Title of Invention

STABLE MICROENCAPSULATED IODINE COMPOUNDS

Abstract ABSTRACT This invention relates to stable, microencapsulated iodine conpounds which are biocompatible and bioabsorbable iodine compounds. The iodine compounds have a coat of acid, heat and moisture resistant agents which are also biocompatible. The coated compounds are microencapsulated either simultaneously or subsequently. The ooating agents and the microencapsulating agents may be the same or different. The microencapsulated iodine compounds find use in fortifying salt particularly crystal salt. The encapsulated iodine compounds release iodine under acidic pH conditions.
Full Text

This invention relates to stable microencapsulated iodine compounds which are particularly but not exclusively useful in fortifying crystal salts with sustained release iodine compounds.
Fortification of pure and refined powder salt with iodine and iron is known and such fortified salts are available in the market. Iodisation of pure refined salt is relatively easy and the thus fortified refined salt has good stability and shelf life. This is due to the alkaline pH in the range of 8 of pure refined salt at which pH iodine compounds are stable and do not dissooiate into free iodine.
However, fortification of crystal salt is not easy and so far attempts to fortify crystal salt with iodine to produce stable fortified crystal salt have not been successful. Crystal salt is produced in salt pans by the evaporation of sea water using solar heat. Sea water contains salts of calcium and magnesium in addition to salts of sodium. During slow evaporation leading to crystallisation, a nucleus of calcium salts is formed first before sodium chloride crystals are deposited. Finally magnesium salts crystallise over the sodium chloride constituting the top most layer. Ideally, salt must be harvested before magnesium salt layer formation. But in actual practice and to increase the bulk of the final product, salt is harvested only after considerable magnesium salt deposition.

Magnesium salts are highly hygroscopic in nature and for this reason, commercially available crystal salt has higher moisture content. Presence of calcium and magnesium salts inorease the acidity of the crystal salt which has a lower pH than refined salt. It is established that iodine compounds dissociate under acidic pH and thus iodisation of crystal salt in the normal manner does not produoe a stable composition.
It is already established that mioronutrients like iron and iodine, necesary for health and growth can be supplimented through the use of iron and iodine fortified common salt. A very large section of our population, especially people belonging to the lower income group consume only crystal salt and not refined powder salt. Therefore it is possible to supply this essential micronutrient, iodine, to all sections of the society only if crystal salt is also fortified with iodine. We have already established that stable crystal salt fortified with iodine is difficult to produce and store due to the inherent contaminations, low pH and hygroscopic nature of crystal salt.
Microencapsulated iodine compounds are found to exhibit good stability and shelf life. They are also acid, heat and moisture resistant and do not dissociate under harsh environmental conditions. Microencapsulated iodine compounds are thus found ideal for iodising crystal salt at the salt pans or immediately after harvesting salt from the pans. This results in cost reduction and consequential affordability by the common man.

Microencapsulated iodine compounds of this invention have been developed with these objectives in view. Biocompatible and bioabsorbable iodine compounds are selected and microencapsulated with acid, heat and moisture resistant coating agents to increase their stability and to provide prolonged shelf life.
Iodine compounds, suitable for fortifying salts, must be biocompatible and bioabsorbable. Alkali and alkaline earth metal iodides and iodates are examples of such compounds. For example, sodium iodide, sodium iodate, potassium iodide, potassium iodate, calcium iodide and calcium iodate are some of the suitable iodine sources. The process of microencapsulating the above compounds with acid, heat and moisture resistant coat materials and the products obtained by such process are novel, though the coating techniques involved in this process are known in the art. Some of the coating techniques used in producing microencapsulated , iodine are listed herein below:
(1) SPRAY DRYING, SPRAY DEHYDRATION:
The process involves three steps.
(a) Preparation of the solute/dispersion/emulsion to be
processed.
(b) Homogenisation of the above and finally spraying
resulting in atomisation of the mass in the drying chamber. The
core material which has to be microencapsulated is dispersed into
a solution which contains the wall coating material and then
homogenised.

(c) The homogenised product is then sprayed into a drying chamber where heated air removes the solvent and the microencapsulated product settles below. Alternatively the core materials are taken in a homogeniser and the coat material dissolved in suitable solvent or melted if necessary and is sprayed onto the core materials to ensure uniform and proper microencapsulation. The solvent is removed by.proper temperature control and recovered if desired.
(2) AIR SUSPENSION COATING, FLUIDISBD BED COATING:
This is accomplished by suspending solid particles of the core material in an upward moving stream of air which may be heated or cooled. The wall coating material which may be in a molten state or dissolved in an evaporable solvent is atomised through nozzles into the chamber and deposits as a thin layer on the surface of the suspended core particles. The turbulence of the air column is sufficient to maintain the suspension of the coating particles allowing them to tumble and thereby become uniformly coated.
(3) EXTRUSION:
This involves forcing a core material dispersed in the wall material solution through a series of dies into a bath of the dehydrated liquid. Upon contacting the liquid, the coating material hardens to entrap the core material. The extruded filaments are separated from the fluid bath and dried.

(4) SPRAY COOLING, SPRAY CHILLING & SPRAY FREEZING:
This involves dispersing the oore material into the liquified wall ooating material and spraying through heated nozzles into a Drying Chamber where cool air is used to solidify the wall coating material which in the process encapsulates the core.
(5) CENTRIFUGAL EXTRUSION, MULTI-ORIFICE CENTRIFUGAL EXTRUSION:
This process consists of concentric feed tubes through which the coat material and the core material are pumped separately to the many nozzles mounted on the outer surface of the device. The entire device is attached to a rotating shaft suoh that the head rotates around its vertical axis. As the head rotates, the core material and the coating material are co-extruded through the concentric orifices of the nozzles as a Fluid "Rod" of the core sheethed in the coating material. Centrifugal force impels the rod outward, causing it to break into tiny particles, by the action of the surface tension, the coating material envelopes the core material, thus accomplishing encapsulation.
(6) ROTATIONAL SUSPENSION SEPARATION:
This process involves suspending the core partioles in a pure liquified coating material, then pouring the suspension through a rotating disc apparatus under such conditions that the excess liquid between the core particles separates into a film

thinner than the core particles diameters. The excess liquid is then atomised into very small particles which are separated from the product and recycled. The core particles leave the disc with the residual liquid still around them which forms ooating. The particles are hardened by chilling or drying.
(7) COACERVATION/PHASE SEPARATION, AQUEOUS AND NON-AQUEOUS PHASE SEPARATION:
In this process both the wall coating material and the core material are in the liquid phase. Coacervation involves the separation of a liquid phase of coating material and wrapping of that phase as a uniform layer around suspended core particles. Coacervation may be brought about when the surface energies of the core material and the coating material are adjusted by varying some parameters of the system such as temperature pH or composition. The coating material is then solidified by means of heat or cross-linking or solvent removal techniques. The microcapsules are usually collected by filtration or oentrifugation, washed with an appropriate solvent and subsequently dried. Coacervation may be divided into aqueous phase separation and non-aqueous phase separation. Aqueous phase separation requires hydrophilic coating and a water insoluble oore particle. In non-aqueous phase separation the coating is usually hydro-phobic and the core may be water »«i»Kl« nv usfpr imminaihie.

(8) INCLUSION COMPLEXION:
This process involves the forming of a complex of the core material with the coating material - for example, when Beta-cyclo-dextrin is used as a coating material, this molecule has a doughnut shaped structure with a hollow which enables it to form complexes with many flavours, colours and vitamins. The Beta-cyclo-dextrin molecule forms inolusion complexes with compounds that can fit dimensionally within its cavity.
(9) LIPOSOME ENTRAPMENT:
Liposomes are vesicles which are formed when films of phospho lipids are dispersed in aqueous media. Liposomes are selectively permeable to ions. These liposomes could be used to entrap core materials. Structurally there are three types of Liposomes Multi Lamellar vesicles, single compartment vesicles and macro vesicles.
(10) CO-CRYSTALISATION:
This process involves inclusion of the core materials or entrapment of the core materials into and in between crystals during the process of crystalisation - for example, when sucrose is spontaneously crystalised from super saturated solution, aggregates of crystals from 3 to 30 micro metres form which can entrap the core material. The co-crystalisation process involves

concentrating the syrup to the point of super saturation and adding the material to be encapsulated and nixing the syrup to induce nucleation and agglomeration.
(11) INTER FACIAL POLYMERISATION:
This prooess involves dissolving a hydrophobic polymerisable monomer in a hydrophobic core material. Then polymerisation of the monomer is induced. The polymer is insoluble in the hydrophobic core material and deposits as a wall around the core.
Prior to encapsulation, iodine compounds may be mixed with alkaline and alkaline earth metal carbonates and bicarbonates to maintain alkaline pH necessary for stability of iodine.
Known coating materials may be used to protect iodine compounds by making them heat, acid and moisture resistant. Wall coating materials, suitable for coating iodine are listed exhaustively herein after.
GUMS like gum copal, guargum, gum acacia, gum arabic, gum tragacanth, gum karaya.
ALGINATES like sodium alginate, carrageenan, agar, corn syrups.
CELLULOSES like carboxy methyl cellulose, carboxy methyl cellulose sodium, methyl cellulose, ethyl cellulose, acetyl cellulose, cellulose esters, and ethers, oellulose acetate butyl phthalate, cellulose nitrate, cellosolve.

WATER SOLUBLE RESINS such as poly vinyl pyrrolidone, hydroxy ethyl cellulose, hydroxy methyl cellulose, arablno galactan, poly vinyl alcohol, hydroxy propyl methyl cellulose.
WATER INSOLUBLE RESINS such as rosin, cellulose acetate, poly methyl acrylate.
ENTERIC RESINS such as shellac, cellulose acetate phthalate, cellulose acetate butyrate, cellulose acetate succinate, zein, danalac, poly anionic oellulose.
CARBOHYDRATES such as sugars for example sucrose, lactose, dextrose.
STARCHES AND MODIFIED STARCHES like carboxy methyl starch, pregelatinised starch, dextrin, dextrin white, malto dextrin.
PROTEINS like gelatin, soy protein, casein, gluten, albumin, sodium caseinate, calcium caseinate.
INORGANIC MATERIALS like calcium sulphate, silicates, clays, talc, zinc oxide, barium, sulphate, magnesium stearate, calcium stearate. Psyllum, husk and seeds.
LIPIDS like parafin, tristearin, 12hydroxy stearic acid, stearic acid, stearine, monoglycerides, diglycerides, hydrogenated fat, glycerol mono stearate, glycerol distrearate, bees wax, hardened oils, glyceryl tri-12 hydroxy stearate, glycerene, silicones, carnauba wax, spermaceti, Chinese castor

wax, bayberry, montan wax, decanoic acid, oleic acid, palmatic acid, myristic acid, lauric acid, lauryl alcohol, oleyl cetyl alcohol, cetyl alcohol, stearyl alcohol, cetostearyl alcohol, candillila wax, oeresin wax, micro crystaline wax, ozokerite wax, poly ethylene wax, castor oil, myristyl alochol, glyceryl stearates, glyceryl laurates, glyceryl palmitates, glyceryl myristates, ethyl palmitate and ethyl oleate.
LIPSOMES, Oleo resin, Cyclo dextrans.
ORGANIC PHASE SEPARATING SYSTEMS like styrene maleic acid-copolymers.
Poly DL lactic acid, N-substituted acrylamide, poly vinyl alcohol cyclic, borate ester complex, hydroxy apatite complex, sodium starch glycolate, titanium dioxide.
EMULSIFIERS such as span, tweens, polysorbates 20, 40, 60, 80, lecithin, soy lecithin, bentonite, micro crystaline cellulose.
BUFFERS like ethyl acetate, sodium acetate, sodium mono chloro acetate.
Stable microencapsulated iodine compounds according to this invention comprises biocompatible and bioabsorbable iodine compounds coated with and microencapsulated in at least one known biocompatible acid, heat and moisture resistant agents.

Biocompatible alkaline and alkaline earth metal carbonates may be added to the selected iodine compounds to maintain alkaline pH at which iodine is stable. At alkaline pH, iodine compounds remain stable and are not easily dissociated.
Buffers and emulsifiers disclosed in paragraphs ante' may also be added either to the coating compositions or to the iodine compounds. These agents must also be biocompatible and bioabsorbable. Coating medium and the encapsulating medium may be identical or different.
Crystal and refined salts may be fortified with the microencapsulated iodine compounds. Salts fortified with microencapsulated iodine compounds according to this invention do not discolour on keeping. Heating during conventional cooking does not dissociate and release the iodine compounds thereby preventing discolouration. Iodine compounds used for fortification dissociate only in the acid medium of the digestive system.


We Claim:
1. Stable microencapsulated iodine compounds comprising
biocompatible and bioabsorbable iodine compounds coated with and
microencapsulated in at least one known biocompatible acid, heat
and moisture resistant agents.
2. Stable microencapsulated iodine compounds as claimed in
claim 1 wherein the said iodine compounds oontain biocompatible
alkaline and alkaline earth metal carbonates to maintain an
alkaline pH.
3. Stable microencapsulated iodine compounds as claimed in
claims 1 and 2, wherein the said acid, heat and moisture
resistant agent contains known biocompatible buffers and
emulsifiers.
.4. Stable microencapsulated iodine compounds as claimed in any
of the abovementioned claims wherein the poating medium and the
microencapsulating medium are the same.
S. Stable microencapsulated iodine compounds substantially as herein described.


Documents:

1998-mas-1996 abstract duplicate.pdf

1998-mas-1996 abstract.pdf

1998-mas-1996 claims duplicate.pdf

1998-mas-1996 claims.pdf

1998-mas-1996 correspondence others.pdf

1998-mas-1996 correspondence po.pdf

1998-mas-1996 description (complete) duplicate.pdf

1998-mas-1996 description (complete).pdf

1998-mas-1996 form-1.pdf

1998-mas-1996 form-18.pdf

1998-mas-1996 form-26.pdf


Patent Number 222530
Indian Patent Application Number 1998/MAS/1996
PG Journal Number 47/2008
Publication Date 21-Nov-2008
Grant Date 14-Aug-2008
Date of Filing 12-Nov-1996
Name of Patentee K RAMU
Applicant Address 26 C MALONY ROAD, T.NAGAR, CHENNAI 600 017,
Inventors:
# Inventor's Name Inventor's Address
1 K RAMU 26 C MALONY ROAD, T.NAGAR, CHENNAI 600 017,
2 MALAVIKA VINOD KUMAR 100 ST. MARY'S ROAD, CHENNAI 600 018,
PCT International Classification Number A23L01/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA