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Process for efficiently purifying azadirachtin technical

A kind of technology of azadirachtin, which is applied in the direction of insecticide, animal repellent, botanical equipment and method, etc., can solve the problems of low content of azadirachtin, unfavorable storage, low content of extract, etc., and achieve the extraction rate High, avoid loss, simple process effect

Inactive Publication Date: 2017-12-29
YUNNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to literature reports, the content of azadirachtin in neem seeds is very low, generally 0.2% to 0.4%, high up to 0.6%, and the oil content is 30% to 40%, usually using hydrocarbon solvents or by pressing The method removes most of the neem oil such as CN1362020A, CN1184222C, CN1524858A, CN101440099A, CN1423939A, CN101029276, and then extracts the neem cake from which the neem oil is removed with an organic solvent, and then obtains an extract containing azadirachtin through liquid-liquid extraction , but the process of deoiling first and then extracting also loses part of azadirachtin in the process of deoiling, so that the content in the final extract is basically low and contains large polar molecular compounds, such as proteins, sugars, etc., which have poor stability and are not good for storage
In view of the current domestic extraction and purification process of azadirachtin is relatively backward, and the content is generally lower than 15%, it is urgent to research and develop a method for efficient and rapid extraction and purification to prepare high-content azadirachtin original drug

Method used

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  • Process for efficiently purifying azadirachtin technical
  • Process for efficiently purifying azadirachtin technical
  • Process for efficiently purifying azadirachtin technical

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Grind the dried azadirachtin seed kernels with shells with a pulverizer, remove most of the shells with a 20-mesh sieve, take 700 g of powder, add 2 L of methanol, and stir mechanically for 3 hours at room temperature. Then stand still for 1 hour until the precipitation is complete, then filter and separate, and extract the filter residue with methanol for 1 to 2 times, collect the extract and concentrate in vacuum below 50°C to obtain neem concentrate.

[0034] Add an equal amount of ethyl acetate and 500 mL of saturated saline to the concentrate obtained in the previous step, mix and stir evenly, and then let stand for about 1 hour until ester-water is completely separated. The ethyl acetate layer was washed with saturated brine to remove organic acids, water-soluble proteins, polysaccharides, etc., and the aqueous layer was extracted once with ethyl acetate to increase the extraction rate of azadirachtin, and the ethyl acetate layer was collected and dried with anhydr...

Embodiment 2

[0037] Grind the dried azadirachtin seed kernels with shells with a pulverizer, remove most of the shells with a 20-mesh sieve, take 700 g of powder, add 2 L of methanol, and stir mechanically for 3 hours at room temperature. Then stand still for 1 hour until the precipitation is complete, then filter and separate, and extract the filter residue with methanol for 1 to 2 times, collect the extract and concentrate in vacuum below 50°C to obtain neem concentrate.

[0038] Add an equal amount of ethyl acetate and 500 mL of saturated saline to the concentrate obtained in the previous step, mix and stir evenly, and then let stand for about 1 hour until ester-water is completely separated. The ethyl acetate layer was washed with saturated brine to remove organic acids, water-soluble proteins, polysaccharides, etc., and the aqueous layer was extracted once with ethyl acetate to increase the extraction rate of azadirachtin, and the ethyl acetate layer was collected and dried with anhydr...

Embodiment 3

[0041] Grind the dried azadirachtin seed kernels with shells with a pulverizer, remove most of the shells with a 20-mesh sieve, take 700 g of powder, add 2 L of methanol, and stir mechanically for 3 hours at room temperature. Then stand still for 1 hour until the precipitation is complete, then filter and separate, and extract the filter residue with methanol for 1 to 2 times, collect the extract and concentrate in vacuum below 50°C to obtain neem concentrate.

[0042]Add an equal amount of ethyl acetate and 500 mL of saturated saline to the concentrate obtained in the previous step, mix and stir evenly, and then let stand for about 1 hour until ester-water is completely separated. The ethyl acetate layer was washed with saturated brine to remove organic acids, water-soluble proteins, polysaccharides, etc., and the aqueous layer was extracted once with ethyl acetate to increase the extraction rate of azadirachtin, and the ethyl acetate layer was collected and dried with anhydro...

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Abstract

The invention discloses a process for efficiently purifying azadirachtin technical and belongs to the field of purifying preparation of natural plant extract. The process comprises the following steps: 1) shelled neem seeds are smashed, seed shells are removed, and seed powder is obtained; 2) neem extract is prepared; 3) crude azadirachtin powder is prepared; 4) rapid gradient elution is performed on the crude azadirachtin powder with flash chromatography, azadirachtin-containing eluates are mixed and concentrated under reduced pressure, and faint yellow and white azadirachtin technical powder with high content is obtained. The schematic diagram of the process for efficiently purifying the azadirachtin technical is shown as attached drawing 2. The process for efficiently purifying the azadirachtin technical is simple, the extraction rate is high, the content is high, the cost can be reduced, a good processing scheme is provided for rapidly obtaining high-content azadirachtin in industry, and firm technical basis is laid for current development of neem as a biopesticide.

Description

technical field [0001] The invention belongs to the field of purification and preparation of natural plant extracts, and in particular relates to a process for efficiently purifying azadirachtin as a raw drug. Background technique [0002] Azadirachtin is the main component of a biopesticide with the characteristics of broad spectrum, high efficiency, low toxicity, no residue, no toxic and side effects to humans and animals, safe to natural enemies of pests, and not easy to produce drug resistance. According to literature reports, the content of azadirachtin in neem seeds is very low, generally 0.2% to 0.4%, high up to 0.6%, and the oil content is 30% to 40%, usually using hydrocarbon solvents or by pressing The method removes most of the neem oil such as CN1362020A, CN1184222C, CN1524858A, CN101440099A, CN1423939A, CN101029276, and then extracts the neem cake from which the neem oil is removed with an organic solvent, and then obtains an extract containing azadirachtin thro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/00A01N43/90A01N61/02A01P7/04
CPCC07D519/00A01N43/90A01N61/02
Inventor 金毅糜金甫任思浩严辉焕罗开秀蒋涵林军
Owner YUNNAN UNIV
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