首页> 外国专利> PESTICIDAL DRY POWDER FORMULATION ENRICHED IN AZADIRACHTIN UPTO 88, AN EMULSIFIABLE CONCENTRATE ENRICHED UPTO 30 OF AZADIRACHTIN AND A PROCESS FOR PREPARING SUCH FORMULATION ANDCONCENTRATE FROM NEEM SEED/KERNEL

PESTICIDAL DRY POWDER FORMULATION ENRICHED IN AZADIRACHTIN UPTO 88, AN EMULSIFIABLE CONCENTRATE ENRICHED UPTO 30 OF AZADIRACHTIN AND A PROCESS FOR PREPARING SUCH FORMULATION ANDCONCENTRATE FROM NEEM SEED/KERNEL

机译:叠氮菊酯含量高达88%的农药干粉配方,叠氮素含量高达30%的可乳化浓缩物,以及从NEEM种子/籽粒中制备这种配方和浓缩物的方法

摘要

The invention relates to a preparation of azadirachtin, in a dry solid powderform,having a purity upto 88% ; an emulsion concentrate having upto 30% by weightofazadirachtin, and a process for preparing said azadirachtin dry powder fromneemseeds/kernels, which comprising: (a) disintegrating the neem seeds/kernelsinto apowder; (b) subjecting the said powder to continuous extraction using methanoloraqueous methanol or ethanol (rectified spirit) or aqueous ethanol at ambienttemperature; (c) concentrating the extract and stirring the concentrate withpetroleumether or hexane and phase separating by conventional methods; (d)stirring the denser phase containing major quantity of azadirachtin with awaterimmiscible organic solvent and water as required depending on the solvent usedfor extraction and phase separating by conventional methods; (e) concentratingtheorganic phase and gradually adding the concentrate to petroleumether or hexaneunder stirring at ambient temperature (f), filtering under suction and dryingundervacuum at a temperature in the range of 25 - 65°C. to obtain a neemseed/kernelextract as a powder having azadirachtin of 10-19% purity; (g) re~dissolvingtheproduct obtained in step (f) in a solvent and adding the solution topetroleumetheror hexane at ambient temperature gradually under stirring yielding a whitesolid,which after filtration and drying under vacuum at 65°C. resulting inazadirachtinhaving 15-26% purity as a white powder (h), dissolving the azadirachtin (10-19%)from step (e) in an organic solvent and subjecting to column chromatography(silicagel) by stepwise elution using different compositions ofhexane/petroleumether and ethylacetate leading to solid azadirachtin powderupto49% (i) dissolving the azadirachtin having upto 49% purity in methanol,ethanol oracetonitrile and subjecting it to HPLC (C18 column) to produce azadirachtin ofpurity upto 88% in a solid powder form, and (j) and stirring the product ofstep(i) with solvents and emulsifiers with or without synergist and UV stabilisertoobtain the emulsifiable concentrate.
机译:本发明涉及干燥固体粉末中的印za素的制剂形成,纯度高达88%;乳液浓缩物,含量最高为30%的印za素,以及从其制备所述印za素干粉的方法印em种子/仁,包括:(a)分解印em种子/仁变成一个粉末; (b)使用甲醇对所述粉末进行连续萃取要么室温下的甲醇或乙醇水溶液(精制酒精)或乙醇水溶液温度; (c)浓缩提取物并将浓缩物与石油醚或己烷,通过常规方法进行相分离; (d)将含有大量印za素的致密相与水不混溶的有机溶剂和水,视使用的溶剂而定通过常规方法进行萃取和相分离; (e)专心的有机相,并将浓缩物逐渐添加到石油醚或己烷中在室温(f)搅拌下,抽滤并干燥下在25-65°C的温度范围内抽真空。获得印em种子/内核提取物为印a素含量为10-19%的粉末; (g)重新溶解的步骤(f)中获得的产物在溶剂中并将溶液添加到石油醚或己烷,于室温下在搅拌下逐渐产生白色固体,过滤并在65°C真空干燥后。导致印za素纯度为15-26%的白色粉末(h),可溶解印za素(10-19%)步骤(e)中得自有机溶剂并经柱层析(硅胶)逐步洗脱,使用不同组成的己烷/石油醚和乙酸乙酯制成固体印za素粉末取决于49%(i)将印za素达到最高49%的纯度溶于甲醇中,乙醇或乙腈并进行HPLC(C18色谱柱)制备印a素固体粉末形式的纯度最高可达88%,并且(j)并搅拌以下产物步(i)含有或不含有增效剂和紫外线稳定剂的溶剂和乳化剂至获得乳油。

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