Pesticidal dry powder formulation enriched in azadirachtin up to

Details Pesticidal dry powder formulation enriched in azadirachtin up to Pesticidal dry powder formulation enriched in azadirachtin up to

1996-10-02

1999-01-05

Owens, Amelia

Organic compounds -- part of the class 532-570 series

Organic compounds

Heterocyclic carbon compounds containing a hetero ring...

514450, 504291, C07D32112, A01N 4302

Patent

active

058565264

ABSTRACT:
The invention relates to a preparation of azadirachtin, in a dry solid powder form, having a purity upto 88%; an emulsion concentrate having upto 30% by weight of azadirachtin, and a process for preparing said azadirachtin dry powder from neem seeds/kernels, which comprising: (a) disintegrating the neem seeds/kernels into a powder; (b) subjecting the said powder to continuous extraction using methanol or aqueous methanol or ethanol (rectified spirit) or aqueous ethanol at ambient temperature; (c) concentrating the extract and stirring the concentrate with petroleumether or hexane and phase separating by conventional methods; (d) stirring the denser phase containing major quantity of azadirachtin with a water immiscible organic solvent and water as required depending on the solvent used for extraction and phase separating by conventional methods; (e) concentrating the organic phase and gradually adding the concentrate to petroleumether or hexane under stirring at ambient temperature (f), filtering under suction and drying under vacuum at a temperature in the range of 25.degree.-65.degree. C. to obtain a neem seed/kernel extract as a powder having azadirachtin of 10-19% purity; (g) redissolving the product obtained in step (f) in a solvent and adding the solution to petroleumether or hexane at ambient temperature gradually under stirring yielding a white solid, which after filtration and drying under vacuum at 65.degree. C. resulting in azadirachtin having 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 of hexane/petroleumether and ethylacetate leading to solid azadirachtin powder upto 49% (i) dissolving the azadirachtin having upto 49% purity in methanol, ethanol or acetonitrile and subjecting it to HPLC (C18 column) to produce azadirachtin of purity upto 88% in a solid powder form, and (j) and stirring the product of step (i) with solvents and emulsifiers with or without synergist and UV stabiliser to obtain the emulsifiable concentrate.

REFERENCES:
K.J. Feuerhake, "Effectiveness and Selectivity of Technical Solvents for the Extraction of Neem Seed Components with Insecticidal Activity," Proc. 2nd Int. Neem Conf., Rauischholzhausen, 1983, pp. 103-114.
H.C. Sharma, K. Leuschner, A.V.B. Sankaram, D. Gunasekhar, M. Marthandamurthi, K. Bhaskariah, M. Subramanyam, N. Sultana, "Insect Antifeedants and Growth Inhibitors from Azadirachta Indica and Plumbago Zeylanica," Proc. 2nd Int. Neem Conf., Rauischholzhausen, 1983, pp. 291-320.
J.H. Butterworth and E.D. Morgan, "Isolation of a Substance that Suppresses Feeding in Locusts", Chemical Communications, 1968, pp. 23-24.
Isao Kubo and James A. Klocke, "Azadirachtin, Insect Ecdysis Inhibitor," Agric. Biol. Chem. 46 (7), 1982, pp. 1951-1953.
M. Jacobson, "Neem Research in the U.S. Department of Agriculture: Chemical, Biological and Cultural Aspects," Proc. 1st Int. Neem Conf., Rottach-Egern, 1980, pp. 33-42.
J.H. Butterworth and E.D. Morgan, "Investigation of the Locust Feeding Inhibition of the Seeds of the Neem Tree, Azadirachta Indica," T. Insect Physiol., vol. 17, 1971, pp. 969-977.
R.B. Yamasaki, J.A. Klocke, S.M. Lee, G.A. Stone and M.V. Darlington, "Isolation and Purufication of Azadirachtin from Neem (Azadirachta indica) Seeds Using Flash Chromatography and High-Performance Liquid Chromatography," Journal of Chromatography 356 (1986), pp. 220-226.
D.R. Schroeder and K. Nakanishi, "A Simplified Isolation Procedure for Azadirachtin,", Journal of Natural Products, vol. 50, No. 2, Mar.-Apr. 1987, pp. 241-244.

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