cholestan-6-one, has the molecular formula C2. 28 H 48 O6, with a molecular weight of 480.7, appears as a white crystalline powder with a melting point between 256℃ and 258℃. It is soluble in various organic solvents such as methanol, ethanol, tetrahydrofuran, and acetone, but has extremely low solubility in water. 24-Epibrassinolide is a class VI biological hormone that promotes plant growth, enhances crop resistance, improves crop quality, and promotes germination and rooting. 24-Epibrassinolide is suitable for a variety of crops, including but not limited to food crops (such as rice, wheat, and corn) and cash crops (such as fruit trees, vegetables, cotton, soybeans, tea, tobacco, and flowers). Currently, there are 37 registered products in my country, including soluble concentrates, emulsifiable concentrates, powders, and aqueous solutions. Soluble concentrates account for 64.9% (24 products), but they generally suffer from poor formulation stability and incompatible adjuvants, which significantly affect the efficacy of the pesticide. Summary of the Invention

[0004] To address the aforementioned technical problems, this invention provides a 24-epibrassinolide soluble concentrate, its preparation method, and its application.

[0005] The 24-epibrassinolide soluble concentrate of the present invention comprises the following components by weight percentage: 0.01-0.02% 24-epibrassinolide, 6%-10% nonionic surfactant, 3%-8% biosurfactant, 3%-8% ethanol, and deionized water to make up to 100%.

[0006] The nonionic surfactant is a fatty alcohol polyoxyethylene ether, and the biosurfactant is sophorolipid.

[0007] Preferably, the mass ratio of fatty alcohol polyoxyethylene ether to sophorolipid is 4:3.

[0008] Preferably, the 24-epibrassinolide soluble concentrate of the present invention comprises the following components by mass percentage: 0.01% 24-epibrassinolide, 8% fatty alcohol polyoxyethylene ether, 6% sophorolipid, 5% ethanol, and deionized water to make up to 100%.

[0009] The method for preparing the 24-epibrassinolide soluble concentrate of the present invention includes the following steps:

[0010] (1) Add ethanol and 24-epibrassinolide to the preparation vessel, turn on the stirring to dissolve and mix, and take samples for observation during the process until 24-epibrassinolide is completely dissolved and the solution is clear and transparent;

[0011] (2) Add nonionic surfactant and biosurfactant, and stir to mix evenly;

[0012] (3) Add deionized water and stir to mix evenly;

[0013] (4) After passing the test, filter, settle, and repackage; if the test fails, make adjustments until the test is passed before performing the filtering, settling, and repackaging steps.

[0014] Preferably, a heating device is used in step (1) to promote the dissolution of active ingredients; in step (2), the surfactant is heated to above 50°C to improve fluidity, reduce viscosity, and facilitate feeding and mixing.

[0015] Preferably, in steps (1) to (3), the stirring is carried out for at least 20-40 minutes.

[0016] Preferably, the settling time in step (4) is at least 10-16 hours.

[0017] The 24-epibrassinolide soluble concentrate of the present invention can be used in vegetables and grain crops such as cucumbers and wheat, and can promote crop root growth, improve photosynthesis and crop stress resistance.

[0018] By adopting the above technical solution, the present invention has the following beneficial effects:

[0019] (1) The 24-epibrassinolide soluble agent of the present invention can reduce persistent foaming and improve the solubility and storage stability of active ingredients through the synergistic effect of nonionic surfactants and biosurfactants.

[0020] (2) 24-Epibrassinolide has poor solubility. In the process of dissolving the active ingredient, the present invention can use a heating device to promote dissolution and use ethanol as a co-solvent to significantly reduce the content of water-insoluble matter to ≤0.5%. In the process of adding surfactant, it can be heated to above 50°C to improve fluidity and reduce viscosity, so as to better feed and mix.

[0021] (3) The 24-epibrassinolide soluble concentrate of the present invention has high dilution stability. After dilution by 20 times, the diluted solution is uniform and there are no precipitates. The persistent foaming property is reduced, which reduces the risk of clogging of the application equipment.

[0022] (4) The 24-epibrassinolide soluble concentrate of the present invention has significant effects on promoting crop root growth, improving photosynthesis and stress resistance, and is suitable for growth regulation of crops such as wheat and cucumber. Attached Figure Description

[0023] Figure 1 This is a production process flow diagram for a formulation preparation example. Detailed Implementation

[0024] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0025] I. Formulation Preparation Examples

[0026] Formula composition

[0027]

[0028] Preparation method:

[0029] (1) Add ethanol and 24-epibrassinolide to the preparation vessel, turn on the stirrer, stir for 30 minutes to dissolve and mix, and take samples for observation during the process until 24-epibrassinolide is completely dissolved and the solution is clear and transparent;

[0030] (2) Heat fatty alcohol polyoxyethylene ether JFC and sophorolipid to 65°C. After the viscosity decreases and the fluidity increases, add them to the preparation vessel and stir for 30 minutes to mix evenly.

[0031] (3) Add deionized water and stir for 30 minutes until well mixed;

[0032] (4) After passing the test, filter, settle for 12 hours, and repackage; if the test fails, make adjustments until the test is passed, and then perform the filtration, settling, and repackaging steps.

[0033] Multiple batches of samples from Example 1 were prepared, and quality control indicators were tested:

[0034]

[0035] Comparative Example 1:

[0036] Comparative Example 1 sample was prepared according to the formulation components and preparation method of Example 1, except that sophorolipid was not used and the amount of fatty alcohol polyoxyethylene ether (JFC) was 14%.

[0037] Comparative Example 2:

[0038] Comparative Example 2 was prepared according to the formulation components and preparation method of Example 1, except that fatty alcohol polyoxyethylene ether JFC was not used and the amount of sophorolipid was 14%.

[0039] Prepare multiple batches of comparative examples 1-2 and test the quality control indicators:

[0040]

[0041] Comparative Examples 1 and 2 did not use a combination of fatty alcohol polyoxyethylene ether (JFC) and sophorolipid, resulting in some quality control indicators failing to meet standards. Without being bound by any theoretical constraints, the inventors believe that fatty alcohol polyoxyethylene ether (JFC) and sophorolipid have different solubilizing effects on 24-epibrassinolide. Comparative Example 1 used only fatty alcohol polyoxyethylene ether (JFC), but its solubilizing effect on 24-epibrassinolide was poor. During dilution, JFC molecules could not adequately encapsulate the active ingredient. At lower temperatures, the viscosity of JFC increased, and micelles in the solution contracted, again making it difficult to adequately encapsulate the active ingredient molecules. Therefore, under both conditions, active ingredient crystals precipitated, resulting in these two indicators failing to meet standards. Comparative Example 2 used only sophorolipid, which had a higher solubilizing effect on 24-epibrassinolide. Its dilution stability and cold storage stability were acceptable, but sophorolipid had strong foaming ability, and the foam exhibited good anti-burst and anti-compression properties, resulting in excessive foam in the formulation and failing the persistent foaming performance indicator.

[0042] Comparative Example 3

[0043] Comparative Example 3 sample was prepared according to the formulation components of Example 1, and the preparation method is as follows:

[0044] (1) Add ethanol and 24-epibrassinolide to the preparation vessel, start stirring, and add fatty alcohol polyoxyethylene ether JFC, sophorolipid and deionized water in sequence, and stir for 120 minutes.

[0045] (2) Filter and settle for 12 hours to obtain the finished product.

[0046] Although Comparative Example 3 used the same formulation components as Example 1, the preparation method differed from that of this application in the following ways:

[0047] ① In step (1), after adding ethanol and 24-epibrassinolide to the preparation vessel, the two surfactants and deionized water were added directly without waiting for the 24-epibrassinolide to completely dissolve. At this point, visible particles still remain.

[0048] ② The fatty alcohol polyoxyethylene ether (JFC) and sophorolipid were not heated beforehand.

[0049] The above differences lead to problems with the preparation method of Comparative Example 3: both fatty alcohol polyoxyethylene ether (JFC) and sophorolipid are viscous liquids, and JFC is poorly soluble in ethanol. When added to the preparation vessel, the local viscosity of the mixture is too high, making stirring difficult. Prolonged stirring is required for homogeneous mixing, but visible precipitates still exist. Even after filtration and settling for 12 hours, a small amount of precipitate still forms. Analysis revealed that most of the precipitate is 24-epibrassinolide. Without any theoretical constraints, the inventors believe that the preparation method of Comparative Example 3 fails to ensure complete dissolution of the active ingredient before adding the surfactant. Furthermore, the surfactant is not preheated, resulting in high viscosity and poor flowability. When added to the preparation vessel, it cannot adequately encapsulate the active ingredient molecules, thus failing to achieve the desired solubilizing effect.

[0050] II. Field Trials

[0051] Test location and application time:

[0052] Wheat: At the Xingtai Wheat Experimental Base in Hebei Province (Xingmai 6, clay loam soil), pesticides were applied on March 20 (early jointing stage) and April 25 (heading stage).

[0053] Cucumbers: Shandong Shouguang facility vegetable base (Zhongnongda No. 22, sandy loam soil, multi-span greenhouse), pesticides applied on April 10 (seedling stage), April 25 (initial flowering stage), and May 10 (young fruit stage).

[0054]

[0055] Plot design: length × width = 5m × 4m, area 20㎡, plot spacing 1m protective belt, each treatment 3 replicates, randomized block design; pesticide dosage: wheat 40kg / mu, cucumber 75kg / mu, uniform spraying with backpack sprayer.

[0056] Sampling method:

[0057] Root growth: Root samples were taken from the 0-30cm soil layer 20 days after the last application of pesticide. The total root length and root surface area were measured using a WinRHIZO root analyzer.

[0058] Photosynthesis: Functional leaves (wheat flag leaf, cucumber third true leaf) were collected 15 days after the last application, and chlorophyll content was measured using a SPAD-502 chlorophyll meter.

[0059] Wheat trial results

[0060]

[0061] Cucumber Experiment Results

[0062]

[0063] The experimental data show that the agent of the present invention can significantly promote the root growth of wheat and cucumber and promote photosynthesis.

[0064] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A soluble form of 24-epibrassinolide, characterized in that, The product contains the following components by weight percentage: 0.01% 24-epibrassinolide, 8% fatty alcohol polyoxyethylene ether, 6% sophorolipid, 5% ethanol, and deionized water to bring the total to 100%. The fatty alcohol polyoxyethylene ether is Nanjing Taihua's fatty alcohol polyoxyethylene ether JFC; the sophorolipid is Degussa's sophorolipid.

2. A soluble concentrate of 24-epibrassinolide, characterized in that, The product contains the following components by weight percentage: 0.02% 24-epibrassinolide, 10% fatty alcohol polyoxyethylene ether, 7.5% sophorolipid, 7% ethanol, and deionized water to bring the total to 100%. The fatty alcohol polyoxyethylene ether is Nanjing Taihua's fatty alcohol polyoxyethylene ether JFC; the sophorolipid is Degussa's sophorolipid.

3. A method for preparing a 24-epibrassinolide soluble concentrate according to any one of claims 1-2, characterized in that... Includes the following steps: (1) Add ethanol and 24-epibrassinolide to the preparation vessel, turn on the stirring to dissolve and mix, stir for 20-40 minutes, and take samples for observation during the process until 24-epibrassinolide is completely dissolved and the solution is clear and transparent. (2) Add fatty alcohol polyoxyethylene ether and sophorolipid, and stir to mix evenly; (3) Add deionized water and stir to mix evenly; (4) After passing the test, filter, settle for 10-16 hours, and repackage; if the test fails, make adjustments until the test is passed, and then perform the filtration, settling, and repackaging steps.

4. The method for preparing a 24-epibrassinolide soluble concentrate according to claim 3, characterized in that, In step (1), a heating device is used to accelerate dissolution.

5. A method for preparing a 24-epibrassinolide soluble concentrate according to any one of claims 3-4, characterized in that, In step (2), fatty alcohol polyoxyethylene ether and sophorolipid are heated to above 50°C.

6. The use of the 24-epibrassinolide soluble concentrate according to any one of claims 1-2 for promoting crop root growth and enhancing photosynthesis, characterized in that, The crop in question is either cucumber or wheat.

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