Indian Patents. 199867:A process for preparation of composition useful for the insect free storage of cereals.

Title of Invention	A process for preparation of composition useful for the insect free storage of cereals.
Abstract	A process for preparation of composition useful for the insect free storage of cereals comprising, mixing a) substituted phenol in the range of 0.75 to 25% (v/w), b) dried roots powder of D. hamiltonii in the range of 0.25 to 75% (w/w)

Full Text	The present invention relates to a process for preparation of composition useful for the insect free storage of cereals The invention described in this patent can be used to protect stored cereals from insect infestation for a minimum period of four months. The invention provides for the insect free storage of cereals without the use of poisonous insecticides, but a formulation made up of safe food grade materials, so that there is absolutely no risk of poisoning upon consuming the treated grain. Reference may be made to Pereira, J and Wohlgemuth, R 1982 .Neem Azadirahta indica.(AJuss) of West African origin as a protectant of stored maize. Z.ange.Entomol.94, 208-214, wherein the traditional practice of mixing neem leaves with stored grain was investigated. However, the drawback is that this treatment did not prevent the multiplication of the insect pests. Reference may be made to Golob,P and Webley,D.J., (1980) The use of plants and minerals as traditional protectants of stored products, G138, Chatham,UK, Natural Resources Institute wherein another traditional method of mixing sand with stored grain is documented. However, since the sand particles are used to block the intefgranular spaces and act as a physical barrier to the movement of insect pests, large quantities of sand have to be used which is unhygienic and also necessitates sieving off the sand before using the grain. Reference may be made to Madura Rao et.al., Influence of the purity of Tricalcium Phosphate on its toxicity to stored product insects, Life Sciences 10(2)1081-1088,1971, wherein Tricaicium Phosphate (TCP) is advocated as a nontoxic grain protectant. However, the drawbacks are that the TCP used should be 99% pure and the material is expensive. Reference may be made to Frank H.A., Grain protectants:Current status and prospects for the future, J.stored Prod.Res.32(4)293-302 1996, wherein the use of diatomaceous earth based formulations for the protection of stored grain in the USA and Australia is documented. However the drawbacks are that the treatment inhibits the free flow of grain and also damages grain handling equipment. More recently health problems to workers have restricted its use considerably. Reference may be made to Walter Ebling, Use of mineral dusts for protection against insect pests with special reference to cereal grains, in Grain Sanitation, Eds.S.K.Majumder & J.S.Venugopal, Academy of Pest Control Sciences, Mysore, India, 1969, pp.81-96, wherein activated clay is used as a nontoxic grain protectant. However the treatment is not effective on grain with high moisture content or in regions with high Relative Humidity as in coastal areas. Reference may be made to Singal,S.K. and Singh,Z,1990, Studies on plant oils as surface protectant against pulse beetle Callosobruchus chinensis L . in chickpea, Cicer arietinum L.,Tropical Pest Management,36.314-316, wherein the traditional practice of mixing stored grain with vegetable oils is documented. However, the drawbacks are that the oils apart from being expensive also turn rancid and may impart an off-flavour to the grain as shown by Pereira,J and Wholgemuth,R. 1983, The effect of six vegetable oils as protectants of cowpeas and Bambara groundnut against infestation by Callosobruchus maculatus. J.stored Prod.Res. 19,57-62. Reference may be made to a patent application filed in 1998 (1301/Del/98) titled A method for the preparation of an active fraction from the roots of Decalepis hamiltonii, Wight & Arn. useful as a biopesticide , wherein formulations employing extracts of the root of D.hamiltonii are described. However the drawbacks are that these extracts or its formulations exhibited a very poor shelf life and lose the insecticidal activity within 2 weeks. Reference may be made to Jacob George et.al, (1999), Current Science,77(4),501-502, wherein the insecticidal activity of the roots of D.hamiltonii have been described. The powder of air dried roots and the volatile fraction obtained from it exhibited toxicity to adults of the rice weevil, Sitophilus oryzae, lesser grain borer, Rhizopertha dominica and red flour beetle, Tribolium castaneum. However, there is no report on the stabilisation/synergism of the insecticidal activity of the roots or its extracts. The main object of the present invention is to provide a formulation useful for the insect free storage of cereals which obviates the drawbacks as stated above. Another object of the present invention is to provide an insecticide formulation employing roots of D.hamiltonii having an active shelf life of longer period. Yet another object of the present invention is to provide an insecticidal formulation exhibiting enhanced insecticidal and Ovicidal activity. A process for preparation of composition useful for the insect free storage of cereals comprising, mixing a) substituted phenol such as herein described in the range of 0.75 to 25% (v/w), b) dried roots powder of Decalepis hamiltonii in the range of 0.25 to 75% (w/w) In an embodiment of the present invention the substituted phenol used is selected from guaiacol, dimethoxybenzaldehyde and vanillin. In an another embodiment the particle roots is in the range of 50 to 100mesh. In yet another embodiment the shredded cortex of the roots used are dried by freeze drying or at a low temperature of less than 40°C using a mechanical device. The formulation obtained by the process of the present invention is neither a product of chemical reaction nor a mere admixture but is a synergistic formulation having properties different than the aggregate properties of the individual components. The root material is washed thoroughly to remove all a adhering soil, and other debris. The roots are then sorted into mature and young roots based on the colour of the cortex, amount of latex and nature of the pith. In the mature roots the cortex is reddish, less oflatex such that there is no free flowing latex when the root is broken and the pith is fibrous and comparatively thick. The young roots on the other hand have a white cortex with profuse and free flowing latex and tender pith which snaps clean when the root is broken. The sorted root material is chipped manually with a knife or shredded in a mechanical shredder. With the mature roots, care is taken to separate out the fibrous pith before feeding into the shredder. The shredded root material is then dried in a lyophiliscr or at room temperature or in an oven at The dried root material is powdered in a hand pounder or a mechanical pounder or a hammer mill. The powder is sieved to obtain a particle size of 50 to 100 mesh, preferably 60 to 80 mesh. Care is taken during the powdering operation so that the temperature of the powder does not exceed 45°C. The substituted phenol like dimethoxybenzaldehyde or guaiacol or vanillin etc., dissolved in a volatile solvent like diethylether, petroleum ether, chloroform etc is mixed with the powdered root material and the solvent allowed to evaporate with intermittant stirring of the formulated powder. The substituted phenol is mixed with the root powder in the ratio of 0.75 to 25%(W/W) preferably in the ratio of 1.5 to 10% (WAV). For the first time, an edible root has been used to prepare a formulation for the insect free storage of cereals. All the materials used in the formulation are food materials/additives which in effect is that food materials are used to protect stored cereals from insect infestation. The following examples are given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention. EXAMPLE-1 Bioefficacy of the synergistic mixture of D.hamiltonii root powder + guaiacol against the rice weevil, Sitophilus oryzae L.(Coleoptera:curculionidae)on wheat. 500g of the roots of D.hamiltonii was shredded in a mechanical shredder and the uncut fibrous pith portion was manually separated. The shredded cortex of the root was freeze dried and powdered to 50mesh. The root powder was mixed with guaiacol dissolved in diethyl ether and the solvent was allowed to evaporate overnight. Formulations comprising guaiacol mixed with the root powder at 1.5,0.75,0.38 and 0.19% was prepared. Each formulation was mixed with 20g wheat (moisture content 12%) at 5,3,1 and 0.5% in stoppered glass tubes 150x23mm and the grain mixed with the formulated powder by a tumbling action of the tubes for one minute. Twenty adult Sitophilus oryzae (1-2 weeks old) were released into each tube and the tubes covered by muslin held by rubber bands. There were four replicates in each treatment. At weekly intervals the number of insects dead in each replicate was noted and the dead insects discarded. At the end of the third week the dead and live insects were discarded and the tubes incubated for emergence of the progeny (Fl generation). The results of the various parameters recorded are given in tables 1 and 2. Table 1. Mortality of S.oryzae on wheat treated with D.hamiltonii root powder + guaiacol (Table Removed) Conclusions: An increase in the proportion of guaiacol mixed with the powdered root of D.hamiltonii synergised the toxicity of the root powder to the test insect and also increased the speed of insect kill. Table.2. Productivity of S.otyzae on wheat treated with formulations of D.hamiltonii root powder + guaiacol. (Table Removed) (40df) The statistical analysis was made for 20 treatments inclusive of the controls. Conclusions: An increase in the proportion of guaiacol mixed with D.hamiltonii root powder increased the Insecticidal efficacy of the root powder by reducing the fecundity of the test insect. EXAMPLE 2. Bioefficacy of the synergistic formulation of D.hamiltonii root powder mixed with guaiacol aged for four months. 500g of the freeze dried roots of D.hamiltonii and powdered to 50mesh was mixed with guaiacol dissolved in diethyl ether. Formulations comprising guaiacol mixed with root powder at 1.5, 0.75,0.38 and 0.19% were prepared. The formulations were aged for four months by storing them in separate beakers covered by aluminium foils. The formulations were thus not stored in airtight containers. The bioefficacy of the formulated and unformulated (ie.control) root powders was examined after four months storage. Each formulation was mixed with 20g wheat (moisture content 12%) at 5,3,1 and 0.5% in stoppered glass tubes 150x23mm and the grain mixed with the formulated powder by a tumbling action of the tubes for one minute. Twenty adult Sitophilus oryzae (1-2 weeks old) were released into each tube and the tubes covered by muslin held by rubber bands. There were four replicates in each treatment. At weekly intervals the number of insects dead in each replicate was noted and the dead insects discarded. At the end of the third week the dead and live insects were discarded and the tubes incubated for emergence of the progeny (Fl generation). The results of the various parameters recorded are given in tables 3. Table3. Bioefficacy of D.hamiltonii root powder + guaiacol aged for 4 months against S.oryzae on wheat. (Table Removed) Conclusions: The addition of guaiacol to D hamiltonii root powder prolonged the residual toxicity of the root powder beyond 4 months, whereas the powder alone was least toxic to the test insects. The synergistic mixture of D.hamiltonii root powder + guaiacol was active even after 4 months by reducing the productivity of the test insects, whereas the root powder alone was ineffective. The main advantages of the present invention are: 1. An ecofriendly insecticide comprising a mixture of natural plant products for the protection of stored cereals from insect infestation. 2. A safe insecticide comprising a mixture of natural plant foods and/or products. 3. The insecticide formulation described not only exhibits toxicity to the adult insect pests but also exhibits the unique ovicidal activity even to eggs oviposited within the grain, thus enhancing the insecticidal potential of the formulation. 4. The insecticidal formulation described exhibited an active shelf life of more than four months compared to less than two months for the unformulated root powder. 5. The synergised insecticidal formulation described exhibited enhanced insecticidal activity compared to the unsynergised root powder of D.hamiltonii. We Claim: 1. A process for preparation of composition useful for the insect free storage of cereals comprising, mixing a) substituted phenol such as herein described in the range of 0.75 to 25% (v/w), b) dried roots powder of Decalepis hamiltonii in the range of 0.25 to 75% (w/w) 2. A process as claimed in claim 1, wherein the substituted phenol used is selected from guaiacol, dimethoxybenzaldehyde and vanillin. 3. A process as claimed in claims 1&2, wherein the particle size of dried roots is in the range of 50 to 100 mesh. 4. A process for preparation of composition useful for the insect free storage of cereals substantially as herein described with reference to the examples accompanying this specification.

Full Text

The present invention relates to a process for preparation of composition useful for the insect free storage of cereals
The invention described in this patent can be used to protect stored cereals from insect infestation for a minimum period of four months. The invention provides for the insect free storage of cereals without the use of poisonous insecticides, but a formulation made up of safe food grade materials, so that there is absolutely no risk of poisoning upon consuming the treated grain.
Reference may be made to Pereira, J and Wohlgemuth, R 1982 .Neem Azadirahta indica.(AJuss) of West African origin as a protectant of stored maize. Z.ange.Entomol.94, 208-214, wherein the traditional practice of mixing neem leaves with stored grain was investigated. However, the drawback is that this treatment did not prevent the multiplication of the insect pests.
Reference may be made to Golob,P and Webley,D.J., (1980) The use of plants and minerals as traditional protectants of stored products, G138, Chatham,UK, Natural Resources Institute wherein another traditional method of mixing sand with stored grain is documented. However, since the sand particles are used to block the intefgranular spaces and act as a physical barrier to the movement of insect pests, large quantities of sand have to be used which is unhygienic and also necessitates sieving off the sand before using the grain.
Reference may be made to Madura Rao et.al., Influence of the purity of Tricalcium Phosphate on its toxicity to stored product insects, Life Sciences 10(2)1081-1088,1971, wherein Tricaicium Phosphate (TCP) is advocated as a
nontoxic grain protectant. However, the drawbacks are that the TCP used should be 99% pure and the material is expensive.
Reference may be made to Frank H.A., Grain protectants:Current status and prospects for the future, J.stored Prod.Res.32(4)293-302 1996, wherein the use of diatomaceous earth based formulations for the protection of stored grain in the USA and Australia is documented. However the drawbacks are that the treatment inhibits the free flow of grain and also damages grain handling equipment. More recently health problems to workers have restricted its use considerably.
Reference may be made to Walter Ebling, Use of mineral dusts for protection against insect pests with special reference to cereal grains, in Grain Sanitation, Eds.S.K.Majumder & J.S.Venugopal, Academy of Pest Control Sciences, Mysore, India, 1969, pp.81-96, wherein activated clay is used as a nontoxic grain protectant. However the treatment is not effective on grain with high moisture content or in regions with high Relative Humidity as in coastal areas.
Reference may be made to Singal,S.K. and Singh,Z,1990, Studies on plant oils as surface protectant against pulse beetle Callosobruchus chinensis L . in chickpea, Cicer arietinum L.,Tropical Pest Management,36.314-316, wherein the traditional practice of mixing stored grain with vegetable oils is documented. However, the drawbacks are that the oils apart from being expensive also turn rancid and may impart an off-flavour to the grain as shown by Pereira,J and Wholgemuth,R. 1983, The effect of six vegetable oils as protectants of cowpeas and Bambara groundnut against infestation by Callosobruchus maculatus. J.stored Prod.Res. 19,57-62.
Reference may be made to a patent application filed in 1998 (1301/Del/98) titled A method for the preparation of an active fraction from the roots of Decalepis hamiltonii, Wight & Arn. useful as a biopesticide , wherein formulations employing extracts of the root of D.hamiltonii are described. However the drawbacks are that these extracts or its formulations exhibited a very poor shelf life and lose the insecticidal activity within 2 weeks.
Reference may be made to Jacob George et.al, (1999), Current Science,77(4),501-502, wherein the insecticidal activity of the roots of D.hamiltonii have been described. The powder of air dried roots and the volatile fraction obtained from it exhibited toxicity to adults of the rice weevil, Sitophilus oryzae, lesser grain borer, Rhizopertha dominica and red flour beetle, Tribolium castaneum. However, there is no report on the stabilisation/synergism of the insecticidal activity of the roots or its extracts.
The main object of the present invention is to provide a formulation useful for the insect free storage of cereals which obviates the drawbacks as stated above.
Another object of the present invention is to provide an insecticide formulation employing roots of D.hamiltonii having an active shelf life of longer period.
Yet another object of the present invention is to provide an insecticidal formulation exhibiting enhanced insecticidal and Ovicidal activity.
A process for preparation of composition useful for the insect free storage of cereals comprising, mixing
a) substituted phenol such as herein described in the range of 0.75 to 25%
(v/w),
b) dried roots powder of Decalepis hamiltonii in the range of 0.25 to 75%
(w/w)
In an embodiment of the present invention the substituted phenol used is selected from guaiacol, dimethoxybenzaldehyde and vanillin.
In an another embodiment the particle roots is in the range of 50 to 100mesh.
In yet another embodiment the shredded cortex of the roots used are dried by
freeze drying or at a low temperature of less than 40°C using a mechanical
device.
The formulation obtained by the process of the present invention is neither a
product of chemical reaction nor a mere admixture but is a synergistic
formulation having properties different than the aggregate properties of the
individual components.
The root material is washed thoroughly to remove all a adhering soil, and other debris. The roots are then sorted into mature and young roots based on the colour of the cortex, amount of latex and nature of the pith. In the mature roots the cortex is reddish, less oflatex such that there is no free flowing latex when the root is broken and the pith is fibrous and comparatively thick. The young roots on the other hand have a white cortex with profuse and free flowing latex and tender pith which snaps clean when the root is broken.
The sorted root material is chipped manually with a knife or shredded in a mechanical shredder. With the mature roots, care is taken to separate out the fibrous
pith before feeding into the shredder. The shredded root material is then dried in a lyophiliscr or at room temperature or in an oven at The dried root material is powdered in a hand pounder or a mechanical pounder or a hammer mill. The powder is sieved to obtain a particle size of 50 to 100 mesh, preferably 60 to 80 mesh. Care is taken during the powdering operation so that
the temperature of the powder does not exceed 45°C.
The substituted phenol like dimethoxybenzaldehyde or guaiacol or vanillin etc., dissolved in a volatile solvent like diethylether, petroleum ether, chloroform etc is mixed with the powdered root material and the solvent allowed to evaporate with intermittant stirring of the formulated powder. The substituted phenol is mixed with the root powder in the ratio of 0.75 to 25%(W/W) preferably in the ratio of 1.5 to 10% (WAV).
For the first time, an edible root has been used to prepare a formulation for the insect free storage of cereals. All the materials used in the formulation are food materials/additives which in effect is that food materials are used to protect stored cereals from insect infestation.
The following examples are given by way of illustration of the present invention and therefore should not be construed to limit the scope of the present invention.
EXAMPLE-1
Bioefficacy of the synergistic mixture of D.hamiltonii root powder + guaiacol against the rice weevil, Sitophilus oryzae L.(Coleoptera:curculionidae)on wheat.
500g of the roots of D.hamiltonii was shredded in a mechanical shredder and the uncut fibrous pith portion was manually separated. The shredded cortex of the root was freeze dried and powdered to 50mesh. The root powder was mixed with guaiacol dissolved in diethyl ether and the solvent was allowed to evaporate overnight. Formulations comprising guaiacol mixed with the root powder at 1.5,0.75,0.38 and 0.19% was prepared. Each formulation was mixed with 20g wheat (moisture content 12%) at 5,3,1 and 0.5% in stoppered glass tubes 150x23mm and the grain mixed with the formulated powder by a tumbling action of the tubes for one minute. Twenty adult Sitophilus oryzae (1-2 weeks old) were released into each tube and the tubes covered by muslin held by rubber bands. There were four replicates in each treatment. At weekly intervals the number of insects dead in each replicate was noted and the dead insects discarded. At the end of the third week the dead and live insects were discarded and the tubes incubated for emergence of the progeny (Fl generation). The results of the various parameters recorded are given in tables 1 and 2.
Table 1. Mortality of S.oryzae on wheat treated with D.hamiltonii root powder + guaiacol
(Table Removed)
Conclusions:
An increase in the proportion of guaiacol mixed with the powdered root of D.hamiltonii synergised the toxicity of the root powder to the test insect and also increased the speed of insect kill.
Table.2. Productivity of S.otyzae on wheat treated with formulations of D.hamiltonii root powder + guaiacol.
(Table Removed)
(40df)
The statistical analysis was made for 20 treatments inclusive of the controls.
Conclusions:
An increase in the proportion of guaiacol mixed with D.hamiltonii root powder increased the Insecticidal efficacy of the root powder by reducing the fecundity of the test insect.
EXAMPLE 2.
Bioefficacy of the synergistic formulation of D.hamiltonii root powder mixed with guaiacol aged for four months.
500g of the freeze dried roots of D.hamiltonii and powdered to 50mesh was mixed with guaiacol dissolved in diethyl ether. Formulations comprising guaiacol mixed with root powder at 1.5, 0.75,0.38 and 0.19% were prepared. The formulations were aged for four months by storing them in separate beakers covered by aluminium foils. The formulations were thus not stored in airtight containers. The bioefficacy of the formulated and unformulated (ie.control) root powders was examined after four months storage.
Each formulation was mixed with 20g wheat (moisture content 12%) at 5,3,1 and 0.5% in stoppered glass tubes 150x23mm and the grain mixed with the formulated powder by a tumbling action of the tubes for one minute. Twenty adult Sitophilus oryzae (1-2 weeks old) were released into each tube and the tubes covered by muslin held by rubber bands. There were four replicates in each treatment. At weekly intervals the number of insects dead in each replicate was noted and the dead insects discarded. At the end of the third week the dead and live insects were discarded and
the tubes incubated for emergence of the progeny (Fl generation). The results of the various parameters recorded are given in tables 3.
Table3. Bioefficacy of D.hamiltonii root powder + guaiacol aged for 4 months against S.oryzae on wheat.
(Table Removed)
Conclusions:
The addition of guaiacol to D hamiltonii root powder prolonged the residual toxicity of the root powder beyond 4 months, whereas the powder alone was least toxic to the test insects.
The synergistic mixture of D.hamiltonii root powder + guaiacol was active even after 4 months by reducing the productivity of the test insects, whereas the root powder alone was ineffective.
The main advantages of the present invention are:
1. An ecofriendly insecticide comprising a mixture of natural plant products for the protection of stored cereals from insect infestation.
2. A safe insecticide comprising a mixture of natural plant foods and/or products.
3. The insecticide formulation described not only exhibits toxicity to the adult insect pests but also exhibits the unique ovicidal activity even to eggs oviposited within the grain, thus enhancing the insecticidal potential of the formulation.
4. The insecticidal formulation described exhibited an active shelf life of more than four months compared to less than two months for the unformulated root powder.
5. The synergised insecticidal formulation described exhibited enhanced insecticidal activity compared to the unsynergised root powder of D.hamiltonii.

We Claim:
1. A process for preparation of composition useful for the insect free storage
of cereals comprising, mixing
a) substituted phenol such as herein described in the range of 0.75 to 25% (v/w),
b) dried roots powder of Decalepis hamiltonii in the range of 0.25 to 75% (w/w)

2. A process as claimed in claim 1, wherein the substituted phenol used is selected from guaiacol, dimethoxybenzaldehyde and vanillin.
3. A process as claimed in claims 1&2, wherein the particle size of dried roots is in the range of 50 to 100 mesh.
4. A process for preparation of composition useful for the insect free storage of cereals substantially as herein described with reference to the examples accompanying this specification.

Documents:

0086-del-2001-abstract.pdf

0086-del-2001-claims.pdf

0086-del-2001-complete specification granted.pdf

0086-DEL-2001-Correspondence-Others.pdf

0086-del-2001-correspondence-po.pdf

0086-del-2001-description (complete).pdf

0086-del-2001-form-1.pdf

0086-del-2001-form-2.pdf

0086-del-2001-form-4.pdf

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Patent Number

199867

Indian Patent Application Number

0086/DEL/2001

PG Journal Number

36/2008

Publication Date

05-Sep-2008

Grant Date

05-Jan-2007

Date of Filing

31-Jan-2001

Name of Patentee

Council of Scientific and Industrial Research

Applicant Address

Rafi Marg, New Delhi.

Inventors:

#	Inventor's Name	Inventor's Address
1	Pareira John	Central food technological research institute, Mysore-570013.
2	Mummigatti Suresh Gurappa	Central food technological research institute, Mysore-570013.
3	Krishnaiahi Hullukere Eraiah	Central food technological research institute, Mysore-570013.

PCT International Classification Number

AO IN 65/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA