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Industrial large scale extracting method for nimbin dry powder

An extraction method, technology of azadirachtin, applied in botany equipment and methods, animal husbandry, animal repellent, etc., can solve the problems of a large number of solvents and giant equipment, complex components, cumbersome and complicated processes, etc., and achieve the convenience of large-scale The production and equipment requirements are not high, and the effect of high yield and purity

Inactive Publication Date: 2009-05-27
牛赡光 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 1. Water and methanol are used as the liquid phase, in which amino acids, proteins, nucleic acids, polysaccharides, alcohols, aldehydes, alkaloids, organic acids and other organic substances are difficult to separate, which affects the purity
Not only poor stability, complex components pollute the environment, but also difficult to make advanced dosage forms such as powder, dry suspension, tablet, etc.
[0007] 2. Separating the dry powder of azadirachtin by layer washing column, the purity can be improved through repeated elution of normal phase column and reverse phase column, but, due to the constant change of washing solvent, the process is cumbersome and complicated, the separation speed is very slow, and the amount of solvent is large
[0008] 3. A single solvent is used as the extraction phase and the back extraction phase. The amount of solvent is too large, which requires a large amount of solvent and huge equipment. The investment and energy consumption in solvent recovery increase, and the cost rises!
[0009] 4. The high-content samples extracted from azadirachtin are mainly obtained in the laboratory at present, and there are no mature reports on the large-scale operation of real application in production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] A large amount of extraction method of azadirachtin dry powder industry, the steps are:

[0030] 1), the preparation mass percent concentration is 20% ammonium sulfate solution D1, adjust pH value 5.0, add methanol and mix, make mixed solution M1 (separate liquid phase), standby; Wherein, the addition amount of methanol is calculated by volume ratio, D1: Methanol=1:2;

[0031] 2), peel the neem seeds, squeeze the oil from the kernels, crush the deoiled cake to 60 meshes, add M1 whose mass is 5 times that of the cake, stir for 2 hours, press filter to remove the dregs, Add the extract phase M2 which is 3 times the volume of the filtrate to the filtrate, stir for 45 minutes, and let it stand; the M2 is prepared from ethyl acetate and dichloromethane in a volume ratio of 9:1;

[0032] 3) After standing for complete stratification, remove the lower impurity part and leave the upper oil phase solution;

[0033] 4), the collected upper oil phase solution was evaporated and ...

Embodiment 2

[0042] A large amount of extraction method of azadirachtin dry powder industry, the steps are:

[0043] 1), the preparation mass percent concentration is 25% ammonium sulfate solution D1, adjust pH value 5.5, add methanol and mix, make mixed solution M1 (separate liquid phase), standby; Wherein, the addition amount of methanol is calculated by volume ratio, D1: Methanol=1:9;

[0044] 2), peel the neem seeds, squeeze the oil from the kernels, crush the deoiled cake to 40 meshes, add M1 whose mass is 5 times that of the cake, stir for 1.5 hours, press filter to remove the residue, Add 3 times the volume of the filtrate to the extract phase M2, stir for 50 minutes, and let it stand; the M2 is prepared from ethyl acetate and dichloromethane in a volume ratio of 4:1;

[0045] 3) After standing for complete stratification, remove the lower impurity part and leave the upper oil phase solution;

[0046] 4) Concentrate the collected upper oil phase solution by evaporating under reduc...

Embodiment 3

[0053] A large amount of extraction method of azadirachtin dry powder industry, the steps are:

[0054] 1), the preparation mass percent concentration is 1% ammonium sulfate solution D1, adjust pH value 5.3, add methanol and mix, make mixed solution M1 (separate liquid phase), standby; Wherein, the addition amount of methanol is calculated by volume ratio, D1: Methanol=1:7;

[0055] 2), peel the neem seeds, squeeze the oil from the kernels, crush the deoiled cake to 40 meshes, add M1 whose mass is 5 times that of the cake, stir for 1 hour, press filter to remove the dregs, Add 3 times the volume of the filtrate to the extract phase M2, stir for 60 minutes, and let it stand; the M2 is prepared from ethyl acetate and dichloromethane in a volume ratio of 8:1;

[0056] 3) After standing for complete stratification, remove the lower impurity part and leave the upper oil phase solution;

[0057] 4), the collected upper oil phase solution was evaporated and concentrated under reduc...

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PUM

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Abstract

The invention discloses a method for industrially extracting azadirachtin dry powder in great amount, which is used for solving the problem of industrially extracting the azadirachtin dry powder as a raw material of pesticide in great amount. The azadirachtin dry powder comprises a neem methanol crude extract, and is prepared by the following steps: preparing a phase separation solution by an ammonium sulphate solution, and preparing an extraction liquid by ethyl acetate and methylene dichloride; removing clotted oil residual and lower separated liquid phase; collecting oil phase; concentrating by a film evaporator and a condenser; reversely extracting and degreasing by n-hexane and petroleum ether; collecting an organic solvent; centrifugalizing a target product; drying and crushing; and the like. The method saves the solvent; the yield for extracting azadirachtin once reaches 82 percent, and reaches over 96 percent if extraction is repeated once with purity reaching 23 to 26 percent; industrialized production yield and purity are high; the method is simple; furthermore, amino acid, protein, nucleic acid, polysaccharide, alcohols, aldehydes, alkaloid, organic acid and other organic materials can be effectively separated with improved stability. The azadirachtin dry powder can be used as powder, suspension, tablet and other advanced preparation formulations. The method does not have high requirement on equipment, and is convenient for large-scale manufacture.

Description

technical field [0001] The invention relates to a process for extracting azadirachtin used in pesticides, in particular to a method for industrially extracting a large amount of dry powder of azadirachtin. Background technique [0002] Neem (Azadirachta indica A.Juss) is an arbor of the family Meliaceae, widely planted in tropical and subtropical regions. Originated in Myanmar and India, it is distributed and planted in more than 70 countries, with the largest output in Asian countries such as India. Active substances are contained in neem fruit, seeds, seed cores, branches, leaves, bark and sap, but especially in seeds. So far, more than 100 compounds have been found in neem, at least 70 compounds have biological activity, they are diterpenes, triterpenoids, pentatriterpenoids and non-terpenoids. It is mainly azadirachtin, azadirachtriol and azadirachtin, etc. These extracts have the functions of repelling insects, interfering with oviposition, interfering with insect var...

Claims

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Application Information

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IPC IPC(8): C07D519/00A01N43/90A01P7/00
Inventor 牛赡光齐庆俊王清海刘幸红张淑静
Owner 牛赡光
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