Indian Patents. 235631:CHEMICALLY STABLE MONOCROTOPHOS FORMULATION AND PROCESS FOR PREPARATION THEREOF

Title of Invention	CHEMICALLY STABLE MONOCROTOPHOS FORMULATION AND PROCESS FOR PREPARATION THEREOF
Abstract	A chemically stable monocrotophos formulation having better shelf life and activity and stability comprising monocrotpphos as active ingredient, an absorbent, and one or more saccharides as stabilizing agents is provided.

Full Text	CHEM/MCP FORM 2 THE PATENTS ACT, 1970 (39 of 1970) & THE PATENTS RULES, 2003 PROVISIONAL SPECIFICATION (See Section 10 and Rule 13) 1. Title of the Invention:- "Chemically Stable Monocrotophos Formulation and Process for Preparation Thereof 2. Applicants:- (a) Name: CHEMINOVA INDIA LTD. (b) Nationality: An Indian National (c) Address: 7th Floor, Keshava Building, Bandra-Kula Complex, Bandra East, MUMBAI - 400 051, Maharashtra, INDIA 3. Preamble to the Description:- Provisional Specification: The following specification describes the nature of the Invention. CHEM/MCP Title of the Invention: Chemically Stable Monocrotophos Formulation and Process for Preparation Thereof. Field of the Invention: The present invention relates to a chemically stable monocrotophos formulation and process for preparation thereof. Particularly it relates to chemically stable solid form of monocrotophos formulation and process for preparation thereof. More particularly it relates to chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules of monocrotophos formulation and process for preparation thereof. Background of the Invention: The monocrotophos is commercially available insecticide, which can be systematically taken up by a plant so that insects, which feed and/or which live on the plants are killed, in addition to those insects which directly ingest or are contacted by the insecticide. The solid formulations are generally known to be more stable and easy to be packed, stored and transported because the solid formulations can be prepared without a solvent. Therefore, the main object of the present invention is to have monocrotophos formulation in solid form. The main problem in making solid formulation of monocrotophos is its poor chemical stability due to catalytically driven degradation of monocrotophos -the active ingredient [hereinafter referred to as AI] with carriers, fillers and base materials used in preparation of the solid formulation thereby 25 shortening, drastically, the shelf life of monocrotophos solid formulation. The AI degradation results in reduction of activity of the active ingredient meaning thereby the degradation problem renders the formulation useless for the desired purpose such as insecticides, etc. Therefore, AI degradation of solid form of monocrotophos formulation possesses serious problem for its 30 storage, which appears to be the main reason for non-availability of solid form of monocrotophos formulation. CHEM/MCP The another problem of solid formulations is that these comprise fillers and base materials which are generally not soluble in water, that is will have higher insoluble matter sediments, and therefore, cannot be made available as water soluble formulations, and hence, such solid formulations are always less preferred due to their higher insoluble matter sediments which poses a serious problem of chocking of spray nozzles thereby making such solid formulations less acceptable for use as spray formulation, and hence, cannot be easily applied on plants after dilution in water in a spray tank. 10 In US patent application no. 10/410,354, a reference has been made to solid form of monocrotophos formulation. This patent application discloses that a formulation consisting of monocrotophos and essentially an ester as active ingredients and an inert carrier is possible and can be formulated in general including as wettable powders, dusts, granules, fumigants formulations, etc. 15 However, no disclosure about activity and stability of disclosed formulations when comprising monocrotophos has been made in this application. Further, there is no indication whether the monocrotophos, without disclosed ester, but with defined carriers can result in chemically stable solid form of monocrotophos formulation. It is observed from the formulation 20 examples discussed in this application that chemically stable solid form of monocrotophos formulation even with defined ester may not be possible. Need of the Invention: Therefore, there is a need to develop a chemically stable monocrotophos formulation, particularly to develop a chemically stable solid form of 25 monocrotophos formulation and to have a chemically stable monocrotophos formulation, particularly a chemically stable solid form of monocrotophos formulation. Objects of the Invention: The main object of the present invention is to provide a chemically stable 30 monocrotophos formulation, particularly a chemically stable solid form of monocrotophos formulation, which does not suffer from the disadvantage of catalytically driven degradation of the active ingredient, and therefore, has CHEM/MCP better shelf life of the active ingredient and improved activity of the active ingredient meaning thereby the formulation is useful for the desired purpose as insecticides, etc. for a longer duration. Another object of the present invention is to provide a monocrotophos 5 formulation in solid form comprising reduced insoluble matter / sediments so as to have more acceptability as spray formulation. Still another object of the present invention is to provide a chemically stable monocrotophos formulation in the form of water soluble powder, or water dispersible powder, or water soluble granule, or water dispersible granules. 10 Yet another object of the present invention is to provide a monocrotophos formulation which is stable and can be easily packed, stored and transported without major loss of activity and stability of the active ingredient over a desired period of time. This is another object of the present invention to provide a monocrotophos 15 formulation in solid form which avoids use of undesired carriers, base materials, fillers etc. thereby making the disclosed formulation more economical and more easy to be formulated in-addition to being more stable. This is still an object of the present invention to provide a process for preparation of the chemically stable monocrotophos formulation, particularly 20 chemically stable solid form of monocrotophos formulation. The other objects and advantages of the present invention will become apparent from the following description of the invention. Brief Description and Nature of the Invention: The solid form of monocrotophos formulation has been found to be 25 chemically unstable due to catalytically driven degradation of the active ingredient meaning thereby the shelf life of solid form of monocrotophos formulation is greatly reduced. The reduced activity of the active ingredient [monocrotophos] of solid form of monocrotophos formulation due to catalytically driven degradation of CHEM/MCP monocrotophos makes the formulation useless for the desired purpose as insecticides, etc. for desired duration. The un-stability of the monocrotophos formulation possesses serious problem for its storage and then transportation. 5 The present invention is based on the observation that if chemical stability of the monocrotophos formulation, particularly of solid form of monocrotophos formulation can be increased, then the problem of un-stability of the monocrotophos formulation, particularly of solid form of monocrotophos formulation can be easily overcome. It is understood that formulation of monocrotophos with known carriers, fillers and base materials cannot overcome this problem. It has been surprisingly observed that if monocrotophos can be formulated with one or more saccharides, then its chemical stability has been found to be surprisingly very high. 15 However, in order to have solid form of monocrotophos formulation, the first need is to develop a mechanism to convert liquid form monocrotophos into solid form monocrotophos without disturbing its activity. It has been observed that if liquid form monocrotophos is mixed with an absorbent, preferably with silica, more preferably with precipitated silica, then it 20 converts to a solid form monocrotophos, which has been found to be convenient for formulating with saccharides. Accordingly, the present invention relates to a chemically stable monocrotophos formulation, particularly it relates to chemically stable solid form of monocrotophos formulation, more particularly it relates to chemically stable and water soluble powder, or chemically stable and water dispersible powder, or chemically stable and water soluble granular, or chemically stable and water dispersible granular forms of monocrotophos formulation comprising monocrotophos as active ingredient, an absorbent, and one or more saccharides as stabilizing agents. 30 In accordance with the present invention, the absorbent is selected from the group comprising silica, silicate or mixture thereof. The absorbent is preferably silica, more preferably precipitated silica which absorbs the liquid CHEM/MCP form active ingredient and converts it into a solid form active ingredient and makes it suitable for formulating with one or more saccharides to produce desired chemically stable solid monocrotophos formulation. In accordance with the present invention, the saccharide is selected from the 5 group comprising mono-saccharides, di-saccharides, or mixtures thereof, particularly from the group comprising lactose, dextrose, sucrose, or the mixture thereof. The lactose is preferably lactose monohydrate. In accordance with preferred embodiment of the present invention, the monocrotophos formulation may comprise one or more surfactants. The 10 surfactants may be selected from a group comprising napthalene phenol formaldehyde condensate [Tysperse DN], aryl alkyl sulphonate and aryl sulphonic acid formaldehyde condensate, sodium salt of phenol sulphonic acid condensate, sodium salt of sulphated fatty alcohol, sodium ligno sulphonates, napthalene sulphonic acid formaldehyde condensate, or 15 mixtures thereof. The preferred surfactant is Tysperse DN. In accordance with the present invention, the surfactant is so selected, which can also act as dispersing agent, or as wetting agent or as dispersing agent and wetting agent thereby resulting in improvement of spreading properties of the formulation. The advantage of selecting Tysperse DN is that 20 it has been found to act as dispersing agent as well as wetting agent. Further, Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica] in suspension form causing less sediment on dissolution in water thereby has been surprisingly found to avoid the chocking problem of the spray nozzles when the presently 25 disclosed formulation is used as spray formulation. In accordance with one of the preferred embodiments of the present invention, the monocrotophos formulation may optionally comprise one or more binding agents. The binding agent is selected from the group comprising vinyl acetate copolymer, hydroxy propyl methyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl pyrrolidone co-polymer, polyacrylic acid, cabo methoxy cellulose, casein, gelatin, acacia, synthetic glue, xanthan gum, guar gum, gum arabic, lignin, or mixture thereof. CHEM/MCP In accordance with another preferred embodiment of the present invention, the monocrotophos formulation may optionally comprise one or more coating agents. The coating agent is selected from the group comprising sugar, polyvinyl alcohol, lignosulphonates, starch, cellulose derivatives, methyl 5 cellulose, hydoxy propyl methyl cellulose, alginates, or mixture thereof. In accordance with still another preferred embodiment of the present invention, the monocrotophos formulation may optionally comprise one or more additional active ingredient selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof. The 10 fungicide may be selected from the group comprising carbendazim, hexaconazole, mancozeb, thiram, captafol, captan, maneb, propicanazole, tricyclazole, tebuconazole, chlorothalonil, zineb, ziram, methyl thiophanate, or mixture thereof. The additional insecticide may be selected from the group comprising chlorpyriphos, qunalphos, acephate, dichlorvos, dimethyl, 15 phenthoate, malathion, ethion, fenvelarate, cypermethrin, permethrin, cyhalothrin, deltamethrin, cycloprothrin, or mixture thereof. It has been surprising observed that when monocrotophos in absorbed form on silica is formulated with selected one or more saccharides, it does not suffer from the disadvantage of catalytically driven degradation of the active 20 ingredient even on storage, and therefore, it has been found to have unexpectedly better shelf life of the active ingredient and surprisingly improved activity and stability of the active ingredient meaning thereby the presently disclosed formulation has been found to be more stable and useful for the desired purpose as insecticides, etc. even for a longer duration, 25 preferably for about one year or more. It has been further observed that selected saccharides in the monocrotophos formulation of the present invention wherein monocrotophos is taken in absorbed form on silica and formulated with one or more selected saccharides enhance water soluble matter of the formulation. 30 The enhanced water soluble matter in the presently disclosed formulation has been observed to overcome problem of chocking of spray nozzles thereby making the presently disclosed formulation more acceptable for use as spray CHEM/MCP formulation, and hence can be easily applied on plants after dilution in water in a spray tank. The presently disclosed formulation in water soluble powder form or in water soluble granular form has better solubility in water. However, after 5 dissolution in water, the spray solution form of the formulation may contain certain amount of insoluble silica, which is employed as absorbent, as insoluble matter/sediments. However, it has been observed that the advantages of silica as absorbent overcome disadvantage of it being in insoluble form, therefore, the insoluble nature of silica does not pose serious 10 problem within the selected range as described herein. Further, as described herein, the presently selected surfactant, preferably Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica] in suspension form causing less sediment on dissolution in water thereby has been surprisingly found to avoid the chocking problem of 15 the spray nozzles when the presently disclosed formulation is used as spray formulation. If the additional active ingredients are insoluble or less soluble in water, then the presently disclosed formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible 20 granules. The presently disclosed monocrotophos formulation has been observed to have more than about 50% water soluble matter, that is more than about 50% solubility. The addition of additional active ingredients has been observed to result in lowering of solubility of monocrotophos. 25 It has also been surprisingly observed that when monocrotophos in absorbed form on silica is formulated with selected one or more saccharides, the saccharide also serves the purpose of carrier, filler and base material, thereby in accordance with the present invention no additional carrier, filler and base material is required to be mixed with the formulation meaning 30 thereby making the presently disclosed formulation more economical and more easy to be formulated by avoiding use of undesired carriers, base materials, fillers etc. CHEM/MCP It has also been observed that use of fillers, carriers and base materials in a formulation may also reduce solubility of the formulation, therefore, it can be said that absence of fillers, carriers and base materials in the present formulations helps in increase in solubility of the present formulation. 5 The solid form of chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules of the presently disclosed monocrotophos formulation have been found to have additional advantages of ease of packaging, storing and transportation even without major loss of 10 activity and stability of the active ingredient over a desired period of time. The presently disclosed solid form monocrotophos formulation which can be made available as chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules can be dissolved or dispersed 15 in water and sprayed thereby it has been found to overcome the disadvantages of water insolubility and chocking during spraying. In accordance with the present invention, the monocrotophos formulation can be made available with desired activity of the active ingredient. For example, monocrotophos formulation can be made available with the activity 20 varying from about 5% to about 50% of the active ingredient, preferably with the activity varying from about 15% to about 40% of the active ingredient, more preferably with the activity varying from about 20% to about 35% of the active ingredient. In accordance with one embodiment of the present invention, the 25 monocrotophos formulation comprises at least about 5%, preferably from about 5% to about 90% of one or more saccharides of the total formulation. In accordance with another embodiment of the present invention, the monocrotophos formulation comprises from about 10% to about 40% of one or more saccharides of the total formulation. 30 In accordance with preferred embodiment of the present invention, the monocrotophos formulation comprises from about 20% to about 35% of one or more saccharides of the total formulation. CHEM/MCP In accordance with another preferred embodiment of the present invention, the monocrotophos formulation comprises about 30% of one or more saccharides of the total formulation. In accordance with the present invention, the monocrotophos formulation comprises at least about 5% of monocrotophos of the desired activity and at least about 5% of one or more saccharides and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation. The percent amount referred is with reference to amount of the total formulation. 10 In accordance with one embodiment of the present invention, the monocrotophos formulation comprises monocrotophos of the desired activity in an amount varying from about 5% to about 70% of the total formulation and one or more saccharides in an amount varying from about 5% to about 90% of the total formulation and the balance being absorbent while taking 15 care that the amount of silica is restricted upto about 50% of the total formulation. In accordance with one embodiment of the present invention, the monocrotophos formulation comprises monocrotophos of the desired activity in an amount varying from about 5% to about 70% of the total formulation and one or more saccharides in an amount varying from about 10% to about 40% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation. In accordance with one embodiment of the present invention, the monocrotophos from about 5% to about 50% of the total formulation and one or more saccharides in an amount varying from about 20% to about 35% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total 30 formulation. In accordance with one embodiment of the present invention, the monocrotophos formulation comprises monocrotophos of the desired activity CHEM/MCP in an amount varying from about 5% to about 50% of the total formulation and one or more saccharides in an amount of about 30% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation. 5 The amount of one or more saccharides as described herein is the amount of all saccharides, if the formulation comprises more than one saccharides. In accordance with one of the preferred embodiments of the present invention, the monocrotophos formulation may additionally comprise one or more auxiliaries selected from the group comprising surfactants, binding agents, coating agents, or mixtures thereof in an amount so that the total amount of these auxiliaries does not exceed more than about 10% of the total formulation. In accordance with another preferred embodiment of the present invention, the monocrotophos formulation may additionally comprise one or more additional active ingredient selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof in any amount, preferably in an amount so that the total amount of these additional active ingredients varies upto about 10% of the total formulation so that the desired activity of the monocrotophos is not suppressed. 20 In one embodiment, the present invention relates to a process for preparation of chemically stable monocrotophos formulation comprising absorbing weighed quantity of liquid monocrotophos on weight quantity of absorbent to result in formation of powder of monocrotophos followed by mixing the powder of monocrotophos with weighed quantity of one or more 25 of saccharides to form monocrotophos formulation which can be made available as chemically stable water soluble powder or chemically stable water dispersible powder. In another embodiment, the present invention relates to a process for preparation of chemically stable monocrotophos formulation comprising absorbing weighed quantity of liquid monocrotophos on weight quantity of absorbent to result in formation of powder of monocrotophos followed by mixing the powder of monocrotophos with weighed quantity of one or more CHEM/MCP of saccharides to form monocrotophos formulation which is then mixed with water to result in dough which is extruded through an extruder. On drying the extrudates in a fluid bed drier, the present formulation can be made available as chemically stable water soluble granules or chemically stable water dispersible granules. It may be noted that the present formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible granules when the additional active ingredient is either insoluble or less soluble in water. 10 The homogeneous mixing of the ingredients while blending results in formation of homogeneous, chemically stable, water soluble powder or homogeneous, chemically stable, water dispersible powder form of the formulation. The mixing while granulating results in formation of chemically stable, water soluble granules or water dispersible granules. 15 In accordance with preferred embodiment of the present invention, one or more of auxiliaries and/or additional active ingredients may also be mixed in the monocrotophos formulation while formulating powder or granules of monocrotophos with one or more selected saccharides of the present invention. 20 The term granules, as employed herein, is intended to include solid pellets, granules, grains and the like. In accordance with present invention, the term granules, as employed herein, is intended to include a granule wherein monocrotophos forms core of the granule and the saccharide forms a coating over the core of the granule, and a granule wherein the saccharide forms 25 core of the granule and monocrotophos forms a coating over the core of the granule, and a granule wherein no such discrete core or coating is formed, that is, the granule having a substantially uniform composition. The granules may have any particle size, preferably may have particle size varying from about 0.1mm or more, more preferably from about 0.1mm to about 2.0mm diameter. The term chemically stable, as employed herein, means that the activity of the active ingredient does not fall more than 10%, preferably more than 7% CHEM/MCP of the originally selected activity of the active ingredient, and such drop in activity of the active ingredient is calculated after about 28 days in accelerated storage at about 54°C [ace storage] and after about one year at ambient storage. 5 The active ingredient referred herein is monocrotophos and the additional active ingredient referred herein is selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof. It has been observed that drop in activity of the active ingredient of the formulation in accordance with present invention is well within the limits, that is less than 10% over a period of one year. The activity of the active ingredient is checked by Bureau of Indian standards - IS specification no. 8025 : 1990. It may be noted that the scope of the present invention is not restricted by the manner of mixing saccharides, other auxiliaries and additional active ingredients, which may be mixed in any manner. The present invention is now described with the help of following experimental examples, which are illustrated in following tables wherein compositions of various formulations prepared in accordance with present invention have been disclosed. 20 Table no. 1 illustrates seven formulations prepared in accordance with present invention wherein the saccharide is either lactose monohydrate, or dextrose, or sucrose, or combination of lactose monohydrate and dextrose, or combination of lactose monohydrate and sucrose, or combination of dextrose and sucrose, or combination of lactose monohydrate, dextrose and 25 sucrose. The formula H illustrates a standard formulation prepared without saccharide disclosed in the present invention. Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared CHEM/MCP without incorporating one or more of saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 75% water soluble matter. Table no.: 1 Stability of MCP 30% SP using Lactose Monohydrate, Dextrose, Sucrose and its combinations 10 Name of the ingredient Weight percentage Formula. A Formula. B Formula. C Formula. D Formul E Formula. F Formula. G Formula. H Monocrotophos Al in formulation 30% 30% 30% 30% 30% 30% 30% 30% Monocrotophos tech (74% Al) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% Ppt Silica (Sypernat 22 S) 25% 25% 25% 25% 25% 25% 25% 25% Lactose Monohydrate 29.5% 19.5% 19.5% - - - 10% - Dextrose - 10% - 19.5% 29.5% - 10% - Sucrose - - 10% 10% - 29.5% 9.5% - Kaolin - - - - - - - 29.5% Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% Drop in Monocrotophos Al after 28 days ace storage 4% 4.2% 4.6% 4.9% 4.6% 5.1% 4.6% 11% Drop in Monocrotophos AI after one year ambient storage 4% 4.4% 4.7% 5.0% 4.4% 5.3% 4 9% 12% Water soluble matter 75% 75% 75% 75% 75% 75% 75% 45.5% Table no. 2 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right side of the table. The formula H illustrates a standard formulation prepared without saccharide. Each formulation was analyzed for drop in activity of active ingredient - monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 7% of the originally selected CHEM/MCP activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was 5 observed that each formulation prepared in accordance with present invention shows about 70 to 90% water soluble matter. Table no. : 2 Stability of different concentrations of MCP AI with Lactose Monohydrate Name of the ingredient Weight percentage Formul A Formula. B Formula. C Formul. D Formula. E Formul F Formula. G Formula. H Monocrotophos AI in formulation 5% 10% 15% 20% 25% 35% 40% 50% Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 47.30% 54.05% 67.57% Ppt Silica (Sypernat 22 S) 10% 15% 20% 25% 25% 25% 30% 27.43% Lactose Monohydrate 78.24% 66.46% 54.73% 42.98% 36.22% 22.70% 10.95% - Dextrose - - - - - - - - Sucrose - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% Drop in Monocrotophos AI after 28 days ace storage 0.70% 1.30% 2.10% 3.0% 3.9% 4.5% 5.8% 11% Drop inMonocrotophosAI after oneyear ambientstorage 0.80% 1.40% 2.50% 3.2% 4.6% 4.7% 5.6% 12% Water soluble matter 90% 85% 80% 75% 75% 75% 70% 72.50% Table no. 3 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide. Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 10.1% of the originally selected activity of the active ingredient. However, the standard formulation CHEM/MCP prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 50 to 80% water soluble matter. The formulations disclosed in Table 3 confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10 10% or more show better stability even after one year of storage and very high water soluble matter. Table no. : 3 Stability of MCP 30% AI with different concentrations of Lactose Monohydrate 15 Name of the ingredient Weight percentage Formula. A Formula. B Formula. C Formula. D Formula. E Formula. F Formula. 0 Formul. H Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30% Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34.5% 29.5% 24.5% 19.5% 54.5% Lactose Monohydrate 5% 10% 15% 20% 25% 30% 35% - Dextrose - - - - - - - - Sucrose - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% Drop in Monocrotophos AI after 28 days ace storage 10.1% 8.9% 7.5% 6.2% 5.0% 4% 3.6% 11% Drop in Monocrotophos AI after one year ambient storage 9.8% 8.8% 7.3% 6.3% 4.9% 4% 3.4% 12% Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5% Table no. 4 illustrates formulations prepared in accordance with present invention wherein the saccharide is dextrose and initial activity of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide. Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient CHEM/MCP storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 10.3% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 50 to 80% water soluble matter. The formulations disclosed in Table 4 also confirm that monocrotophos formulations comprising dextrose within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. Table no. : 4 Stability of MCP 30% AI with different concentrations of Dextrose Name of the ingredient Weight percentage Formul A Formul B Formul C Formula D FormulaE Formula F Formula G Formula H Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30% Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34 5% 29.5% 24.5% 19.5% 54.5% Lactose Monohydrate - - - - - - - - Dextrose 5% 10% 15% 20% 25% 30% 35% - Sucrose - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% Drop in Monocrotophos AI after 28 days ace storage 10.3% 9.2% 7.7% 6.5% 5.3% 4.4% 3.8% 11% Drop in Monocrotophos AI after one year ambient storage 10.0% 9.1% 7.6% 6.5% 5.3% 4.3% 3.6% 12% Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5% Table no. 5 illustrates formulations prepared in accordance with present invention wherein the saccharide is sucrose and initial activity of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide. CHEM/MCP Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 10.4% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 50 to 80% water soluble matter. The formulations disclosed in Table 5 also confirm that monocrotophos formulations comprising sucrose within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. Table no. : 5 Stability of MCP 30% AI with different concentrations of Sucrose Name of the ingredient Weight percentage Formula A Formula B Formula C Formula D FormulaE FormulaF Formula G Formula H Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30% Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34.5% 29.5% 24.5% 19.5% 54.5% Lactose Monohydrate - - - - - - - - Dextrose - - - - - - - - Sucrose 5% 10% 15% 20% 25% 30% 35% - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% Drop in Monocrotophos AI after 28 days ace storage 10.4% 9.4% 7.8% 6.7% 5.5% 5% 4.1% 11% Drop in Monocrotophos AI after one year ambient storage 10.1% 9.1% 7.7% 6.9% 5.7% 5.2% 3.8% 12% Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5% Table no. 6 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right. The formulation I illustrates a standard formulation prepared without saccharide. The formulations illustrated in Table 6 also comprise one or more of fungicides described hereinabove. Each formulation was analyzed for drop in activity of active CHEM/MCP ingredient - monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 35 to 70% water soluble matter. The formulations disclosed in Table 6 also confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, fungicide. Table no.: 6 Stability of different cone, of MCP Al + different cone, of Fungicides Al with Lactose Monohydrate Name of the ingredient Weight percentage Formul A Formula B Formula C Formula D Formul E Formula F Formula G Formul H Formul I Monocrotophos Al in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50% Monocrotophos tech (74% Al) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57% Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 27.43% Lactose Monohydrate 26.14% 24.65% 23.15% 16.66% 15.17% 13.72% 12.18% 10.69% - Dextrose - - - - - - - - - Sucrose - - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5% Fungicide 42.1% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% - Drop in Monocrotophos Al after 28 days ace storage 0.90% 1.60% 2.40% 3.20% 4.0% 4.4% 5.0% 6.5% 11% Drop in Monocrotophos Al after one year ambient storage 1.0% 1.50% 2.60% 3.3% 3.9% 4.3% 5.1% 6.4% 12% Water soluble matter 37.86% 43.16% 48.42% 48.68% 53.95% 59.22% 64.48% 69.74% 72.57% Table no. 7 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right. The formulation I illustrates CHEM/MCP a standard formulation prepared without saccharide. The formulations illustrated in Table 7 also comprise one or more of additional active ingredient - insecticides described hereinabove. Each formulation was analyzed for drop in activity of active ingredient - monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared without 10 incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 30 to 70% water soluble matter. The formulations disclosed in Table 7 15 also confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide. 20 Table no.: 7 Stability of different cone, of MCP AI + different cone, of insecticides AI with Lactose Monohydrate Name of the ingredient Weight percentage Formul A Formula B Formul. C Formul D Formul E Formul F Formul G Formul H Formul I Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50% Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57% Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 27.43% Lactose Monohydrate 24.77% 23.45% 22.13% 15.81% 14.48% 13.21% 11.83% 10.52% - Dextrose - - - - - - - - - Sucrose - - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5% Insecticide 43.47% 38.04% 32.60% 27.17% 21.74% 16.29% 10.87% 5.43% - Drop inMonocrotophos AI after 28 days ace storage 0.80% 1.3% 2.1% 3.0% 4.0% 4.3% 4.9% 6.2% 11% Drop inMonocrotophos AI after one year ambient storage 0.9% 1.50% 2.2% 3.1% 3.8% 4.2% 4.7% 6.0% 12% Water soluble matter 33.53% 41.96% 47.4% 47.83% 53.26% 58.71% 64.13% 69.57% 72.57% CHEM/MCP Table no. 8 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right. The formulation I illustrates a standard formulation prepared without saccharide. The formulations illustrated in Table 8 also comprise one or more of additional active ingredient - insecticides and auxiliaries - binding agent and coating agent described hereinabove. Each formulation was analyzed for drop in activity of active ingredient - monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of 10 monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 15 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 30 to 70% water soluble matter. The formulations disclosed in Table 8 also confirm that monocrotophos formulations comprising lactose monohydrate within 20 preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide. Table no.: 8 25 Stability of different cone, of MCP AI + different cone, of insecticides AI with Lactose Monohydrate Name of the ingredient Weight percenta ge Formula A Formula B Formula C Formul D Formul E FormulaF Formula G Formula H Formula 1 Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50% Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57% Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 26.43% Lactose Monohydrate 23.77% 22.45% 21.13% 14.81% 13.48% 12.21% 10.83% 9.52% - Dextrose - - - - - - - - - Sucrose - - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5% Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% Insecticide 43.47% 38.04% 32.60% 27.17% 21.74% 16.29% 10.87% 5.43% - Fungicide - - - - - - - - - CHEM/MCP Drop inMonocrotophosAlafter 28 daysace storage 0.9% 1.2% 2.0% 2.9% 4.0% 4.5% 5.0% 5.8% 11% Drop inMonocrotophosAlafter one yearambient storage 0.7 % 1.3% 2.2% 3.0% 3.9% 4.4% 5.2% 6.0% 12% Water soluble matter 33.53% 41.96% 47.4% 47.83% 53.26% 58.71% 64.13% 69.57% 72.57% Table no. 9 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right. The formulation I illustrates a standard formulation prepared without saccharide. The formulations illustrated in Table 9 also comprise one or more of additional active ingredient - fungicides and auxiliaries - binding agent and coating agent described hereinabove. Each formulation was analyzed for drop in activity of active ingredient - 10 monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared 15 without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 35 to 70% water soluble matter. The formulations 20 disclosed in Table 9 also confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, 25 fungicide. CHEM/MCP Table no.: 9 Stability of different cone, of MCP AI + different cone, of fungicide AI with Lactose Monohydrate Name of the ingredient Weight percentage Formula A Formula B Formula C Formula D Formul E Formula F Formula G Formula H Formul I Monocrotophos Al in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50% Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57% Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 26.43% Lactose Monohydrate 25.14% 23.65% 22.15% 15.66% 14.17% 12.72% 11.18% 9.69% - Dextrose - - - - - - - - - Sucrose - - - - - - - - - Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5% Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% Fungicide 42.1% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% - Drop inMonocrotophos AI after 28 days ace storage 1.0% 1.70% 2.30% 3.10% 40% 4.5% 5.2% 6.6% 11% Drop inMonocrotophos AI after one year ambient storage 0.9% 1.50% 2.40% 3.0% 3.8% 4.6% 5.3% 6.4% 12% Water soluble matter 37.86% 43.16% 48.42% 48.68% 53.95% 59.22% 64.48% 69.74% 72.57% It may be noted various modifications are possible for the formulations illustrated in the Tables provided herein without deviating from the intended scope of present invention. Therefore, in one embodiment the present invention includes all formulations which can be prepared without deviating from its scope. It may be noted that the term water soluble powder or granules as employed herein means a formulation in which the active ingredient is fully dissolved in spray solution despite the fact that the spray solution may contain a certain amount of insoluble silica which is very low in the monocrotophos 15 formulation disclosed in the present invention and the term water dispersible powder or granules means a formulation in which the active ingredient is not fully dissolved in the final spray solution, but it is dispersed. The amounts or volumes of various ingredients described herein and in the 20 Tables are with reference to the total weight or total volume of the formulation and are taken in a way so as to have a total of 100%. These CHEM/MCP amounts may, however, vary within the permissible limits of practically allowable ranges of each ingredient of the present formulation. The word "about" appearing before various values is intended to include practically permissible limits of variations in respective value. 5 Dated this 24th day of June, 2006. [Dr. Ramesh kr. MEHTA] Patent Attorney for the Applicants 10 Of Mehta & Mehta Associates

Full Text

CHEM/MCP
FORM 2
THE PATENTS ACT, 1970 (39 of 1970)
&
THE PATENTS RULES, 2003
PROVISIONAL SPECIFICATION
(See Section 10 and Rule 13)
1. Title of the Invention:-
"Chemically Stable Monocrotophos Formulation and Process for Preparation Thereof
2. Applicants:-
(a) Name: CHEMINOVA INDIA LTD.
(b) Nationality: An Indian National
(c) Address: 7th Floor, Keshava Building, Bandra-Kula Complex,
Bandra East, MUMBAI - 400 051, Maharashtra, INDIA
3. Preamble to the Description:-
Provisional Specification:
The following specification describes the nature of the Invention.

CHEM/MCP
Title of the Invention:
Chemically Stable Monocrotophos Formulation and Process for Preparation Thereof.
Field of the Invention:
The present invention relates to a chemically stable monocrotophos formulation and process for preparation thereof. Particularly it relates to chemically stable solid form of monocrotophos formulation and process for preparation thereof. More particularly it relates to chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules of monocrotophos formulation and process for preparation thereof.
Background of the Invention:
The monocrotophos is commercially available insecticide, which can be systematically taken up by a plant so that insects, which feed and/or which live on the plants are killed, in addition to those insects which directly ingest or are contacted by the insecticide.
The solid formulations are generally known to be more stable and easy to be packed, stored and transported because the solid formulations can be prepared without a solvent. Therefore, the main object of the present invention is to have monocrotophos formulation in solid form.
The main problem in making solid formulation of monocrotophos is its poor chemical stability due to catalytically driven degradation of monocrotophos -the active ingredient [hereinafter referred to as AI] with carriers, fillers and base materials used in preparation of the solid formulation thereby
25 shortening, drastically, the shelf life of monocrotophos solid formulation. The AI degradation results in reduction of activity of the active ingredient meaning thereby the degradation problem renders the formulation useless for the desired purpose such as insecticides, etc. Therefore, AI degradation of solid form of monocrotophos formulation possesses serious problem for its
30 storage, which appears to be the main reason for non-availability of solid form of
monocrotophos formulation.

CHEM/MCP
The another problem of solid formulations is that these comprise fillers and base materials which are generally not soluble in water, that is will have higher insoluble matter sediments, and therefore, cannot be made available as water soluble formulations, and hence, such solid formulations are always less preferred due to their higher insoluble matter sediments which poses a serious problem of chocking of spray nozzles thereby making such solid formulations less acceptable for use as spray formulation, and hence, cannot be easily applied on plants after dilution in water in a spray tank.
10 In US patent application no. 10/410,354, a reference has been made to solid form of monocrotophos formulation. This patent application discloses that a formulation consisting of monocrotophos and essentially an ester as active ingredients and an inert carrier is possible and can be formulated in general including as wettable powders, dusts, granules, fumigants formulations, etc.
15 However, no disclosure about activity and stability of disclosed formulations when comprising monocrotophos has been made in this application. Further, there is no indication whether the monocrotophos, without disclosed ester, but with defined carriers can result in chemically stable solid form of monocrotophos formulation. It is observed from the formulation
20 examples discussed in this application that chemically stable solid form of monocrotophos formulation even with defined ester may not be possible.
Need of the Invention:
Therefore, there is a need to develop a chemically stable monocrotophos formulation, particularly to develop a chemically stable solid form of
25 monocrotophos formulation and to have a chemically stable monocrotophos formulation,
particularly a chemically stable solid form of monocrotophos formulation.
Objects of the Invention:
The main object of the present invention is to provide a chemically stable
30 monocrotophos formulation, particularly a chemically stable solid form of
monocrotophos formulation, which does not suffer from the disadvantage of
catalytically driven degradation of the active ingredient, and therefore, has

CHEM/MCP
better shelf life of the active ingredient and improved activity of the active ingredient meaning thereby the formulation is useful for the desired purpose as insecticides, etc. for a longer duration.
Another object of the present invention is to provide a monocrotophos
5 formulation in solid form comprising reduced insoluble matter / sediments so as to have more
acceptability as spray formulation.
Still another object of the present invention is to provide a chemically stable monocrotophos formulation in the form of water soluble powder, or water dispersible powder, or water soluble granule, or water dispersible granules.
10 Yet another object of the present invention is to provide a monocrotophos formulation which is stable and can be easily packed, stored and transported without major loss of activity and stability of the active ingredient over a desired period of time.
This is another object of the present invention to provide a monocrotophos
15 formulation in solid form which avoids use of undesired carriers, base
materials, fillers etc. thereby making the disclosed formulation more
economical and more easy to be formulated in-addition to being more stable.
This is still an object of the present invention to provide a process for preparation of the
chemically stable monocrotophos formulation, particularly 20 chemically stable solid form of monocrotophos formulation.
The other objects and advantages of the present invention will become apparent from the following description of the invention.
Brief Description and Nature of the Invention:
The solid form of monocrotophos formulation has been found to be 25 chemically unstable due to catalytically driven degradation of the active ingredient meaning
thereby the shelf life of solid form of monocrotophos formulation is greatly reduced.
The reduced activity of the active ingredient [monocrotophos] of solid form of monocrotophos formulation due to catalytically driven degradation of

CHEM/MCP
monocrotophos makes the formulation useless for the desired purpose as insecticides, etc. for desired duration. The un-stability of the monocrotophos formulation possesses serious problem for its storage and then transportation.
5 The present invention is based on the observation that if chemical stability of the
monocrotophos formulation, particularly of solid form of monocrotophos formulation
can be increased, then the problem of un-stability of the monocrotophos formulation,
particularly of solid form of monocrotophos formulation can be easily overcome. It is
understood that formulation of monocrotophos with known carriers, fillers and base
materials cannot overcome this problem.
It has been surprisingly observed that if monocrotophos can be formulated with one or more saccharides, then its chemical stability has been found to be surprisingly very high.
15 However, in order to have solid form of monocrotophos formulation, the first need is to develop a mechanism to convert liquid form monocrotophos into solid form monocrotophos without disturbing its activity. It has been observed that if liquid form monocrotophos is mixed with an absorbent, preferably with silica, more preferably with precipitated silica, then it
20 converts to a solid form monocrotophos, which has been found to be convenient for formulating with saccharides.
Accordingly, the present invention relates to a chemically stable monocrotophos formulation, particularly it relates to chemically stable solid form of monocrotophos formulation, more particularly it relates to chemically stable and water soluble powder, or chemically stable and water dispersible powder, or chemically stable and water soluble granular, or chemically stable and water dispersible granular forms of monocrotophos formulation comprising monocrotophos as active ingredient, an absorbent, and one or more saccharides as stabilizing agents.
30 In accordance with the present invention, the absorbent is selected from the group comprising silica, silicate or mixture thereof. The absorbent is preferably silica, more preferably precipitated silica which absorbs the liquid

CHEM/MCP
form active ingredient and converts it into a solid form active ingredient and makes it suitable for formulating with one or more saccharides to produce desired chemically stable solid monocrotophos formulation.
In accordance with the present invention, the saccharide is selected from the
5 group comprising mono-saccharides, di-saccharides, or mixtures thereof, particularly
from the group comprising lactose, dextrose, sucrose, or the mixture thereof. The
lactose is preferably lactose monohydrate.
In accordance with preferred embodiment of the present invention, the monocrotophos formulation may comprise one or more surfactants. The
10 surfactants may be selected from a group comprising napthalene phenol formaldehyde condensate [Tysperse DN], aryl alkyl sulphonate and aryl sulphonic acid formaldehyde condensate, sodium salt of phenol sulphonic acid condensate, sodium salt of sulphated fatty alcohol, sodium ligno sulphonates, napthalene sulphonic acid formaldehyde condensate, or
15 mixtures thereof. The preferred surfactant is Tysperse DN.
In accordance with the present invention, the surfactant is so selected, which can also act as dispersing agent, or as wetting agent or as dispersing agent and wetting agent thereby resulting in improvement of spreading properties of the formulation. The advantage of selecting Tysperse DN is that
20 it has been found to act as dispersing agent as well as wetting agent. Further, Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica] in suspension form causing less sediment on dissolution in water thereby has been surprisingly found to avoid the chocking problem of the spray nozzles when the presently
25 disclosed formulation is used as spray formulation.
In accordance with one of the preferred embodiments of the present invention, the monocrotophos formulation may optionally comprise one or more binding agents. The binding agent is selected from the group comprising vinyl acetate copolymer, hydroxy propyl methyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl pyrrolidone co-polymer, polyacrylic acid, cabo methoxy cellulose, casein, gelatin, acacia, synthetic glue, xanthan gum, guar gum, gum arabic, lignin, or mixture thereof.

CHEM/MCP
In accordance with another preferred embodiment of the present invention, the monocrotophos formulation may optionally comprise one or more coating agents. The coating agent is selected from the group comprising sugar, polyvinyl alcohol, lignosulphonates, starch, cellulose derivatives, methyl
5 cellulose, hydoxy propyl methyl cellulose, alginates, or mixture thereof.
In accordance with still another preferred embodiment of the present invention, the monocrotophos formulation may optionally comprise one or more additional active ingredient selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof. The
10 fungicide may be selected from the group comprising carbendazim, hexaconazole, mancozeb, thiram, captafol, captan, maneb, propicanazole, tricyclazole, tebuconazole, chlorothalonil, zineb, ziram, methyl thiophanate, or mixture thereof. The additional insecticide may be selected from the group comprising chlorpyriphos, qunalphos, acephate, dichlorvos, dimethyl,
15 phenthoate, malathion, ethion, fenvelarate, cypermethrin, permethrin, cyhalothrin, deltamethrin, cycloprothrin, or mixture thereof.
It has been surprising observed that when monocrotophos in absorbed form on silica is formulated with selected one or more saccharides, it does not suffer from the disadvantage of catalytically driven degradation of the active
20 ingredient even on storage, and therefore, it has been found to have unexpectedly better shelf life of the active ingredient and surprisingly improved activity and stability of the active ingredient meaning thereby the presently disclosed formulation has been found to be more stable and useful for the desired purpose as insecticides, etc. even for a longer duration,
25 preferably for about one year or more.
It has been further observed that selected saccharides in the monocrotophos formulation of the present invention wherein monocrotophos is taken in absorbed form on silica and formulated with one or more selected saccharides enhance water soluble matter of the formulation.
30 The enhanced water soluble matter in the presently disclosed formulation has been observed to overcome problem of chocking of spray nozzles thereby making the presently disclosed formulation more acceptable for use as spray

CHEM/MCP
formulation, and hence can be easily applied on plants after dilution in water in a spray tank.
The presently disclosed formulation in water soluble powder form or in water soluble
granular form has better solubility in water. However, after 5 dissolution in water, the spray solution form of the formulation may contain certain
amount of insoluble silica, which is employed as absorbent, as insoluble
matter/sediments. However, it has been observed that the advantages of silica as
absorbent overcome disadvantage of it being in insoluble form, therefore, the insoluble
nature of silica does not pose serious
10 problem within the selected range as described herein. Further, as described herein, the presently selected surfactant, preferably Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica] in suspension form causing less sediment on dissolution in water thereby has been surprisingly found to avoid the chocking problem of
15 the spray nozzles when the presently disclosed formulation is used as spray formulation.
If the additional active ingredients are insoluble or less soluble in water, then the presently disclosed formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible
20 granules.
The presently disclosed monocrotophos formulation has been observed to have more than about 50% water soluble matter, that is more than about 50% solubility. The addition of additional active ingredients has been observed to result in lowering of solubility of monocrotophos.
25 It has also been surprisingly observed that when monocrotophos in absorbed form on silica is formulated with selected one or more saccharides, the saccharide also serves the purpose of carrier, filler and base material, thereby in accordance with the present invention no additional carrier, filler and base material is required to be mixed with the formulation meaning
30 thereby making the presently disclosed formulation more economical and more easy to be formulated by avoiding use of undesired carriers, base materials, fillers etc.

CHEM/MCP
It has also been observed that use of fillers, carriers and base materials in a formulation may also reduce solubility of the formulation, therefore, it can be said that absence of fillers, carriers and base materials in the present formulations helps in increase in solubility of the present formulation.
5 The solid form of chemically stable water soluble powder, or chemically stable water
dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules of the presently disclosed monocrotophos formulation have been found to have additional advantages of ease of packaging, storing and
transportation even without major loss of
10 activity and stability of the active ingredient over a desired period of time.
The presently disclosed solid form monocrotophos formulation which can be made available as chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules can be dissolved or dispersed
15 in water and sprayed thereby it has been found to overcome the disadvantages of
water insolubility and chocking during spraying.
In accordance with the present invention, the monocrotophos formulation can be made available with desired activity of the active ingredient. For example, monocrotophos formulation can be made available with the activity
20 varying from about 5% to about 50% of the active ingredient, preferably with the
activity varying from about 15% to about 40% of the active ingredient, more preferably
with the activity varying from about 20% to about 35% of the active ingredient.
In accordance with one embodiment of the present invention, the 25 monocrotophos formulation comprises at least about 5%, preferably from about 5% to
about 90% of one or more saccharides of the total formulation.
In accordance with another embodiment of the present invention, the monocrotophos formulation comprises from about 10% to about 40% of one or more saccharides of the total formulation.
30 In accordance with preferred embodiment of the present invention, the monocrotophos formulation comprises from about 20% to about 35% of one or more saccharides of the total formulation.

CHEM/MCP
In accordance with another preferred embodiment of the present invention, the monocrotophos formulation comprises about 30% of one or more saccharides of the total formulation.
In accordance with the present invention, the monocrotophos formulation comprises at least about 5% of monocrotophos of the desired activity and at least about 5% of one or more saccharides and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation. The percent amount referred is with reference to amount of the total formulation.
10 In accordance with one embodiment of the present invention, the monocrotophos formulation comprises monocrotophos of the desired activity in an amount varying from about 5% to about 70% of the total formulation and one or more saccharides in an amount varying from about 5% to about 90% of the total formulation and the balance being absorbent while taking
15 care that the amount of silica is restricted upto about 50% of the total formulation.
In accordance with one embodiment of the present invention, the
monocrotophos formulation comprises monocrotophos of the desired activity
in an amount varying from about 5% to about 70% of the total formulation
and one or more saccharides in an amount varying from about 10% to about
40% of the total formulation and the balance being absorbent while taking
care that the amount of silica is restricted upto about 50% of the total
formulation.
In accordance with one embodiment of the present invention, the
monocrotophos from about 5% to about 50% of the total formulation and one or more saccharides in an amount varying from about 20% to about 35% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total
30 formulation.
In accordance with one embodiment of the present invention, the monocrotophos formulation comprises monocrotophos of the desired activity

CHEM/MCP
in an amount varying from about 5% to about 50% of the total formulation and one or more saccharides in an amount of about 30% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation.
5 The amount of one or more saccharides as described herein is the amount of
all saccharides, if the formulation comprises more than one saccharides.

In accordance with one of the preferred embodiments of the present
invention, the monocrotophos formulation may additionally comprise one or
more auxiliaries selected from the group comprising surfactants, binding
agents, coating agents, or mixtures thereof in an amount so that the total
amount of these auxiliaries does not exceed more than about 10% of the
total formulation.
In accordance with another preferred embodiment of the present invention, the monocrotophos formulation may additionally comprise one or more additional active ingredient selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof in any amount, preferably in an amount so that the total amount of these additional active ingredients varies upto about 10% of the total formulation so that the desired activity of the monocrotophos is not suppressed.
20 In one embodiment, the present invention relates to a process for preparation of chemically stable monocrotophos formulation comprising absorbing weighed quantity of liquid monocrotophos on weight quantity of absorbent to result in formation of powder of monocrotophos followed by mixing the powder of monocrotophos with weighed quantity of one or more
25 of saccharides to form monocrotophos formulation which can be made available as chemically stable water soluble powder or chemically stable water dispersible powder.
In another embodiment, the present invention relates to a process for
preparation of chemically stable monocrotophos formulation comprising
absorbing weighed quantity of liquid monocrotophos on weight quantity of
absorbent to result in formation of powder of monocrotophos followed by
mixing the powder of monocrotophos with weighed quantity of one or more

CHEM/MCP
of saccharides to form monocrotophos formulation which is then mixed with
water to result in dough which is extruded through an extruder. On drying
the extrudates in a fluid bed drier, the present formulation can be made
available as chemically stable water soluble granules or chemically stable water dispersible granules.
It may be noted that the present formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible granules when the additional active ingredient is either insoluble or less soluble in water.
10 The homogeneous mixing of the ingredients while blending results in formation of homogeneous, chemically stable, water soluble powder or homogeneous, chemically stable, water dispersible powder form of the formulation. The mixing while granulating results in formation of chemically stable, water soluble granules or water dispersible granules.
15 In accordance with preferred embodiment of the present invention, one or more of auxiliaries and/or additional active ingredients may also be mixed in the monocrotophos formulation while formulating powder or granules of monocrotophos with one or more selected saccharides of the present invention.
20 The term granules, as employed herein, is intended to include solid pellets, granules, grains and the like. In accordance with present invention, the term granules, as employed herein, is intended to include a granule wherein monocrotophos forms core of the granule and the saccharide forms a coating over the core of the granule, and a granule wherein the saccharide forms
25 core of the granule and monocrotophos forms a coating over the core of the granule, and a granule wherein no such discrete core or coating is formed, that is, the granule having a substantially uniform composition.
The granules may have any particle size, preferably may have particle size varying from about 0.1mm or more, more preferably from about 0.1mm to about 2.0mm diameter.
The term chemically stable, as employed herein, means that the activity of the active ingredient does not fall more than 10%, preferably more than 7%

CHEM/MCP
of the originally selected activity of the active ingredient, and such drop in activity of the active ingredient is calculated after about 28 days in accelerated storage at about 54°C [ace storage] and after about one year at ambient storage.
5 The active ingredient referred herein is monocrotophos and the additional active ingredient referred herein is selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof.
It has been observed that drop in activity of the active ingredient of the
formulation in accordance with present invention is well within the limits,
that is less than 10% over a period of one year. The activity of the active
ingredient is checked by Bureau of Indian standards - IS specification no.
8025 : 1990.
It may be noted that the scope of the present invention is not restricted by the manner of mixing saccharides, other auxiliaries and additional active ingredients, which may be mixed in any manner.
The present invention is now described with the help of following experimental examples, which are illustrated in following tables wherein compositions of various formulations prepared in accordance with present invention have been disclosed.
20 Table no. 1 illustrates seven formulations prepared in accordance with present invention wherein the saccharide is either lactose monohydrate, or dextrose, or sucrose, or combination of lactose monohydrate and dextrose, or combination of lactose monohydrate and sucrose, or combination of dextrose and sucrose, or combination of lactose monohydrate, dextrose and
25 sucrose. The formula H illustrates a standard formulation prepared without saccharide disclosed in the present invention.
Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient
storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared

CHEM/MCP
without incorporating one or more of saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 75% water soluble matter.
Table no.: 1
Stability of MCP 30% SP using Lactose Monohydrate, Dextrose, Sucrose
and its combinations 10

Name of the ingredient Weight percentage
Formula. A Formula. B Formula. C Formula. D Formul E Formula. F Formula. G Formula. H
Monocrotophos Al in formulation 30% 30% 30% 30% 30% 30% 30% 30%
Monocrotophos tech (74% Al) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5%
Ppt Silica (Sypernat 22 S) 25% 25% 25% 25% 25% 25% 25% 25%
Lactose Monohydrate 29.5% 19.5% 19.5% - - - 10% -
Dextrose - 10% - 19.5% 29.5% - 10% -
Sucrose - - 10% 10% - 29.5% 9.5% -
Kaolin - - - - - - - 29.5%
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5%
Drop in Monocrotophos Al after 28 days ace storage 4% 4.2% 4.6% 4.9% 4.6% 5.1% 4.6% 11%
Drop in Monocrotophos AI after one year ambient storage 4% 4.4% 4.7% 5.0% 4.4% 5.3% 4 9% 12%
Water soluble matter 75% 75% 75% 75% 75% 75% 75% 45.5%

Table no. 2 illustrates formulations prepared in accordance with present
invention wherein the saccharide is lactose monohydrate and initial activity
of monocrotophos is increased from left to right side of the table. The formula H illustrates a standard formulation prepared without saccharide.
Each formulation was analyzed for drop in activity of active ingredient - monocrotophos [MCP] after 28 days ace storage and after one year ambient
storage. It was observed that the drop in activity of monocrotophos of all
formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 7% of the originally selected

CHEM/MCP
activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage.
Each formulation was also analyzed for water soluble matter and it was 5 observed that each formulation prepared in accordance with present
invention shows about 70 to 90% water soluble matter.
Table no. : 2
Stability of different concentrations of MCP AI with Lactose Monohydrate

Name of the ingredient Weight percentage
Formul A Formula. B Formula. C Formul. D Formula. E Formul F Formula. G Formula. H
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 35% 40% 50%
Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 47.30% 54.05% 67.57%
Ppt Silica (Sypernat 22 S) 10% 15% 20% 25% 25% 25% 30% 27.43%
Lactose Monohydrate 78.24% 66.46% 54.73% 42.98% 36.22% 22.70% 10.95% -
Dextrose - - - - - - - -
Sucrose - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5%
Drop in Monocrotophos AI after 28 days ace storage 0.70% 1.30% 2.10% 3.0% 3.9% 4.5% 5.8% 11%
Drop inMonocrotophosAI after oneyear ambientstorage 0.80% 1.40% 2.50% 3.2% 4.6% 4.7% 5.6% 12%
Water soluble matter 90% 85% 80% 75% 75% 75% 70% 72.50%
Table no. 3 illustrates formulations prepared in accordance with present
invention wherein the saccharide is lactose monohydrate and initial activity
of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide.
Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient
storage. It was observed that the drop in activity of monocrotophos of all
formulations prepared in accordance with present invention was well within
the desired value, that is, was less than about 10.1% of the originally selected activity of the active ingredient. However, the standard formulation

CHEM/MCP
prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 50 to 80% water soluble matter.
The formulations disclosed in Table 3 confirm that monocrotophos
formulations comprising lactose monohydrate within preferred range, that is
10 10% or more show better stability even after one year of storage and very
high water soluble matter.
Table no. : 3
Stability of MCP 30% AI with different concentrations of Lactose Monohydrate 15
Name of the ingredient Weight percentage
Formula. A Formula. B Formula. C Formula. D Formula. E Formula. F Formula. 0 Formul. H
Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30%
Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5%
Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34.5% 29.5% 24.5% 19.5% 54.5%
Lactose Monohydrate 5% 10% 15% 20% 25% 30% 35% -
Dextrose - - - - - - - -
Sucrose - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5%
Drop in Monocrotophos AI after 28 days ace storage 10.1% 8.9% 7.5% 6.2% 5.0% 4% 3.6% 11%
Drop in Monocrotophos AI after one year ambient storage 9.8% 8.8% 7.3% 6.3% 4.9% 4% 3.4% 12%
Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5%

Table no. 4 illustrates formulations prepared in accordance with present
invention wherein the saccharide is dextrose and initial activity of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide.
Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient

CHEM/MCP

storage. It was observed that the drop in activity of monocrotophos of all
formulations prepared in accordance with present invention was well within
the desired value, that is, was less than about 10.3% of the originally
selected activity of the active ingredient. However, the standard formulation
prepared without incorporating the one or more saccharides of the present
invention was 11% after 28 days ace storage and 12% after one year ambient
storage.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 50 to 80% water soluble matter.
The formulations disclosed in Table 4 also confirm that monocrotophos
formulations comprising dextrose within preferred range, that is 10%
or more show better stability even after one year of storage and very high water soluble matter.
Table no. : 4
Stability of MCP 30% AI with different concentrations of Dextrose

Name of the ingredient Weight percentage
Formul A Formul B Formul C Formula D FormulaE Formula F Formula G Formula H
Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30%
Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5%
Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34 5% 29.5% 24.5% 19.5% 54.5%
Lactose Monohydrate - - - - - - - -
Dextrose 5% 10% 15% 20% 25% 30% 35% -
Sucrose - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5%
Drop in Monocrotophos AI after 28 days ace storage 10.3% 9.2% 7.7% 6.5% 5.3% 4.4% 3.8% 11%
Drop in Monocrotophos AI after one year ambient storage 10.0% 9.1% 7.6% 6.5% 5.3% 4.3% 3.6% 12%
Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5%
Table no. 5 illustrates formulations prepared in accordance with present invention wherein the saccharide is sucrose and initial activity of monocrotophos is kept constant. The formula H illustrates a standard formulation prepared without saccharide.

CHEM/MCP
Each formulation was analyzed for drop in activity of active ingredient -monocrotophos [MCP] after 28 days ace storage and after one year ambient
storage. It was observed that the drop in activity of monocrotophos of all
formulations prepared in accordance with present invention was well within
the desired value, that is, was less than about 10.4% of the originally
selected activity of the active ingredient. However, the standard formulation
prepared without incorporating the one or more saccharides of the present
invention was 11% after 28 days ace storage and 12% after one year ambient
storage. Each formulation was also analyzed for water soluble matter and it
was observed that each formulation prepared in accordance with present
invention shows about 50 to 80% water soluble matter. The formulations
disclosed in Table 5 also confirm that monocrotophos formulations
comprising sucrose within preferred range, that is 10% or more show better
stability even after one year of storage and very high water soluble matter.
Table no. : 5
Stability of MCP 30% AI with different concentrations of Sucrose

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D FormulaE FormulaF Formula G Formula H
Monocrotophos AI in formulation 30% 30% 30% 30% 30% 30% 30% 30%
Monocrotophos tech (74% AI) 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5% 40.5%
Ppt Silica (Sypernat 22 S) 49.5% 44.5% 39.5% 34.5% 29.5% 24.5% 19.5% 54.5%
Lactose Monohydrate - - - - - - - -
Dextrose - - - - - - - -
Sucrose 5% 10% 15% 20% 25% 30% 35% -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5%
Drop in Monocrotophos AI after 28 days ace storage 10.4% 9.4% 7.8% 6.7% 5.5% 5% 4.1% 11%
Drop in Monocrotophos AI after one year ambient storage 10.1% 9.1% 7.7% 6.9% 5.7% 5.2% 3.8% 12%
Water soluble matter 50.5% 55.5% 60.5% 65.5% 70.5% 75.5% 80.5% 45.5%
Table no. 6 illustrates formulations prepared in accordance with present
invention wherein the saccharide is lactose monohydrate and initial activity
of monocrotophos is increased from left to right. The formulation I illustrates
a standard formulation prepared without saccharide. The formulations
illustrated in Table 6 also comprise one or more of fungicides described
hereinabove. Each formulation was analyzed for drop in activity of active

CHEM/MCP
ingredient - monocrotophos [MCP] after 28 days ace storage and after one
year ambient storage. It was observed that the drop in activity of
monocrotophos of all formulations prepared in accordance with present
invention was well within the preferred value, that is, was less than about
7% of the originally selected activity of the active ingredient. However, the
standard formulation prepared without incorporating the one or more
saccharides of the present invention was 11% after 28 days ace storage and
12% after one year ambient storage. Each formulation was also analyzed for
water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 35 to 70% water soluble
matter. The formulations disclosed in Table 6 also confirm that
monocrotophos formulations comprising lactose monohydrate within
preferred range, that is 10% or more show better stability even after one year
of storage and very high water soluble matter. The drop in water soluble
matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, fungicide.
Table no.: 6
Stability of different cone, of MCP Al + different cone, of Fungicides Al with
Lactose Monohydrate

Name of the ingredient Weight percentage
Formul A Formula B Formula C Formula D Formul E Formula F Formula G Formul H Formul I
Monocrotophos Al in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (74% Al) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57%
Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 27.43%
Lactose Monohydrate 26.14% 24.65% 23.15% 16.66% 15.17% 13.72% 12.18% 10.69% -
Dextrose - - - - - - - - -
Sucrose - - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5%
Fungicide 42.1% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% -
Drop in Monocrotophos Al after 28 days ace storage 0.90% 1.60% 2.40% 3.20% 4.0% 4.4% 5.0% 6.5% 11%
Drop in Monocrotophos Al after one year ambient storage 1.0% 1.50% 2.60% 3.3% 3.9% 4.3% 5.1% 6.4% 12%
Water soluble matter 37.86% 43.16% 48.42% 48.68% 53.95% 59.22% 64.48% 69.74% 72.57%
Table no. 7 illustrates formulations prepared in accordance with present invention wherein the saccharide is lactose monohydrate and initial activity of monocrotophos is increased from left to right. The formulation I illustrates

CHEM/MCP

a standard formulation prepared without saccharide. The formulations
illustrated in Table 7 also comprise one or more of additional active
ingredient - insecticides described hereinabove. Each formulation was
analyzed for drop in activity of active ingredient - monocrotophos [MCP] after
28 days ace storage and after one year ambient storage. It was observed that
the drop in activity of monocrotophos of all formulations prepared in
accordance with present invention was well within the preferred value, that
is, was less than about 7% of the originally selected activity of the active
ingredient. However, the standard formulation prepared without
10 incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 30 to 70% water soluble matter. The formulations disclosed in Table 7
15 also confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide.
20 Table no.: 7
Stability of different cone, of MCP AI + different cone, of insecticides AI with
Lactose Monohydrate

Name of the ingredient Weight percentage
Formul A Formula B Formul. C Formul D Formul E Formul F Formul G Formul H Formul I
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57%
Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 27.43%
Lactose Monohydrate 24.77% 23.45% 22.13% 15.81% 14.48% 13.21% 11.83% 10.52% -
Dextrose - - - - - - - - -
Sucrose - - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5%
Insecticide 43.47% 38.04% 32.60% 27.17% 21.74% 16.29% 10.87% 5.43% -
Drop inMonocrotophos AI after 28 days ace storage 0.80% 1.3% 2.1% 3.0% 4.0% 4.3% 4.9% 6.2% 11%
Drop inMonocrotophos AI after one year ambient storage 0.9% 1.50% 2.2% 3.1% 3.8% 4.2% 4.7% 6.0% 12%
Water soluble matter 33.53% 41.96% 47.4% 47.83% 53.26% 58.71% 64.13% 69.57% 72.57%

CHEM/MCP

Table no. 8 illustrates formulations prepared in accordance with present
invention wherein the saccharide is lactose monohydrate and initial activity
of monocrotophos is increased from left to right. The formulation I illustrates
a standard formulation prepared without saccharide. The formulations
illustrated in Table 8 also comprise one or more of additional active
ingredient - insecticides and auxiliaries - binding agent and coating agent
described hereinabove. Each formulation was analyzed for drop in activity of
active ingredient - monocrotophos [MCP] after 28 days ace storage and after
one year ambient storage. It was observed that the drop in activity of
10 monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and
15 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 30 to 70% water soluble matter. The formulations disclosed in Table 8 also confirm that monocrotophos formulations comprising lactose monohydrate within
20 preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide.
Table no.: 8
25 Stability of different cone, of MCP AI + different cone, of insecticides AI with
Lactose Monohydrate

Name of the ingredient Weight percenta ge
Formula A Formula B Formula C Formul D Formul E FormulaF Formula G Formula H Formula 1
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57%
Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 26.43%
Lactose Monohydrate 23.77% 22.45% 21.13% 14.81% 13.48% 12.21% 10.83% 9.52% -
Dextrose - - - - - - - - -
Sucrose - - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5%
Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Insecticide 43.47% 38.04% 32.60% 27.17% 21.74% 16.29% 10.87% 5.43% -
Fungicide - - - - - - - - -

CHEM/MCP

Drop inMonocrotophosAlafter 28 daysace storage 0.9% 1.2% 2.0% 2.9% 4.0% 4.5% 5.0% 5.8% 11%
Drop inMonocrotophosAlafter one yearambient storage 0.7 % 1.3% 2.2% 3.0% 3.9% 4.4% 5.2% 6.0% 12%
Water soluble matter 33.53% 41.96% 47.4% 47.83% 53.26% 58.71% 64.13% 69.57% 72.57%
Table no. 9 illustrates formulations prepared in accordance with present
invention wherein the saccharide is lactose monohydrate and initial activity
of monocrotophos is increased from left to right. The formulation I illustrates
a standard formulation prepared without saccharide. The formulations
illustrated in Table 9 also comprise one or more of additional active
ingredient - fungicides and auxiliaries - binding agent and coating agent
described hereinabove.
Each formulation was analyzed for drop in activity of active ingredient -
10 monocrotophos [MCP] after 28 days ace storage and after one year ambient storage. It was observed that the drop in activity of monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 7% of the originally selected activity of the active ingredient. However, the standard formulation prepared
15 without incorporating the one or more saccharides of the present invention was 11% after 28 days ace storage and 12% after one year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 35 to 70% water soluble matter. The formulations
20 disclosed in Table 9 also confirm that monocrotophos formulations comprising lactose monohydrate within preferred range, that is 10% or more show better stability even after one year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is,
25 fungicide.

CHEM/MCP
Table no.: 9
Stability of different cone, of MCP AI + different cone, of fungicide AI with
Lactose Monohydrate

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formul E Formula F Formula G Formula H Formul I
Monocrotophos Al in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (74% AI) 6.76% 13.51% 20.27% 27.02% 33.78% 40.50% 47.30% 54.05% 67.57%
Ppt Silica (Sypernat 22 S) 20% 20% 20% 25% 25% 25% 25% 25% 26.43%
Lactose Monohydrate 25.14% 23.65% 22.15% 15.66% 14.17% 12.72% 11.18% 9.69% -
Dextrose - - - - - - - - -
Sucrose - - - - - - - - -
Tysperse DN 5% 5% 5% 5% 5% 5% 5% 5% 5%
Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Fungicide 42.1% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% -
Drop inMonocrotophos AI after 28 days ace storage 1.0% 1.70% 2.30% 3.10% 40% 4.5% 5.2% 6.6% 11%
Drop inMonocrotophos AI after one year ambient storage 0.9% 1.50% 2.40% 3.0% 3.8% 4.6% 5.3% 6.4% 12%
Water soluble matter 37.86% 43.16% 48.42% 48.68% 53.95% 59.22% 64.48% 69.74% 72.57%

It may be noted various modifications are possible for the formulations
illustrated in the Tables provided herein without deviating from the intended
scope of present invention. Therefore, in one embodiment the present
invention includes all formulations which can be prepared without deviating
from its scope.
It may be noted that the term water soluble powder or granules as employed
herein means a formulation in which the active ingredient is fully dissolved
in spray solution despite the fact that the spray solution may contain a
certain amount of insoluble silica which is very low in the monocrotophos
15 formulation disclosed in the present invention and the term water
dispersible powder or granules means a formulation in which the active
ingredient is not fully dissolved in the final spray solution, but it is dispersed.
The amounts or volumes of various ingredients described herein and in the
20 Tables are with reference to the total weight or total volume of the
formulation and are taken in a way so as to have a total of 100%. These

CHEM/MCP
amounts may, however, vary within the permissible limits of practically allowable ranges of each ingredient of the present formulation.
The word "about" appearing before various values is intended to include practically permissible limits of variations in respective value.
5 Dated this 24th day of June, 2006.
[Dr. Ramesh kr. MEHTA]
Patent Attorney for the Applicants
10 Of Mehta & Mehta Associates

Documents:

1003-MUM-2006-ABSTRACT(5-9-2008).pdf

1003-mum-2006-abstract(complete)-(1-6-2007).pdf

1003-mum-2006-abstract(granted)-(9-7-2009).pdf

1003-MUM-2006-CLAIMS(5-9-2008).pdf

1003-MUM-2006-CLAIMS(CANCELLED PAGES)-(5-9-2008).pdf

1003-mum-2006-claims(complete)-(1-6-2007).pdf

1003-mum-2006-claims(granted)-(9-7-2009).pdf

1003-mum-2006-correspondance-recieved.pdf

1003-MUM-2006-CORRESPONDENCE(22-6-2010).pdf

1003-mum-2006-correspondence(24-8-2009).pdf

1003-MUM-2006-CORRESPONDENCE(25-6-2009).pdf

1003-MUM-2006-CORRESPONDENCE(5-9-2008).pdf

1003-mum-2006-correspondence(ipo)-(24-9-2009).pdf

1003-mum-2006-description (provisional).pdf

1003-mum-2006-description (provisional.doc

1003-mum-2006-description(complete)-(1-6-2007).pdf

1003-MUM-2006-DESCRIPTION(COMPLETE)-(5-9-2008).pdf

1003-mum-2006-description(granted)-(9-7-2009).pdf

1003-MUM-2006-DESCRIPTION(PROVISIONAL)-(27-6-2006).pdf

1003-mum-2006-form 1(1-6-2007).pdf

1003-mum-2006-form 1(1-6-2007)0012.pdf

1003-MUM-2006-FORM 1(27-6-2006).pdf

1003-mum-2006-form 18(9-10-2007).pdf

1003-mum-2006-form 2(5-9-2008).pdf

1003-mum-2006-form 2(complete)-(1-6-2007).pdf

1003-mum-2006-form 2(granted)-(9-7-2009).pdf

1003-MUM-2006-FORM 2(PROVISIONAL)-(27-6-2006).pdf

1003-MUM-2006-FORM 2(TITLE PAGE)-(5-9-2008).pdf

1003-mum-2006-form 2(title page)-(complete)-(1-6-2007).pdf

1003-mum-2006-form 2(title page)-(granted)-(9-7-2009).pdf

1003-MUM-2006-FORM 2(TITLE PAGE)-(PROVISIONAL)-(27-6-2006).pdf

1003-MUM-2006-FORM 26(27-6-2006).pdf

1003-mum-2006-form 3(1-6-2007).pdf

1003-MUM-2006-FORM 3(27-6-2006).pdf

1003-MUM-2006-FORM 3(5-9-2008).pdf

1003-mum-2006-form 5(1-6-2007).pdf

1003-MUM-2006-FORM 5(27-6-2006).pdf

1003-MUM-2006-FORM 5(5-9-2008).pdf

1003-mum-2006-form 9(26-6-2007).pdf

1003-mum-2006-form-1.pdf

1003-mum-2006-form-2.doc

1003-mum-2006-form-2.pdf

1003-mum-2006-form-26.pdf

1003-mum-2006-form-3.pdf

1003-mum-2006-form-5.pdf

1003-MUM-2006-REPLY TO FIRST EXAMINATION REPORT(5-9-2008).pdf

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Patent Number

235631

Indian Patent Application Number

1003/MUM/2006

PG Journal Number

30/2009

Publication Date

24-Jul-2009

Grant Date

09-Jul-2009

Date of Filing

27-Jun-2006

Name of Patentee

CHEMINOVA INDIA LTD.

Applicant Address

7th Floor,Keshava Building, Bandra-Kurla Complex, Bandra East, Mumbai-400051,

Inventors:

#	Inventor's Name	Inventor's Address
1	RAJNIKANT RAMJIBHAI PATEL	CHEMINOVA INDIA LTD. 7th Floor, Keshava Building, Bandra-KurlaComplex, Bandra East, MUMBAI-400051,

PCT International Classification Number

A61K31/00

PCT International Application Number

N/A

PCT International Filing date

PCT Conventions:

#	PCT Application Number	Date of Convention	Priority Country
1			NA