Title of Invention

A NOVEL FREE FLOWING SOLID COMPOSITION OF OILY, PUNGENT IRRITATING AND ODEROFEROUS SUBSTANCES AND PROCESS FOR THEIR PREPARATION

Abstract

The present invention relates to novel free flowing solid forms of oily pungent and odoriferous substances and a process for their preparation. The present invention, particularly relates to novel free flowing solid forms of irritant, spicy, odoriferous, oily or pungent substances of plants and a process for their preparation. More particularly, the present invention relates to novel free flowing solid forms of capsicum/capsicum extract/capsaicin and process for their preparation. The novel free flowing solid forms of capsicum/ capsicum extract/capsaicin of the present invention are useful for formulating dry mixes, tablets, capsules, heaps, ointments, pastes, lotions, liniments, mouthwashes, and gargles. More particularly, the novel free flowing solid forms of Capsicum / capsicum extracts Capsaicin are useful in body weight reduction.

Full Text

FORM 2 THE PATENTS ACT 70 (Act 39 of 70) PROVISIONAL SPECIFICATION (Section 10) NOVEL FREE FLOWING SOLID FORMS OF OILY, PUNGENT IRRITATING AND ODORIFEROUS SUBSTANCES AND PROCESS FOR THEIR PREPARATION. OMNIACTIVE HEALTH TECHNOLOGIES PVT LTD Rajan House, Appasaheb Marathe Marg, Prabhadevi, Mumbai 400025. The Description Provides The Nature Of The Invention INTRODUCTION: The present invention relates to novel free flowing solid forms of oily pungent and odoriferous substances and a process for their preparation. The present invention , particularly relates to novel free flowing solid forms of irritant, spicy, odoriferous, oily or pungent substances of plants and a process for their preparation. More particularly, the present invention relates to novel free flowing solid forms of capsicum/ capsicum extract/capsaicin and process for their preparation . The novel free flowing solid forms of capsicum/ capsicum extract/capsaicin of the present invention are useful for formulating dry mixes, tablets, capsules, heaps, ointments, pastes, lotions, liniments, mouthwashes, and gargles. More particularly, the novel free flowing solid forms of Capsicum / capsicum extracts Capsaicin are useful in body weight reduction. PRIOR ART A number of spicy and odoriferous substances have been associated with nutritional and health related benefits. Red pepper and its concentrated extracts have been associated with reducing energy intake, enhancing energy expenditure and facilitating weight control. Mustard extracts and oils are a source of the powerful isothiocyanate group of anti-oxidants which potentially have strong immunity boosting and cancer chemo-preventive benefits. Turmeric extracts have been identified as a rich source of curcuminoids, and turmeric based essential oils with a wide range of anti-bacterial, antiinflammatory, and chemopreventive benefits. Mint oils have been known for their digestive function in certain systems of medicine. Fish oils are a rich source of the Omega -3 oils DHA(Docasohexanoic Acid) and EPA(Eicosapentanoic Acid) associated with eye/brain health and cardiovascular well-being respectively. Cinnamon extracts have potentially significant applications in anti-diabetic nutrition. Ginger extracts have strong anti-nausea and digestive benefits. A common characteristic of the materials exemplified above is their distinctive, intense aroma or odor profile, accompanied by a sensory experience on touching/tasting which majority of people would find difficult to deal with at high levels of concentration when used in industrial manufacturing related handling operations, or when using these in consumer applications as formulated products. A number of applications which require the incorporation of such odoriferous, oily or coloured substances to be used in fairly high levels, but the challenges in processing -where the impact of the aroma/sensory characteristics of the material create difficulties in industrial processing environments: spread of intense/unacceptable odor, discomfort of plant operators and material handling personnel, quarantine and change-over efforts, chances of cross contamination with other flavour neutral material are hazards which prevent the successful incorporation of such materials in a wider range of products than currently available. Similarly, direct exposure to the intense organoleptic/sensory features associated with such materials over an extended period of time reduces the effective compliance in consumption of appropriate and regular dosage by consumers who seek the beneficial effects of such extracts. While technologies exist in the pharmaceutical and flavouring industries for taste/odour masking, no effective solution has been found for addressing high volume industrial use of such odoriferous materials in dry delivery forms. A number of challenges are experienced by formulators and consumers while using such materials for nutritional applications. A few examples are given below to illustrate the point: a) Red pepper powder, capsicum extracts and encapsulated flavours using capsicum extracts are a well known source of standardized delivery of capsaicinoids, the pungent principle associated with cayenne/red pepper. These compounds are associated with reducing energy intake, enhancing energy expenditure and facilitating weight control. However, effective dosage forms require capsaicin levels of much greater than 10-20,000 Scoville Heat Units to be delivered to the consumer in a non-bulky form, and for that the products which need to be used as starting material in manufacturing systems are found at heat levels as high as 250,000-10,00,000 SHU. Such raw materials are at heat levels which are virtually impossible for any normal person to tolerate without a high level of protective gear, and complete isolation of the operating environment from other materials/locations. Direct exposure to capsicum extracts can cause intense burning with reddening and swelling of the skin, swelling of mucosal linings of the eyes/nose/mouth causing difficulties in breathing and swallowing. The discomfort associated with such exposure-depending upon the intensity of material in use-can extend from a few minutes to several hours. Ingestion of capsicum for dietary benefits is associated with dosages identified in studies at levels as high as 30-50,000 SHU per dose, or 100-200,000 SHU per day, over periods of several weeks. Considering that typical items of food such as hot sauces/chilli peppers(which themselves are an acquired taste which a wide segment of population finds difficult to deal with at an organoleptic level) have heat levels of only 5-10,000 SHU, and are items of periodic consumption, the likelihood is very low that a large number of people will accept, purchase, consume or tolerate such materials over extended periods of time . (b) Turmeric extracts contain a wide range of beneficial compounds includes curcuminoids, turmerone and other oils. However, turmeric extracts are difficult to use in formulation lines because of the intense coloring property which spreads across equipment/operators, and requires very high level of effort for cleaning. Turmeric extracts also have a strong turmeric odour which a large number of people consider as disagreeable. Turmeric extracts are usually found as powders or pastes in which the problem of spread is quite high. These are examples to illustrate the need for technologies which would simultaneously deal with: a. preventing the spread of disagreeable or uncomfortable odours, aromas, colours and sensory characteristics of nutritional and pharmaceutical substances prior to their use in formulation lines b. facilitating the development of active ingredient delivery forms which have significantly high loading to facilitate nutritionally relevant dosages c. enabling the use of such high concentration solid dosage forms in manufacturing lines d. enabling consumers to consume the active ingredients of materials without being seriously exposed to the associated disagreeable or uncomfortable odours, aromas, colours and sensory characteristics of such material at sufficiently high dosages on a regular basis through standardized formulated products . Such a need could be appropriately addressed by providing free flowing solid forms of oily and/or pungent and odoriferous substances characterized by: a. high bulk density to prevent the easy spread of active-ingredient containing material in the from of light/air borne particles or dust b. free flowing nature to ensure usage in manufacturing lines without causing line blockages or hold-ups c. Non oily forms of materials to ensure there is no spread of active materials such as taste/odour/colour across operating lines/operators or others handling the material including the consumer d. concentration of active materials with outer protective coatings which would prevent interactions with the operating environment, operators and potential consumers Oily products are converted in to solid powders by the process of microencapsulation with gums such as acacia, tragacanth, guar gum, and certain synthetic polymer. Simple dilution of oily products with solid carriers like colloidal silica, maltodextrin, is another method used for converting oily liquids in to free flowing solids. There are several limitations of these processes like high cost, low bulk density of the resulting solid, excessive dilution of the strength of oily products. However, these methods are not suitable for eliminating pungency and skin irritation of products such as capsicum. US Patent nos. 5676994 and 5882713 describe the process of converting oils in to solids using starch wherein the water immiscible materials such as oils are dispersed in starch at elevated temperature and emulsifying under the conditions of high turbulence. Upon drying these compositions yield solid compositions that can be used in foods and medicines. The main disadvantage of this method is the use of aqueous emulsification systems in which require high temperature and long duration for complete drying. Such procedure is not suitable for highly pungent, skin irritant product such as capsicum oleoresin. US patent application no 20030032562 provides biodegradable chemical compositions wherein oily substances are adsorbed onto particulate or granular starch. The limitations of such process are requirement of large quantities of adsorbing agent per unit volume of oil. Such applications are designed to suit the adsorption of oil in oil well industries. In industrial practice oily products are converted in to free flowing powder after dilution with solids such as colloidal silica and maltodextrin. The main drawback of such practices is low bulk density of resulting powder not suitable for applications such as tableting. Moreover, pungency/irritancy is not masked and therefore such products are not suitable for oral use. Other methods used in the industrial practice for converting oily substances in to powder are freeze drying and spray drying. In freeze drying, the oily product is homogenized using aqueous medium followed by freezing to below the eutectic temperature under low pressure. The water content is then eliminated under low pressure by sublimation with gentle heating, resulting in a free flowing powder. Drawback of such process is high cost and low volume operations. These techniques are not useful for products such as capsaicin. In another process the oily substances after homogenization in water are subjected to spray drying. The main disadvantage of such process being use of high temperature, low bulk density of the resultant powder and aqueous atmosphere in which many oily food ingredients are not stable. The dust generated during the processing causes unbearable irritation and pungency for the operators in the plant. Some oily and odoriferous products such as capsicum or capsaicin , mustard oil , onion oil etc are highly irritating to skin and mucous membrane and cause serious handling hazard during their conversion in to delivery forms such as tableting or capsulation. Currently there are no simple methods available to produce free flowing , solid forms of such products which will facilitate administration at doses adequate for nutritional & health benefits as well as overcoming the handling difficulties of such pungent/irritant substances during formulation and manufacture . In modern times, obesity is identified as cause of serious complications during diseases such as diabetes and myocardial infarction. Therefore, serious attention is being given for weight reduction. For this purpose various compounds are being used , To quote some examples hydroxy citric acid commonly known as garcinia, may be mentioned . In this context, the use of herbal / plant based products have gained importance because of their safety , availability and absence of after effects. In this connection, the importance of capsicum/capsaicin for their use as weight reducing agents is worth mentioning . However, due to intense pungency and skin irritation properties, oily and odoriferous products such as capsicum / capsicum extracts / capsaicin , mustard oil , turmeric , onions etc can not be easily converted in to dosage form such as tablets/capsules . The above products are extremely pungent and irritating to the skin and mucus membrane. Converting these products in to dosage forms such as tablets or capsule will be impractical. In addition , the operators working on the granulation or tablet compression machine can not tolerate the intense pungency arising out of the very fine dust particles of capsicum. Upon ingestion as oral supplement, these products cause intense abdominal pain even at low doses. Thus, it is practically not possible to use such products for administration at adequate doses Therefore, though the oily and odoriferous products such as capsicum / capsicum extract capsaicin , mustard oil , turmeric , onions etc & capsaicinoids are very useful for their use for administration at adequate doses the above drawbacks prevents their use for such purposes purpose. Due to the enhanced awareness of weight loss properties of capsicum / capsicum extract or capsaicinoids and to reduce the complications of excessive fat in diseases such as diabetes, there is a demand for drugs for weight reduction which are cheap, based on herbs and natural products and which have no side effects during their long and continuous use. Capsaicin or capsaicinoids are extracted from capsicum annum through solvent extraction process. It is commercially available up to 40% concentration in the form of oleoresin. The oleoresin is in the form of pungent, irritating semisolid, which can not be easily handled. OBJECTIVES OF THE PRESENT INVENTION : Therefore, the main objective of the present invention is to provide novel free flowing solid forms of oily, pungent, irritating odoriferous substances . Another objective of the present invention is to provide novel free flowing solid forms of oily, pungent, irritating odoriferous plant substances such as capsicum / capsicum extract / capsaicinoids / mustard / onion etc. . Still another objective of the present invention is to provide novel free flowing solid forms of oily, pungent, irritating odoriferous substances in the form of beadlets which can be formulated further as tablet or capsule or a sachet. The present invention has been developed based on the fact that certain hydrophilic polymeric substances can form a gel like substance in specific solvent systems and the oily, pungent, irritating odoriferous substances substances can easily be entrapped in to such gels. Upon drying, the gel forms a hard solid mass along with the oily, pungent, irritating odoriferous substances The resulting solid mass can be pulverized or granulated to suitable solid delivery form. Alternatively, the extract after entrapment in to the gel, the gel can be coated on an inert spherical pellet. The entrapment of the gel like structure reduces the pungency and irritation to a significant level. The pungency of the extract can be substantially masked by coating with a protective polymer. The protective polymer used for coating can additionally prevent gastric irritation upon oral administration. In this way it is possible to convert an oily, pungent, irritating odoriferous substances in to a free flowing solid powder which can then be conveniently used for the purpose of tableting or filling in to two-piece gelatin capsules or in to sachets. Accordingly the present invention provides a novel free flowing solid forms of oily pungent, irritating odoriferous substances which do not loose their earlier biological activities and which are useful for converting into tablets, capsules, blended powders, Heaps, ointments, pastes, lotions, liniments, mouthwashes, and gargles etc. According to the present invention there is provided a process for the preparation of the novel free flowing solid forms of oily pungent, irritating odoriferous substances which do not lose their earlier biological activities and which are useful for converting into tablets , capsules, blended powders, liquid-fill hard-gel capsules, ointments, pastes, lotions, liniments, mouthwashes, and gargles etc. which comprises (i) Mixing thoroughly the oily pungent, irritating odoriferous substances with a hydrophilic polymer and a non polar / polar solvent or a mixture thereof to form a gel and (ii) Passing hot air through the resulting gel to form a solid mass and then grinding the solid mass into powders According to another embodiment of the present invention there is provided another process for the preparation of the novel free flowing solid forms of oily pungent, irritating odoriferous substances which do not lose their inherent biological activity and which are useful for converting into tablets , capsules, blended powders, Heaps, ointments, pastes, lotions, liniments, mouthwashes, and gargles etc. which comprises (i) Mixing thoroughly the oily pungent, irritating odoriferous substances with a hydrophilic polymer and a non polar / polar solvent or their mixtures to form a gel (ii) coating the resulting gel on to non pareil seeds to form beadlets and if desired (iii) providing another protective polymeric coating to the resulting beadlets The oily, pungent, irritating odoriferous substances coming under the scope of the present invention includes capsicum , capsicum extract, capsaicinoids /ginger, paprika, black pepper, white pepper, extracts and essential oils of onion, garlic, mustard, horseradish , mint, peppermint, oils such as fish oil,.. The hydrophilic polymer used for forming the gel includes hydroxy propyl methyl cellulose, polyvinyl pyrrolidone, hydroxy propyl cellulose, polyethylene glycol, polypropylene glycol or their mixtures . In another preferred embodiment the solvent employed may be selected from Acetone, Hexane, Ethyl Acetate, Isopropyl Alcohol, Ethanol, Dichloromethane, Methanol, etc, more preferably form Acetone, Ethanol, Dichloromethane, Isopropyl alcohol, and more preferably Dichloro Methane and Isopropyl Alcohol. In a preferred embodiment of the present invention the polymer employed for preventing coating may be selected from Methyl Cellulose, Agar, Sodium Alginate, Hydroxy Propyl Methyl Cellulose, Hydroxy Propyl Cellulose, Microcrystalline Cellulose, Polyvinyl Pyrrolidone, Starch, Gum Arabic, Xanthan Gum, Polyethylene Glycols, preferably, Microcrystalline Cellulose, Hydroxy Propyl Cellulose, Methyl Cellulose, Hydroxy Propyl Methyl Cellulose, etc, more preferably, Hydroxy Propyl Methyl Cellulose. Methacrylates, Phthalate type polymers The ratio of polymer to solvent may be in the range of 0.1 to 10. The mixing of the solution of the polymer with the materials may be carried at a temperature in the range of 5 deg C to 60 deg C, preferably at the range of 15 to 45 deg C. The mixing may be done for a period of 10 min to 4 hrs , preferably from 30 min to 2 hrs. The spraying of hot air may be done at a temperature in the range of 15 to 60 deg C, preferably in the range of 20-50 deg C. The solid mass obtained may be converted into powder of suitable sizes such as 100-900 microns ADVANTAGES OF THE INVENTION 1. Provides free flowing, non-sticky powder form of oily, pungent, irritating odoriferous substances 2. Provides a suitable method of delivering oily, pungent, irritating odoriferous substances either as tablets or capsules. 3. Provides a dosage form of oily, pungent, irritating odoriferous substances which does not cause irritation/discomfort in the mouth, oesophagus or stomach 4. Provides a convenient delivery form for capsicum or capsaicin, useful as a medicine for weight loss. 5. Provides a solid form of oily, pungent, irritating odoriferous substances which is user-friendly and does not cause skin irritation or pungency during tableting or capsule-filling. 6. Protects the oily, pungent, irritating odoriferous substances from environmental factors such as light, oxygen & heat 7. Retains the volatile materials present in the oily, pungent, irritating odoriferous substances 12

Documents:

2083-MUM-2007-ABSTRACT(15-10-2008).pdf

2083-MUM-2007-CLAIMS(15-10-2008).pdf

2083-MUM-2007-CLAIMS(AMENDED)-(21-3-2012).pdf

2083-MUM-2007-CLAIMS(AMENDED)-(8-11-2012).pdf

2083-MUM-2007-CORRESPONDENCE(15-10-2008).pdf

2083-mum-2007-correspondence(16-10-2007).pdf

2083-MUM-2007-CORRESPONDENCE(30-3-2012).pdf

2083-mum-2007-correspondence-received.pdf

2083-mum-2007-description (provisional).pdf

2083-MUM-2007-DESCRIPTION(COMPLETE(15-10-2008).pdf

2083-MUM-2007-FORM 13(30-3-2012).pdf

2083-MUM-2007-FORM 18(15-10-2008).pdf

2083-mum-2007-form 2(15-10-2008).pdf

2083-MUM-2007-FORM 2(TITLE PAGE)-(15-10-2008).pdf

2083-MUM-2007-FORM 2(TITLE PAGE)-(21-3-2012).pdf

2083-MUM-2007-FORM 2(TITLE PAGE)-(8-11-2012).pdf

2083-MUM-2007-FORM 3(21-3-2012).pdf

2083-MUM-2007-FORM 5(15-10-2008).pdf

2083-mum-2007-form-1.pdf

2083-mum-2007-form-2.doc

2083-mum-2007-form-2.pdf

2083-MUM-2007-MARKED COPY(21-3-2012).pdf

2083-MUM-2007-REPLY TO EXAMINATION REPORT(21-3-2012).pdf

2083-MUM-2007-REPLY TO HEARING(8-11-2012).pdf

2083-MUM-2007-SPECIFICATION(AMENDED)-(21-3-2012).pdf

2083-MUM-2007-SPECIFICATION(AMENDED)-(8-11-2012).pdf

2083-MUM-2007-SPECIFICATION(MARKED COPY)-(8-11-2012).pdf