WO2016147123A2 - A fortified edible salt composition - Google Patents

A fortified edible salt composition Download PDF

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Publication number
WO2016147123A2
WO2016147123A2 PCT/IB2016/051475 IB2016051475W WO2016147123A2 WO 2016147123 A2 WO2016147123 A2 WO 2016147123A2 IB 2016051475 W IB2016051475 W IB 2016051475W WO 2016147123 A2 WO2016147123 A2 WO 2016147123A2
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Prior art keywords
silica
iron
edible salt
iron complex
salt composition
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PCT/IB2016/051475
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French (fr)
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WO2016147123A8 (en
WO2016147123A3 (en
Inventor
Debabrata Rautaray
Prabhat Kumar PARIDA
Shivkant VERMA
Ashwini ANGAL
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Tata Chemicals Limited
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Publication of WO2016147123A2 publication Critical patent/WO2016147123A2/en
Publication of WO2016147123A8 publication Critical patent/WO2016147123A8/en
Publication of WO2016147123A3 publication Critical patent/WO2016147123A3/en

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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/40Table salts; Dietetic salt substitutes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements
    • A23L33/165Complexes or chelates

Definitions

  • the present disclosure provides a fortified edible salt composition and a process for preparing the same. Particularly, present disclosure provides an edible salt composition fortified with iron and iodine.
  • Iron and iodine are essential elements for the human body. Iron acts as a catalyst in the transport, storage and utilization of oxygen. Iron is found in hemoglobin, myoglobin, cytochrome and in other enzymes. Iodine is an essential component of thyroid hormones.
  • Iron deficiency (anemia) and iodine deficiency disorders often coexist and affects more than one third of the world's population in the developing as well as industrialized nations, with serious consequences on mental and physical development.
  • a food source fortified with iron and iodine can help to overcome such problems by ensuring a daily supply of these minerals.
  • Edible salt is an ideal food vehicle for such a fortification owing to its low cost and ubiquitous use.
  • Iron and iodine fortified common salt can be used for the treatment of iron and/or iodine deficiency disorders.
  • double fortification of salt with iron and iodine involves various problems.
  • One such problem is the instability of iodine i.e. when iron and iodine are added to the edible salt, iodine is converted to elemental iodine, which evaporates and thus, is rapidly lost. It is known that such problems can be overcome by encapsulating iron to create a physical barrier for the iodine source.
  • Figure 1 X-ray diffraction data clearly indicating stability of iron-EDTA even after adsorption on silica. No evidence of iron-silicate or iron oxide formation was observed.
  • FIG. 2 Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) analysis of Fe-EDTA adsorbed on silica sample.
  • TEM micrographs indicate adsorption of Fe-EDTA on silica surface and SAED pattern show amorphous nature of silica and some degree of crystallinity of iron EDTA on amorphous silica surface.
  • SAED selected area electron diffraction
  • a fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica is disclosed.
  • a process for preparing a fortified edible salt composition is also disclosed, the process comprising preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt.
  • the present disclosure provides a fortified edible salt composition.
  • an edible salt composition fortified with iron and iodine is disclosed.
  • a fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica is disclosed.
  • the iron complex is selected from the group consisting of sodium iron ethylene diamine tetraacetate, iron sulphate orthophosphoric acid, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
  • iron complex is sodium iron ethylene diamine tetraacetate (ferric sodium EDTA).
  • EDTA is a chelating ligand which is able to bind to most metal ions.
  • Ferric [Fe(III)] ion is strongly bound to three carboxyl oxygens and the two nitrogen atoms of the diamine bridge producing a stable bond. The sodium ion coordinates with the other carboxyl oxygen ion.
  • a representation of the structure is provided below.
  • the EDTA has excellent stability when added to food under food processing and storage conditions. Since the iron is strongly bound within the EDTA molecule, the stability constant of the ferric EDTA complex (iron complex) is greater than the other metals of biological significance indicating the strength of the bond. Such bond facilitates non-availability of iron molecule to catalyse the oxidation of fats and oils in food which in turn prevents production of undesirable flavours, odours and colours etc. Said iron complex is virtually tasteless, odourless and dissolves in water slowly. The bioavailability of iron from ferric sodium EDTA is most often compared to ferrous sulphate because ferrous sulphate is widely used for iron fortification.
  • the iron in ferric sodium EDTA is two to three times better absorbed and incorporated into red blood cells than the iron in ferrous sulphate. Under these conditions, the iron in ferric sodium EDTA can be said to be two to three times more bioavailable than the iron in ferrous sulphate. This improvement in bioavailability is due to ferric sodium EDTA which reduces the effect of the iron absorption inhibitor phytic acid.
  • weight ratio of the iron complex adsorbed on silica and the edible salt in the composition is in a range of 0.8 : 100 to 1.2 : 100.
  • silica acts as a carrier or complexing agent for iron complex and helps in slight masking of the color of the fortified edible salt composition.
  • silica also acts as free flow agent and when added with salt containing iodine, this increases the stability of both iodine and iron in the salt composition with no effect on food matrix (when made using the present salt composition).
  • Silica is food grade silica.
  • iron complex adsorbed on silica comprises iron complex and silica in a weight ratio between 4 : 1 to 9 : 1.
  • the source of iodine is selected from the group consisting potassium iodate, potassium iodide, sodium iodate and sodium iodide and mixtures thereof.
  • iron is present in a concentration between 800 to 1200 ppm in the edible salt composition.
  • iodine is present in a concentration between 15 to 40 ppm in the edible salt composition.
  • the present disclosure also provides a process of preparing said fortified edible salt composition.
  • the process comprises preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt.
  • the iron complex adsorbed on silica is prepared by adsorption of iron complex on silica wherein silica is synthesized in-situ.
  • the iron complex adsorbed on silica is prepared by a process comprising mixing chelating agent, iron salt and silicate solution to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
  • the iron complex adsorbed on silica is prepared by a process comprising preparing a solution of chelating agent (chelating solution), adding a silicate solution to the chelating solution, adding an iron salt to the solution obtained in the previous step to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
  • chelating solution chelating solution
  • silicate solution silicate solution
  • an iron salt added to the solution obtained in the previous step to facilitate formation of a solution having iron complex adsorbed on silica
  • precipitating the iron complex adsorbed on silica separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
  • the iron complex adsorbed on silica is prepared by a process comprising preparing a solution of chelating agent and iron salt, adding a silicate solution to the solution obtained in the previous step to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
  • iron salt is selected from the group consisting of ferric chloride, ferrous sulphate heptahydrate, ferrous sulfate monohydrate, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
  • precipitation of the iron complex adsorbed on silica is carried out by allowing the solution having iron complex adsorbed on silica to stand for a time period in a range of 30 mins to 3 hours at room temperature. Ethanol may be added to the solution to facilitate improved precipitation. Separation of the precipitate is carried out by known separation techniques including centrifugation and filtration. After separation of the precipitate comprising iron complex adsorbed on silica, washing and drying is carried out by known techniques. Said drying is carried out at a temperature in a range of 60 to 80 degree Celsius. By way of example, the precipitate is washed with chilled water and dried overnight at a temperature of 80 degree Celsius to obtain powder of iron complex adsorbed on silica.
  • the chelating agent is selected from the group consisting of ethylene diamine tetraacetate, orthophosphoric acid, ascorbic acid, fumaric acid, lactic acid, gluconic acid and mixtures thereof.
  • the silicate solution is a solution of food grade Si0 2 powder in sodium hydroxide.
  • the iron complex comprises iron chelated with the chelating agent.
  • iron complex adsorbed on silica is added to the edible salt by way of dry blending of the iron complex adsorbed on silica with the edible salt (iodised or uniodised) or by mixing the iron complex adsorbed on silica and iodine salt with aqueous solution of uniodised salt.
  • the iron complex adsorbed on silica is added to the edible salt in a weight ratio in a range of 0.8 : 100 to 1.2 : 100
  • 10 grams of iron complex adsorbed on silica is added to 1000 grams of edible salt to deliver 1000 ppm of iron in the edible salt composition.
  • the edible salt is iodized or non-iodized.
  • 500 ml of 1 M NaOH is taken and 185 g of di-sodium-EDTA is added to it.
  • the mixture is heated at 65 °C while stirring (chelating solution).
  • Another solution is prepared by taking 500 ml of 1 M NaOH with 50 g of food grade Si0 2 powder while stirring and heating at 65°C (called silicate solution). Gradually added silicate solution to chelating solution while stirring the whole mixture (the reaction temperature is maintained at 65 °C). Allowed the solution mixture to stand for 5 mins and the pH was identified.
  • the pH of the solution mixture is adjusted 7.5 by adding dilute HC1 solution. After adjusting the pH, stirring was continued and the solution mixture was allowed to stand for 15 mins and the temperature was maintained at 65 °C.
  • anhydrous ferric chloride 75g FeCl 3 in 250 ml of water was added into the above solution mixture.
  • the pH of the solution pH -1.0 was determined and the solution was slowly brought down to room temperature. Once room temperature is achieved, 200 ml of ethanol was added into this solution mixture to facilitate better precipitation. The solution was allowed to stand for a period of 30 mins to facilitate precipitation. Thereafter, filtered and washed the precipitate with chilled water and dried overnight at 80°C to obtain iron complex adsorbed on silica (silica- Fe-EDTA) powder.
  • the powder obtained was characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of Fe-EDTA and silica.
  • XRD X-ray diffraction
  • TEM Transmission electron microscopy
  • ICP inductively coupled plasma
  • the powder obtained was characterized by X-ray diffraction (XRD), TEM, Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of FeEDTA and silica.
  • anhydrous ferric chloride 75g FeCl 3 in 250 ml of water
  • the pH of the solution pH ⁇ 3 to 4
  • the solution was slowly brought down to room temperature. Once room temperature is achieved, the solution was allowed to stand for a period of 30 mins to facilitate precipitation. Thereafter, filtered and washed the precipitate with chilled water and dried overnight at 80°C to obtain iron complex adsorbed on silica (silica-Fe-EDTA) powder.
  • the powder obtained was characterized by X-ray diffraction (XRD), , ⁇ , Electron Diffraction, inductively coupled plasma (ICP) method, thermo gravimetric analysis (TGA) and quantitative spectrophotometric method for determination of FeEDTA and silica.
  • the powder obtained was characterized by X-ray diffraction (XRD), TEM, Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of FeEDTA and silica.
  • the pellet from the centrifuge was dried in an oven at 60°C for 12 hrs. Ground the dry powder obtained using a kitchen grinder.
  • the silica- iron complex powder obtained was characterized by X-ray diffraction (XRD), and inductively coupled plasma (ICP) method.
  • Iodised salt is used for dry blending Fe-EDTA adsorbed on silica (silica Fe-EDTA complex) to make double fortified salt
  • silica silica
  • silica silica
  • iodised salt 30-40 ppm iodine
  • Salt formed is off-white in color.
  • the double fortified salt formulation (with iodine and iron) is then routinely analyzed for iodine and iron concentration though ICP-MS and titration methods. The stability of iodine in the presence of iron formulation was measured over time.
  • composition 2 Uniodised salt is used for dry blending silica Fe-EDTA complex to make double fortified salt
  • first potassium iodate (KI0 3 ) of 15-30 ppm was blended in salt prior to blending with silica Fe-EDTA complex.
  • the formulation contains 80% FeEDTA, 20% food grade silica where 10 g of silica Fe-EDTA complex when added to 1 kg of iodised salt delivers 1000 ppm of iron. Salt formed is off-white in color.
  • the double fortified salt formulation (with iodine and iron) is then routinely analyzed for iodine and iron concentration though ICP-MS and titration methods. The stability of iodine in the presence of iron formulation is measured over time.
  • composition 3 Mixing of silica Fe-EDTA complex with edible salt
  • Super saturated aqueous solution of uniodised salt (358 g per liter) was prepared. 30 to 40 ppm of KIO 3 and 8 g of Silica-FeEDTA complex was added in to the above super saturated salt solution (silica Fe-EDTA complex is added in a way to deliver 1000 ppm of iron in the salt).
  • the solution was mixed well before evaporating the solution mixture under vacuum by applying heat at 80° C with a pressure of 65 milibar while continuously stirring in a rota vapour (Buchi, rota vapour R-210). After achieving moisture level of 10% w/w (wet cake), transferred the wet cake to a vacuum oven and dried at 80° C for 4 hrs to obtain dry powder.
  • Example 8 Effect of fortified edible salt composition of the present disclosure vis-a-vis commercially available iodised salt on food matrix
  • a fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica.
  • composition(s), wherein weight ratio of the iron complex adsorbed on silica and the edible salt is in a range of 0.8 : 100 to 1.2 : 100.
  • composition(s), wherein iron complex adsorbed on silica comprises iron complex and silica in a weight ratio between 4 : 1 to 9 : 1.
  • composition(s), wherein the iron complex is selected from the group consisting of sodium iron ethylene diamine tetraacetate, iron sulphate orthophosphoric acid, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
  • composition(s), wherein the source of iodine is selected from the group consisting potassium iodate, potassium iodide, sodium iodate and sodium iodide and mixtures thereof.
  • a process for preparing a fortified edible salt composition comprising preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt.
  • Such process(s), wherein the iron complex comprises iron chelated with a chelating agent.
  • Such process(s), wherein the edible salt is iodized or non-iodized.
  • Such process(s), wherein the iron complex adsorbed on silica is prepared by a process comprising mixing chelating agent, iron salt and silicate solution to facilitate formation of a solution having iron complex adsorbed on silica, precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
  • chelating agent is selected from the group consisting of ethylene diamine tetraacetate, orthophosphoric acid, ascorbic acid, fumaric acid, lactic acid, gluconic acid and mixtures thereof.
  • silicate solution is a solution of food grade Si0 2 powder in sodium hydroxide.
  • iron salt is selected from the group consisting of ferric chloride, ferrous sulphate heptahydrate, ferrous sulfate monohydrate, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
  • the disclosed fortified edible salt composition is double fortified with iodine and iron, wherein iron is in a form of iron complex adsorbed on silica. Both iron and iodine in said composition are highly stable thereby attributing to long shelf life.
  • the fortified edible salt composition is inexpensive and has good sensorial properties.
  • the process for preparing said fortified edible salt composition is easy to perform and economical.

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Abstract

A fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica is disclosed. A process for preparing a fortified edible salt composition is also disclosed, the process comprising preparing an iron complex adsorbed 5 on silica; and adding the iron complex adsorbed on silica to the edible salt.

Description

A FORTIFIED EDIBLE SALT COMPOSITION
The present disclosure provides a fortified edible salt composition and a process for preparing the same. Particularly, present disclosure provides an edible salt composition fortified with iron and iodine.
BACKGROUND
Iron and iodine are essential elements for the human body. Iron acts as a catalyst in the transport, storage and utilization of oxygen. Iron is found in hemoglobin, myoglobin, cytochrome and in other enzymes. Iodine is an essential component of thyroid hormones.
Iron deficiency (anemia) and iodine deficiency disorders often coexist and affects more than one third of the world's population in the developing as well as industrialized nations, with serious consequences on mental and physical development. A food source fortified with iron and iodine can help to overcome such problems by ensuring a daily supply of these minerals.
Edible salt is an ideal food vehicle for such a fortification owing to its low cost and ubiquitous use. Iron and iodine fortified common salt can be used for the treatment of iron and/or iodine deficiency disorders. However, double fortification of salt with iron and iodine involves various problems. One such problem is the instability of iodine i.e. when iron and iodine are added to the edible salt, iodine is converted to elemental iodine, which evaporates and thus, is rapidly lost. It is known that such problems can be overcome by encapsulating iron to create a physical barrier for the iodine source.
Many encapsulation formulations developed so far are expensive and hence the price of double fortified salt is significantly higher and unlikely reaching the customers intended i.e lower income groups where both iron and iodine deficiency disorders are common. Further, the stability of both iron and iodine in such formulations is not very promising when it comes to long term storage. Such formulations also do not have good sensorial properties when added to many food matrixes.
Therefore, there is a need for an inexpensive fortified edible salt composition which has improved iron and iodine stability for long term storage. Further, there is a need for a simple process for preparing such a composition.
BRIEF DESCRIPTION OF DRAWINGS
Figure 1: X-ray diffraction data clearly indicating stability of iron-EDTA even after adsorption on silica. No evidence of iron-silicate or iron oxide formation was observed.
Figure 2: Transmission electron microscopy (TEM) and selected area electron diffraction (SAED) analysis of Fe-EDTA adsorbed on silica sample. TEM micrographs indicate adsorption of Fe-EDTA on silica surface and SAED pattern show amorphous nature of silica and some degree of crystallinity of iron EDTA on amorphous silica surface. SUMMARY
A fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica is disclosed. A process for preparing a fortified edible salt composition is also disclosed, the process comprising preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt. DETAILED DESCRIPTION
For the purpose of promoting an understanding of the principles of the invention, reference will now be made to embodiments and specific language will be used to describe the same. It will nevertheless be understood that no limitation of the scope of the invention is thereby intended, such alterations and further modifications in the disclosed process and system, and such further applications of the principles of the invention therein being contemplated as would normally occur to one skilled in the art to which the invention relates.
It will be understood by those skilled in the art that the foregoing general description and the following detailed description are exemplary and explanatory of the invention and are not intended to be restrictive thereof.
Reference throughout this specification to "one embodiment" "an embodiment" or similar language means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment of the present invention. Thus, appearances of the phrase "in one embodiment", "in an embodiment" and similar language throughout this specification may, but do not necessarily, all refer to the same embodiment.
The present disclosure provides a fortified edible salt composition. Particularly, an edible salt composition fortified with iron and iodine is disclosed. More particularly, a fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica is disclosed.
In accordance with an embodiment, the iron complex is selected from the group consisting of sodium iron ethylene diamine tetraacetate, iron sulphate orthophosphoric acid, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof. By way of specific example, iron complex is sodium iron ethylene diamine tetraacetate (ferric sodium EDTA). EDTA is a chelating ligand which is able to bind to most metal ions. Ferric [Fe(III)] ion is strongly bound to three carboxyl oxygens and the two nitrogen atoms of the diamine bridge producing a stable bond. The sodium ion coordinates with the other carboxyl oxygen ion. A representation of the structure is provided below.
Figure imgf000005_0001
EDTA has excellent stability when added to food under food processing and storage conditions. Since the iron is strongly bound within the EDTA molecule, the stability constant of the ferric EDTA complex (iron complex) is greater than the other metals of biological significance indicating the strength of the bond. Such bond facilitates non-availability of iron molecule to catalyse the oxidation of fats and oils in food which in turn prevents production of undesirable flavours, odours and colours etc. Said iron complex is virtually tasteless, odourless and dissolves in water slowly. The bioavailability of iron from ferric sodium EDTA is most often compared to ferrous sulphate because ferrous sulphate is widely used for iron fortification. Under test conditions where test meals are high in phytic acid (a potent inhibitor of iron absorption), the iron in ferric sodium EDTA is two to three times better absorbed and incorporated into red blood cells than the iron in ferrous sulphate. Under these conditions, the iron in ferric sodium EDTA can be said to be two to three times more bioavailable than the iron in ferrous sulphate. This improvement in bioavailability is due to ferric sodium EDTA which reduces the effect of the iron absorption inhibitor phytic acid.
In accordance with an embodiment, weight ratio of the iron complex adsorbed on silica and the edible salt in the composition is in a range of 0.8 : 100 to 1.2 : 100. In iron complex adsorbed on silica, silica acts as a carrier or complexing agent for iron complex and helps in slight masking of the color of the fortified edible salt composition. Further, silica also acts as free flow agent and when added with salt containing iodine, this increases the stability of both iodine and iron in the salt composition with no effect on food matrix (when made using the present salt composition). Silica is food grade silica.
In accordance with an embodiment, iron complex adsorbed on silica comprises iron complex and silica in a weight ratio between 4 : 1 to 9 : 1.
In accordance with an embodiment, the source of iodine is selected from the group consisting potassium iodate, potassium iodide, sodium iodate and sodium iodide and mixtures thereof.
In accordance with an embodiment, iron is present in a concentration between 800 to 1200 ppm in the edible salt composition.
In accordance with an embodiment, iodine is present in a concentration between 15 to 40 ppm in the edible salt composition.
The present disclosure also provides a process of preparing said fortified edible salt composition. The process comprises preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt.
In accordance with an embodiment, the iron complex adsorbed on silica is prepared by adsorption of iron complex on silica wherein silica is synthesized in-situ. The iron complex adsorbed on silica is prepared by a process comprising mixing chelating agent, iron salt and silicate solution to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
In accordance with an embodiment, the iron complex adsorbed on silica is prepared by a process comprising preparing a solution of chelating agent (chelating solution), adding a silicate solution to the chelating solution, adding an iron salt to the solution obtained in the previous step to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
In accordance with an alternate embodiment, the iron complex adsorbed on silica is prepared by a process comprising preparing a solution of chelating agent and iron salt, adding a silicate solution to the solution obtained in the previous step to facilitate formation of a solution having iron complex adsorbed on silica; precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
In accordance with an embodiment, iron salt is selected from the group consisting of ferric chloride, ferrous sulphate heptahydrate, ferrous sulfate monohydrate, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
In accordance with an embodiment, precipitation of the iron complex adsorbed on silica is carried out by allowing the solution having iron complex adsorbed on silica to stand for a time period in a range of 30 mins to 3 hours at room temperature. Ethanol may be added to the solution to facilitate improved precipitation. Separation of the precipitate is carried out by known separation techniques including centrifugation and filtration. After separation of the precipitate comprising iron complex adsorbed on silica, washing and drying is carried out by known techniques. Said drying is carried out at a temperature in a range of 60 to 80 degree Celsius. By way of example, the precipitate is washed with chilled water and dried overnight at a temperature of 80 degree Celsius to obtain powder of iron complex adsorbed on silica. In accordance with an embodiment, the chelating agent is selected from the group consisting of ethylene diamine tetraacetate, orthophosphoric acid, ascorbic acid, fumaric acid, lactic acid, gluconic acid and mixtures thereof.
In accordance with an embodiment, the silicate solution is a solution of food grade Si02 powder in sodium hydroxide.
In accordance with an embodiment, the iron complex comprises iron chelated with the chelating agent.
In accordance with an embodiment, iron complex adsorbed on silica is added to the edible salt by way of dry blending of the iron complex adsorbed on silica with the edible salt (iodised or uniodised) or by mixing the iron complex adsorbed on silica and iodine salt with aqueous solution of uniodised salt.
In accordance with an embodiment, the iron complex adsorbed on silica is added to the edible salt in a weight ratio in a range of 0.8 : 100 to 1.2 : 100 By way of example, 10 grams of iron complex adsorbed on silica is added to 1000 grams of edible salt to deliver 1000 ppm of iron in the edible salt composition. The edible salt is iodized or non-iodized.
The following example(s) should not be understood to be in any way limiting.
Preparation of iron complex adsorbed on silica
Example 1:
500 ml of 1 M NaOH is taken and 185 g of di-sodium-EDTA is added to it. The mixture is heated at 65 °C while stirring (chelating solution). Another solution is prepared by taking 500 ml of 1 M NaOH with 50 g of food grade Si02 powder while stirring and heating at 65°C (called silicate solution). Gradually added silicate solution to chelating solution while stirring the whole mixture (the reaction temperature is maintained at 65 °C). Allowed the solution mixture to stand for 5 mins and the pH was identified. The pH of the solution mixture is adjusted 7.5 by adding dilute HC1 solution. After adjusting the pH, stirring was continued and the solution mixture was allowed to stand for 15 mins and the temperature was maintained at 65 °C. Thereafter, anhydrous ferric chloride (75g FeCl3 in 250 ml of water) was added into the above solution mixture. The pH of the solution (pH -1.0) was determined and the solution was slowly brought down to room temperature. Once room temperature is achieved, 200 ml of ethanol was added into this solution mixture to facilitate better precipitation. The solution was allowed to stand for a period of 30 mins to facilitate precipitation. Thereafter, filtered and washed the precipitate with chilled water and dried overnight at 80°C to obtain iron complex adsorbed on silica (silica- Fe-EDTA) powder.
The powder obtained was characterized by X-ray diffraction (XRD), Transmission electron microscopy (TEM), Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of Fe-EDTA and silica.
Example 2:
500 ml of 1 M NaOH is taken and 185 g of di-sodium-EDTA is added to it. The mixture is heated at 65 °C while stirring (chelating solution). Another solution is prepared by taking 500 ml of 1 M NaOH with 50 g of food grade Si02 powder while stirring and heating at 65°C (called silicate solution). Gradually added silicate solution to chelating solution while stirring the whole mixture (the reaction temperature is maintained at 65 °C). Allowed the solution mixture to stand for 5 mins and the pH was identified. Thereafter, anhydrous ferric chloride (75g FeCl3 in 250 ml of water) was added into the above solution mixture. The pH of the solution (pH ~3 to 4) was determined and the solution was slowly brought down to room temperature. Once room temperature is achieved, 200 ml of ethanol was added into this solution mixture to facilitate better precipitation. The solution was allowed to stand for a period of 30 mins to facilitate precipitation. Thereafter, filtered and washed the precipitate with chilled water and dried overnight at 80°C to obtain iron complex adsorbed on silica (silica-Fe-EDTA) powder.
The powder obtained was characterized by X-ray diffraction (XRD), TEM, Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of FeEDTA and silica.
Example 3:
1000 ml of 1 M NaOH is taken and 185 g of di-sodium-EDTA is added to it. The mixture is heated at 65 °C while stirring (chelating solution). Another solution is prepared by taking 500 ml of 1 M NaOH with 50 g of food grade Si02 powder while stirring and heating at 65 °C (called silicate solution). To form acidic silica sol, 250 ml (20 % HC1) was added to the silicate solution with vigorous stirring. Then gradually added acidic silica sol to chelating solution while stirring (the reaction temperature is maintained at 65 °C). The solution mixture was allowed to stand for 5 mins and the pH was determined. Thereafter, added anhydrous ferric chloride (75g FeCl3 in 250 ml of water) into the above solution mixture. The pH of the solution (pH ~3 to 4) was determined and the solution was slowly brought down to room temperature. Once room temperature is achieved, the solution was allowed to stand for a period of 30 mins to facilitate precipitation. Thereafter, filtered and washed the precipitate with chilled water and dried overnight at 80°C to obtain iron complex adsorbed on silica (silica-Fe-EDTA) powder.
The powder obtained was characterized by X-ray diffraction (XRD), ,ΤΕΜ, Electron Diffraction, inductively coupled plasma (ICP) method, thermo gravimetric analysis (TGA) and quantitative spectrophotometric method for determination of FeEDTA and silica.
Example 4:
500 ml of 1 M NaOH is taken and 185 g of di-sodium-EDTA is added to it. The mixture is heated at 65 °C while stirring (chelating solution). Another solution is prepared by taking 500 ml of 1 M NaOH with 50 g of food grade Si02 powder while stirring and heating at 65°C (called silicate solution). Gradually added silicate solution to chelating solution while stirring the whole mixture (the reaction temperature is maintained at 65 °C). Allowed the solution mixture to stand for 5 mins. Thereafter, anhydrous ferric chloride (75g FeCl3 in 250 ml of water) was added into the above solution mixture. If the pH of the above solution did not reach pH -2.0, continue adding more FeCl3 solution to reach a level of pH~2. The temperature of the solution was slowly brought down to room temperature for precipitation to happen over a period of 1 hour. Thereafter, filtered the precipitate and the precipitate was washed with chilled water and dried overnight at 80°C to obtain silica- Fe-EDTA powder.
The powder obtained was characterized by X-ray diffraction (XRD), TEM, Electron Diffraction, inductively coupled plasma (ICP) method, and quantitative spectrophotometric method for determination of FeEDTA and silica.
Example 5
100 ml of 0.5 M ortho -phosphoric acid (H3P04) was taken in a 1 liter beaker and 20 g of ferrous sulfate heptahydrate (FeS04.7H20) was added slowly while stirring using magnetic stirrer. Added sodium silicate (7% Si02 with pH value of -13) to the above solution until pH 7 was achieved. The above solution was stirred for 1 hr to facilitate precipitation. The precipitated solution was centrifuged at 4000 rpm for 5 minutes. The supernatant was separated and solid cake collected after centrifugation. The cake was washed twice with distilled water while centrifuging at 4000 rpm for 5 minutes each time, to remove any free uncoordinated iron. The pellet from the centrifuge was dried in an oven at 60°C for 12 hrs. Ground the dry powder obtained using a kitchen grinder. The silica- iron complex powder obtained was characterized by X-ray diffraction (XRD), and inductively coupled plasma (ICP) method.
Figure imgf000012_0001
Figure imgf000012_0002
Preparation of Edible Salt Composition (with iron complex adsorbed on silica Example 1-4):
Example 6
Composition 1 Iodised salt is used for dry blending Fe-EDTA adsorbed on silica (silica Fe-EDTA complex) to make double fortified salt A formulation was developed with 80% FeEDTA, 20% food grade silica, where 10 g of silica Fe-EDTA complex was blended with 1 kg of iodised salt (30-40 ppm iodine) which delivers 1000 ppm of iron. Salt formed is off-white in color. The double fortified salt formulation (with iodine and iron) is then routinely analyzed for iodine and iron concentration though ICP-MS and titration methods. The stability of iodine in the presence of iron formulation was measured over time.
Composition 2 Uniodised salt is used for dry blending silica Fe-EDTA complex to make double fortified salt
When uniodised salt was used for double fortified salt formulation, first potassium iodate (KI03) of 15-30 ppm was blended in salt prior to blending with silica Fe-EDTA complex. The formulation contains 80% FeEDTA, 20% food grade silica where 10 g of silica Fe-EDTA complex when added to 1 kg of iodised salt delivers 1000 ppm of iron. Salt formed is off-white in color. The double fortified salt formulation (with iodine and iron) is then routinely analyzed for iodine and iron concentration though ICP-MS and titration methods. The stability of iodine in the presence of iron formulation is measured over time.
Composition 3 Mixing of silica Fe-EDTA complex with edible salt
Super saturated aqueous solution of uniodised salt (358 g per liter) was prepared. 30 to 40 ppm of KIO3 and 8 g of Silica-FeEDTA complex was added in to the above super saturated salt solution (silica Fe-EDTA complex is added in a way to deliver 1000 ppm of iron in the salt). The solution was mixed well before evaporating the solution mixture under vacuum by applying heat at 80° C with a pressure of 65 milibar while continuously stirring in a rota vapour (Buchi, rota vapour R-210). After achieving moisture level of 10% w/w (wet cake), transferred the wet cake to a vacuum oven and dried at 80° C for 4 hrs to obtain dry powder. The double fortified salt formulation (with iodine and iron) was then analyzed for iodine and iron concentration though ICP-MS and titration methods. The stability of iodine in the presence of iron formulation was measured over time. Example 7: Comparative experimental data regarding stability of iron and iodine in the edible salt (DFS: Double Fortified Salt)
Figure imgf000014_0002
Figure imgf000014_0001
Example 8: Effect of fortified edible salt composition of the present disclosure vis-a-vis commercially available iodised salt on food matrix
Figure imgf000015_0001
Iron fortification of iodised salt (based on example 5)
Take 1000 ppm iron (2.27 g of iron loaded silica by considering 22% iron loading onto silica) into an air tight container and pour 200 ppm ascorbic acid into it and mix well by hand for 10 minutes then add 500 gram iodized salt into and mix well for 10 minutes again. Iron and Iodine are found stable after three months.
Iron fortification of uniodised salt
Take 500 g of uniodised salt and add iron-iodine premix as prepared above (example 5). Mix them uniformly using a blender for 30 mins. The salt composition formed is white in color with L* scale of 90.94 (L*A*B value). The salt composition obtained is characterized by ICP-OES for iron estimation and ICP-MS for the determination of iodine. SPECIFIC EMBODIMENTS ARE DESCRIBED BELOW
A fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica.
Such composition(s), wherein weight ratio of the iron complex adsorbed on silica and the edible salt is in a range of 0.8 : 100 to 1.2 : 100.
Such composition(s), wherein iron complex adsorbed on silica comprises iron complex and silica in a weight ratio between 4 : 1 to 9 : 1.
Such composition(s), wherein the iron complex is selected from the group consisting of sodium iron ethylene diamine tetraacetate, iron sulphate orthophosphoric acid, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
Such composition(s), wherein the source of iodine is selected from the group consisting potassium iodate, potassium iodide, sodium iodate and sodium iodide and mixtures thereof.
Such composition(s), wherein iron is present in a concentration between 800 to 1200 ppm.
Such composition(s), wherein iodine is present in a concentration between 15 to 40 ppm.
FURTHER SPECIFIC EMBODIMENTS ARE DESCRIBED BELOW
A process for preparing a fortified edible salt composition comprising preparing an iron complex adsorbed on silica; and adding the iron complex adsorbed on silica to the edible salt.
Such process(s), wherein the iron complex comprises iron chelated with a chelating agent. Such process(s), wherein the edible salt is iodized or non-iodized.
Such process(s), wherein weight ratio of the iron complex adsorbed on silica and the edible salt is in a range of 0.8 : 100 to 1.2 : 100
Such process(s), wherein the iron complex adsorbed on silica is prepared by a process comprising mixing chelating agent, iron salt and silicate solution to facilitate formation of a solution having iron complex adsorbed on silica, precipitating the iron complex adsorbed on silica; separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
Such process(s), wherein the chelating agent is selected from the group consisting of ethylene diamine tetraacetate, orthophosphoric acid, ascorbic acid, fumaric acid, lactic acid, gluconic acid and mixtures thereof.
Such process(s), wherein the silicate solution is a solution of food grade Si02 powder in sodium hydroxide.
Such process(s), wherein iron salt is selected from the group consisting of ferric chloride, ferrous sulphate heptahydrate, ferrous sulfate monohydrate, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
Such process(s), wherein drying is carried out at a temperature in a range of 60 to 80 degree Celsius. INDUSTRIAL APPLICABILITY
The disclosed fortified edible salt composition is double fortified with iodine and iron, wherein iron is in a form of iron complex adsorbed on silica. Both iron and iodine in said composition are highly stable thereby attributing to long shelf life. The fortified edible salt composition is inexpensive and has good sensorial properties. The process for preparing said fortified edible salt composition is easy to perform and economical.

Claims

We Claim:
1. A fortified edible salt composition comprising a source of iodine, and an iron complex adsorbed on silica. 2. A fortified edible salt composition as claimed in claim 1, wherein weight ratio of the iron complex adsorbed on silica and the edible salt is in a range of 0.8: 100 to 1.
2: 100.
3. A fortified edible salt composition as claimed in claim 1, wherein iron complex adsorbed on silica comprises iron complex and silica in a weight ratio between 4 : l to 9 : 1.
4. A fortified edible salt composition as claimed in claim 1, wherein the iron complex is selected from the group consisting of sodium iron ethylene diamine tetraacetate, iron sulphate orthophosphoric acid, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
5. A fortified edible salt composition as claimed in claim 1, wherein the source of iodine is selected from the group consisting potassium iodate, potassium iodide, sodium iodate and sodium iodide and mixtures thereof.
6. A fortified edible salt composition as claimed in claim 1, wherein iron is present in a concentration between 800 to 1200 ppm.
7. A fortified edible salt composition as claimed in claim 1, wherein iodine is present in a concentration between 15 to 40 ppm.
8. A process for preparing a fortified edible salt composition comprising:
preparing an iron complex adsorbed on silica; and
adding the iron complex adsorbed on silica to the edible salt.
9. A process for preparing a fortified edible salt composition as claimed in claim 8, wherein the iron complex comprises iron chelated with a chelating agent.
10. A process as claimed in claim 8, wherein the edible salt is iodized or non-iodized.
11. A process for preparing a fortified edible salt composition as claimed in claim 8, wherein weight ratio of the iron complex adsorbed on silica and the edible salt is in a range of 0.8: 100 to 1.2: 100.
12. A process for preparing a fortified edible salt composition as claimed in claim 8 or 9, wherein the iron complex adsorbed on silica is prepared by a process comprising:
mixing chelating agent, iron salt and silicate solution to facilitate formation of a solution having iron complex adsorbed on silica;
precipitating the iron complex adsorbed on silica;
separating and drying the precipitate to obtain powder of iron complex adsorbed on silica.
13. A process for preparing a fortified edible salt composition as claimed in claim 12, wherein the chelating agent is selected from the group consisting of ethylene diamine tetraacetate, orthophosphoric acid, ascorbic acid, fumaric acid, lactic acid, gluconic acid and mixtures thereof. A process for preparing a fortified edible salt composition as claimed in claim 12, wherein the silicate solution is a solution of food grade Si02 powder in sodium hydroxide.
A process for preparing a fortified edible salt composition as claimed in claim 12, wherein iron salt is selected from the group consisting of ferric chloride, ferrous sulphate heptahydrate, ferrous sulfate monohydrate, ferrous ascorbate, ferrous fumarate, ferrous lactate, ferrous gluconate, ferric caseinate, ferric pyrophosphate, ferrous ammonium phosphate and mixtures thereof.
A process for preparing a fortified edible salt composition as claimed in claim 12, wherein drying is carried out at a temperature in a range of 60 to 80 degree Celsius.
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