Emulsified concentrates containing vitamin d and uses thereof

Abstract

This invention discloses an emulsified concentrate comprising oil, 20 to 250 mg / L of vitamin D, and 5 to 25% by weight of an emulsifier. The invention also discloses an aqueous emulsion comprising the emulsified concentrate and water or an aqueous solution, a method for preparing the emulsified concentrate, and a method for preparing an aqueous emulsion using the emulsified concentrate. The aqueous composition comprising the emulsified concentrate can be used as a foliar fertilizer, particularly for promoting calcium absorption by plant roots.

Description

Technical Field

[0001] This invention relates to the agricultural field, and in particular to vitamin-containing emulsion concentrates. Background Technology

[0002] Vitamins are essential nutrients for maintaining normal physiological functions in the human body. Vitamins are a class of organic molecules, also known as isovitamins. The World Health Organization lists 13 vitamins: Vitamin A, Vitamin B1, Vitamin C, Vitamin D2, Vitamin D3, Vitamin D4, Vitamin D5, Vitamin D6, Vitamin D2, Vitamin D2, Vitamin D2, Vitamin D3, Vitamin D2, Vitamin D3, Vitamin D4 ...3, Vitamin D4, Vitamin D2, Vitamin D3, Vitamin D4, Vitamin D3, Vitamin D4, Vitamin D3, Vitamin D4, Vitamin D5, Vitamin D6, Vitamin D2, Vitamin D2, Vitamin D3, Vitamin D4, Vitamin D2, Vitamin D3, Vitamin D4, Vitamin D2, Vitamin D3 Vitamins Vitamins , Vitamins C, D, E, and K.

[0003] B vitamins and vitamin C are water-soluble vitamins, while the remaining vitamins are fat-soluble vitamins. For many years, it has been known that some vitamins can also be used in agriculture to improve crop growth and promote crop development.

[0004] Agricultural products applied to crops are preferably in aqueous solution form because this form is easier for farmers to handle and can be further diluted with water. For fat-soluble vitamins, a practical solution is to use additives to prepare them as oil-in-water emulsions.

[0005] Agricultural product manufacturers always need to provide products that are easier to use and more stable.

[0006] CN115887379A (Li, 2023) discloses a water-in-oil emulsion containing vitamin D. A mixture containing vitamin D, polysorbate 80, peppermint oil, medium-chain triglycerides, and other components is mixed with water under high-speed shear conditions to obtain a water-in-oil emulsion.

[0007] US20150045333A1 (Hayes, 2015) discloses a compound containing cholecalciferol (a vitamin C). A composition of gum arabic, rice bran oil, and water. Cholecalciferol is dissolved in rice bran oil, and then the mixture is combined with other components, including gum arabic and water, in an online homogenizer to obtain an emulsion.

[0008] US20020001601A1 (Dillon, 2002) discloses an oil-in-oil emulsion containing vitamins in the presence of emulsifiers such as stearic acid and stearates. The gel.

[0009] WO0224165A1 (Schlyter, 2002) discloses an emulsion containing cholecalciferol. An oil phase containing cholecalciferol, lecithin, and medium-chain triglycerides is prepared and mixed with water in two high-intensity mixers to obtain an emulsion.

[0010] TWI805999 (Liu, 2023) discloses an oil-in-water emulsion containing fat-soluble vitamins. The fat-soluble vitamins are dissolved in oil, then mixed with water and a surfactant to obtain the emulsion. Summary of the Invention

[0011] It has been found that applying a vitamin D-containing composition to the leaves of plants can enhance the absorption of calcium by the plant roots and promote plant growth.

[0012] In a first aspect, the present invention provides an emulsion concentrate comprising oil, 20 to 250 mg / L of vitamin D, and 5 to 25% by weight of emulsifier.

[0013] In another aspect, the present invention provides a method for preparing the above-mentioned emulsion concentrate, comprising the following steps: a) Provide oils, especially mineral or vegetable oils; b) Add vitamin D to the oil provided in step a) such that the vitamin D content in the emulsion concentrate obtained by this method is 20 to 250 mg / L; and c) Add an emulsifier to the oil provided in step a) such that the emulsified concentrate obtained by this method contains 5 to 25% by weight of the emulsifier. Detailed Implementation

[0014] Unless otherwise defined, all technical and scientific terms used in this invention have the meanings commonly understood by one of ordinary skill in the art to which this invention pertains. For further clarification, terminology definitions are included herein to better understand the teachings of this invention.

[0015] All references cited in this specification are incorporated herein by reference in their entirety.

[0016] The following terms used in this article have the following meanings: Unless the context clearly indicates otherwise, the terms “an,” “a,” and “the / described” as used herein include both singular and plural references. For example, “an ingredient” refers to one or more ingredients.

[0017] As used herein, "about" refers to a measurable value, such as a parameter, content, or duration of time. Its meaning includes deviations of ±20% or less relative to a specified value, particularly ±10% or less, even more particularly ±5% or less, even more particularly ±1% or less, and most particularly ±0.1% or less, provided such deviations are suitable for carrying out the invention. However, it should be understood that the numerical values ​​modified by the modifier "about" are themselves already explicitly disclosed.

[0018] As used herein, “comprising,” “including,” “containing,” and their various variations are inclusive or open-ended terms that indicate the presence of the elements (e.g., components) described below, but do not exclude the presence of other unlisted components, features, elements, components, or steps known in the art or disclosed herein.

[0019] The range of values ​​represented by endpoints includes all values ​​and fractions within that range, as well as the listed endpoints.

[0020] Unless otherwise defined, “percentage by weight,” “%wt” or “% by weight” as used throughout this specification refers to the relative weight of each component based on the total weight of the formulation.

[0021] The emulsion concentrate used in this article refers to an oil-based composition that spontaneously forms a stable emulsion when diluted with water. When the emulsion concentrate is added to water or an aqueous solution, an emulsion can be obtained without the use of mixing equipment such as a high-intensity mixer. The emulsion concentrate exhibits thermodynamic stability, which means it has excellent storage stability and shelf life. The emulsion concentrate is a homogeneous, single-phase liquid formulation containing a lipophilic active ingredient (vitamin D in this article) dissolved in a water-immiscible solvent.

[0022] Other methods exist for preparing oil-soluble compounds in water emulsions: for example, an oil solution of the compound can be mixed with an aqueous solution containing an emulsifier to form an oil-in-water emulsion, which can then be further diluted to the desired concentration in a storage tank. Alternatively, the oil, compound, and emulsifier can be added to a water tank and mixed to form an emulsion. This method typically requires vigorous stirring to obtain a stable and well-dispersed emulsion.

[0023] One advantage of emulsion concentrate is that it contains all the ingredients needed to prepare an emulsion as a single product, lacking only the water required for the main dilution tank. Therefore, it is a very practical and easy-to-use solution for farmers.

[0024] Emulsions, including those formed from emulsion concentrates and water, may contain emulsion droplets with an average particle size of 0.1 to 1.0 micrometers.

[0025] Vitamin D is a general term for a class of molecules, including (Can be referred to alone or in any combination as "Vitamin D" or "Vitamin D complex"). Vitamins It is a mixture of ergocalciferol (CAS No.: 50-14-6) and zeasterol (CAS No.: 474-69-1) (molar ratio = 1:1). Vitamin It is an ergocalciferol molecule. Vitamin It is a cholecalciferol molecule (CAS No.: 67-97-0). Vitamin It is the molecule of 22-dihydroergocalciferol (CAS No.: 511-28-4). Vitamin It is glutarate ol (CAS No.: 71761-06-3).

[0026] In a first aspect, the present invention provides an emulsion concentrate comprising oil, 20 to 250 mg / L of vitamin D, and 5 to 25% by weight of emulsifier.

[0027] In some embodiments, the present invention provides an emulsion concentrate comprising oil, 20 to 250 mg / L of vitamin D, and 5.0 to 25% by weight of emulsifier.

[0028] The emulsified concentrate contains oil as both vitamin D and an emulsifier solvent.

[0029] Vitamin D has beneficial effects on crops. In particular, studies have shown that foliar application of an aqueous solution containing vitamin D can improve the root system's ability to absorb calcium. Previously, due to the distance between leaves and roots, it was believed that foliar application of vitamin D had no effect on nutrient absorption.

[0030] Compared to plants that receive the same amount of nutrients but are not given vitamin D, applying vitamin D can also promote plant growth, such as increasing the weight of leaves and / or tubers.

[0031] Emulsifiers are soluble in oil. When the emulsion concentrate is mixed with water, the emulsifier forms droplets that encapsulate the oil and vitamin D, and these droplets are suspended in the aqueous solution.

[0032] Studies have found that emulsion concentrates with vitamin D concentrations ranging from 20 to 250 mg / L can be prepared. Vitamin D (such as vitamin D...) Vitamin D is toxic at high concentrations, therefore the concentration of vitamin D in the emulsion concentrate is preferably no more than 250 mg / L to reduce the toxicity risk to operators when they come into contact with the concentrate and emulsions containing the concentrate.

[0033] In some implementations, the concentration of vitamin D in the emulsion concentrate is 30 to 70 mg / L.

[0034] In some implementations, the emulsion concentrate contains 75 to 95% by weight of oil.

[0035] In some embodiments, the oil contained in the emulsion concentrate is a vegetable oil, processed vegetable oil, or mineral oil. Studies have found that a variety of oils can be used to prepare the emulsion concentrate of this invention. Vegetable oils are preferred due to their biodegradability and low environmental footprint. Suitable examples of vegetable oils include sunflower oil and rapeseed oil.

[0036] Processed vegetable oils are products obtained by chemically processing vegetable oils, which may include one or more steps. Suitable examples of processed vegetable oils include methylated seed oils.

[0037] In some implementations, the vitamin D contained in the emulsion concentrate includes cholecalciferol. Studies have found that foliar application of vitamin D containing cholecalciferol (also known as vitamin D...) An aqueous solution of [a substance] can enhance the plant's ability to absorb calcium.

[0038] In some implementations, the emulsifier contained in the emulsion concentrate is a nonionic emulsifier. Studies have found that a variety of emulsifiers (especially nonionic emulsifiers) can be used to prepare vitamin D emulsion concentrates. Emulsion concentrates containing emulsifiers and vitamin D can be easily mixed with water or aqueous solutions and form stable emulsions without the need for mixing equipment.

[0039] In some embodiments, the emulsifier contained in the emulsion concentrate is selected from castor oil ethoxylates, polyethoxylated esters, and mixtures thereof. Studies have found that using castor oil ethoxylates and / or polyethoxylated esters as emulsifiers can form a very stable emulsion when the emulsion concentrate is added to water.

[0040] In some embodiments, the emulsifier is ethoxylated castor oil oleate, CAS number 220037-02-5.

[0041] In some implementations, the emulsifier contained in the emulsion concentrate is a nonionic polymer with a hydrophilic-lipophilic balance of 4 to 10. For emulsion concentrates containing vitamin D in oil, nonionic polymers with a hydrophilic-lipophilic balance of 4 to 10 have been found to be particularly suitable and provide a stable emulsion when mixed with water.

[0042] In some embodiments, the emulsifier is an anionic surfactant.

[0043] In some embodiments, the emulsion concentrate comprises a first emulsifier as an anionic surfactant and a second emulsifier as a nonionic surfactant.

[0044] In some embodiments, the emulsion concentrate comprises a first emulsifier as an anionic surfactant and a second emulsifier selected from castor oil ethoxylates, polyethoxylated esters, and mixtures thereof.

[0045] In some implementations, the emulsion concentrate contains 10 to 25% by weight of emulsifier.

[0046] In some embodiments, the emulsion concentrate contains 0 to 1.0% by weight, 0 to 0.5% by weight, 0 to 0.1% by weight, or 0 to 0.01% by weight of water. Preferably, the emulsion concentrate is anhydrous or has the lowest possible water content. The commercially available forms of the components in the emulsion concentrate may contain small amounts of water.

[0047] In some embodiments, the emulsified concentrate contains antioxidants, particularly tocopherol. Vitamin D is known to be easily oxidized, therefore the inclusion of antioxidants in the emulsified concentrate helps extend its shelf life. Some commercially available vitamin D oil solutions contain tocopherol (also known as vitamin E) as an antioxidant.

[0048] On the other hand, the present invention provides an aqueous emulsion comprising the emulsion concentrate described herein and water. The aforementioned emulsion concentrate is not used directly for field crop spraying, but is added to water or an aqueous solution, such as an aqueous solution containing agricultural products like fertilizers, pesticides, herbicides, and biostimulants. An advantage of the emulsion concentrate of the present invention is that, after adding the emulsion concentrate, only slight stirring of the solution is required to obtain a homogeneous composition (i.e., the emulsion is uniformly distributed in the solution).

[0049] In some embodiments, the aqueous emulsion contains 0.1 to 1.0% by weight of the emulsion concentrate described in this invention. The content of the emulsion concentrate in the aqueous emulsion depends on a variety of factors, such as the concentration of vitamin D in the emulsion concentrate, the crop to which the aqueous emulsion is applied, the field area, and the composition of the aqueous emulsion (which may contain other ingredients besides the emulsion concentrate, such as fertilizers or crop protection products).

[0050] In some implementations, the emulsified concentrate contains 70 to 90% by weight of vegetable oil and 20 to 250 mg / L of vitamins. And 5 to 25% by weight of emulsifier.

[0051] In some implementations, the emulsified concentrate contains 70 to 90% by weight rapeseed oil and 20 to 250 mg / L of vitamins. And 5 to 25% by weight of emulsifier.

[0052] In some implementations, the emulsified concentrate contains 70 to 90% by weight sunflower seed oil and 20 to 250 mg / L of vitamins. And 5 to 25% by weight of emulsifier.

[0053] In some implementations, the emulsified concentrate contains 70 to 90% by weight of vegetable oil and 20 to 250 mg / L of vitamins. And 5.0 to 25% by weight of emulsifier.

[0054] In some implementations, the emulsified concentrate contains 70 to 90% by weight rapeseed oil and 20 to 250 mg / L of vitamins. And 5.0 to 25% by weight of emulsifier.

[0055] In some implementations, the emulsified concentrate contains 70 to 90% by weight sunflower seed oil and 20 to 250 mg / L of vitamins. And 5.0 to 25% by weight of emulsifier.

[0056] In another aspect, the present invention provides a method for preparing the emulsion concentrate of the present invention, comprising the following steps: a) Provide oils, especially mineral oils, processed vegetable oils, or vegetable oils; b) Add vitamin D to the oil provided in step a) such that the vitamin D content in the emulsion concentrate obtained by this method is 30 to 70 mg / L; and c) Add an emulsifier to the oil provided in step a) such that the emulsified concentrate obtained by this method contains 10 to 30% by weight of the emulsifier.

[0057] Emulsion concentrates are prepared by mixing their components in a solvent oil.

[0058] In another aspect, the present invention provides a method for applying the emulsified concentrate of the present invention to the field, comprising the following steps: a) Provide an aqueous solution; b) Adding the emulsified concentrate of the present invention to the aqueous solution; and c) Apply an aqueous solution containing the emulsion concentrate to the field.

[0059] The aqueous solution receiving the emulsion concentrate may contain other useful agrochemicals, such as fertilizers, biostimulants, herbicides, pesticides, or fungicides. It may be more advantageous to add the emulsion concentrate as the final component to the aqueous solution, allowing the other components to dissolve without excessive stirring.

[0060] The aqueous solution containing the emulsion concentrate can be gently stirred to homogenize it. The amount of emulsion concentrate added to the aqueous solution may be low, for example, 0.1 to 1.0% by weight, and therefore, due to the inherent viscosity of the aqueous solution, a homogeneous emulsion may not form immediately after the addition of the emulsion concentrate. Gentle stirring may be necessary to ensure that the emulsion is dispersed throughout the aqueous solution. Emulsification of the oil and aqueous phases can occur without stirring.

[0061] Once the aqueous solution containing the emulsion concentrate is prepared, it can be applied to the field using standard methods known to those skilled in the art.

[0062] In another aspect, the present invention provides the use of an aqueous composition comprising the emulsified concentrate described herein as a foliar fertilizer.

[0063] In another aspect, the present invention provides the use of an aqueous composition comprising the emulsified concentrate described herein as a foliar fertilizer for improving the ability of plant roots to absorb calcium.

[0064] Example 1 An emulsified concentrate was prepared, comprising 80% by weight rapeseed oil and 20% by weight ethoxylated castor oil oleate (CAS No.: 220037-02-5). Vitamins were added to the concentrate. The concentration was increased to 50 mg / L. This emulsion concentrate was then added to water (0.5% by volume) to form a stable emulsion.

[0065] Example 2 An emulsified concentrate was prepared, comprising 80% by weight sunflower seed oil and 20% by weight ethoxylated castor oil oleate (CAS No.: 220037-02-5). Vitamins were added to the concentrate. The concentration was increased to 50 mg / L. This emulsion concentrate was then added to water (0.5% by volume) to form a stable emulsion.

[0066] Example 3 An emulsion concentrate was prepared, comprising 85% by weight rapeseed oil and 15% by weight polyethoxylated ester. Vitamins were added to the concentrate. The concentration was increased to 50 mg / L. This emulsion concentrate was then added to water (0.5% by volume) to form a stable emulsion.

[0067] Example 4 An emulsified concentrate was prepared, comprising 85% by weight rapeseed oil and 15% by weight ethoxylated castor oil oleate (CAS No.: 220037-02-5). Vitamins were added to the concentrate. The concentration was increased to 50 mg / L. This emulsion concentrate was then added to water (0.5% by volume) to form a stable emulsion.

[0068] Example 5 Radish seeds were germinated in pots filled with quartz sand, then thinned to 6 plants per pot and allowed to continue growing under greenhouse conditions until harvest. Seedlings were treated with a Hoagland solution containing all essential nutrients, including calcium. When the plants reached the stage of having 4-5 fully expanded leaves, they were foliar sprayed with the solution prepared in Example 1, or with water as a control. The application rates in Table 1 (liters / hectare) refer to the application rate of the emulsion concentrate, which was applied as a water-in-oil emulsion. During foliar spraying, the soil was completely covered with cotton wool to prevent direct root absorption. Plants were harvested 20 days after foliar spraying. The plants were separated into old leaves, new leaves, and tubers and dried in a drying oven for 5 days. Afterward, their dry weight was recorded, and their tissue nutrient concentrations were analyzed. The results for tuber calcium concentration are shown in Table 1 below.

[0069] As shown in Table 1, compared with the control group, the administration of vitamins The calcium concentration in the plant tubers was significantly increased.

[0070] Example 6 The experiment described in Example 5 was repeated using the emulsion prepared in Example 4, but at different application rates (in liters / ha of emulsion concentrate). After harvest, the tubers and leaves in each pot were weighed. The results are shown in Table 2 below.

[0071] As shown in Table 2, when radishes obtain 100% of the recommended calcium nutrition, the application of vitamins... It can increase the weight of tubers and leaves.

[0072] Example 7 An emulsion concentrate was prepared, comprising: 84.8% by weight rapeseed oil, 15% by weight ethoxylated castor oil oleate (CAS No.: 220037-02-5), and 0.2% by weight a product containing 25 mg / g vitamin C. An α-tocopherol (vitamin E) solution. Based on the total weight of the emulsion concentrate, the vitamin E content in this emulsion concentrate is... The concentration was 50 mg / kg. When this emulsion concentrate was added to water (0.5% by volume), a stable emulsion was formed without any mechanical stirring.

[0073] Example 8 An emulsion concentrate was prepared, comprising: 84% by weight rapeseed oil, 15% by weight ethoxylated castor oil oleate (CAS No.: 220037-02-5), and 1% by weight a product containing 25 mg / g vitamin C. An α-tocopherol (vitamin E) solution. Based on the total weight of the emulsion concentrate, the vitamin E content in this emulsion concentrate is... The concentration was 250 mg / kg. When this emulsion concentrate was added to water (0.5% by volume), a stable emulsion was formed without any mechanical stirring.

[0074] Example 9 The experiments described in Example 5 were repeated using the emulsions prepared in Examples 7 and 8, but with different application rates (in liters / ha of emulsion concentrate). After harvest, the tubers and leaves in each pot were weighed. The results are shown in Table 3 below.

[0075] As shown in Table 3, emulsions prepared using a higher concentration (250 mg / kg) of emulsion concentrate can also produce beneficial agronomic effects. Emulsion concentrates with higher vitamin D concentrations can reduce the amount of water required for field application.

Claims

1. An emulsion concentrate, characterized in that, It contains oil, 20 to 250 mg / L of vitamin D, 5 to 25% by weight of emulsifier, and 0 to 1.0% by weight of water.

2. The emulsion concentrate according to claim 1, characterized in that, The emulsion concentrate contains 75 to 95% by weight of oil.

3. The emulsion concentrate according to claim 1 or 2, characterized in that, The oil mentioned is vegetable oil, processed vegetable oil, or mineral oil.

4. The emulsion concentrate according to any one of claims 1 to 3, characterized in that, The vitamin D mentioned is cholecalciferol.

5. The emulsion concentrate according to any one of claims 1 to 4, characterized in that, The emulsifier is a nonionic emulsifier, an anionic emulsifier, or a mixture of a nonionic emulsifier and an anionic emulsifier.

6. The emulsion concentrate according to claim 5, characterized in that, The nonionic emulsifier is a nonionic polymer with a hydrophilic-lipophilic balance value of 4 to 10.

7. The emulsion concentrate according to any one of claims 1 to 6, characterized in that, The emulsifier is selected from castor oil ethoxylates, polyethoxylated esters, and mixtures thereof.

8. The emulsion concentrate according to any one of claims 1 to 7, characterized in that, The emulsion concentrate contains antioxidants, and in particular, the antioxidant is tocopherol.

9. The emulsion concentrate according to any one of claims 1 to 8, characterized in that, The concentration of vitamin D in the emulsion concentrate is 30 to 70 mg / L.

10. An aqueous emulsion, characterized in that, It comprises the emulsion concentrate according to any one of claims 1 to 9 and water.

11. The aqueous emulsion according to claim 10, characterized in that, The aqueous emulsion comprises 0.1 to 1.0% by weight of the emulsion concentrate according to any one of claims 1 to 9.

12. A method for preparing an emulsion concentrate, characterized in that, Includes the following steps: a) Provide oil; b) Add vitamin D to the oil provided in step a) such that the vitamin D content in the emulsion concentrate obtained by the method is 20 to 250 mg / L; and c) Add an emulsifier to the oil provided in step a) such that the emulsified concentrate obtained by the method contains 5 to 25% by weight of the emulsifier.

13. A method for preparing an aqueous emulsion, characterized in that, include: Provide an emulsion concentrate according to any one of claims 1 to 9; as well as The emulsified concentrate is added to water or an aqueous solution to prepare the aqueous emulsion.

14. Use of an aqueous composition comprising the emulsified concentrate of any one of claims 1 to 9 as a foliar fertilizer.

15. The use of an aqueous composition comprising the emulsified concentrate of any one of claims 1 to 9 as a foliar fertilizer for improving the ability of plant roots to absorb calcium.

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