WO2016147123A2 - Composition de sel comestible fortifié - Google Patents

Composition de sel comestible fortifié Download PDF

Info

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
Authority
WO
WIPO (PCT)
Prior art keywords
silica
iron
edible salt
iron complex
salt composition
Prior art date
Application number
PCT/IB2016/051475
Other languages
English (en)
Other versions
WO2016147123A8 (fr
WO2016147123A3 (fr
Inventor
Debabrata Rautaray
Prabhat Kumar PARIDA
Shivkant VERMA
Ashwini ANGAL
Original Assignee
Tata Chemicals Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Tata Chemicals Limited filed Critical Tata Chemicals Limited
Publication of WO2016147123A2 publication Critical patent/WO2016147123A2/fr
Publication of WO2016147123A8 publication Critical patent/WO2016147123A8/fr
Publication of WO2016147123A3 publication Critical patent/WO2016147123A3/fr

Links

Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16—Inorganic salts, minerals or trace elements
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/40—Table salts; Dietetic salt substitutes
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, 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
    • A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16—Inorganic salts, minerals or trace elements
    • A23L33/165—Complexes 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.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Mycology (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

Cette invention concerne une composition de sel comestible fortifié comprenant une source d'iode, et un complexe de fer adsorbé sur une silice. Un procédé de préparation d'une composition de sel comestible fortifié est en outre décrit, ledit procédé comprenant la préparation d'un complexe de fer adsorbé sur une silice ; et l'ajout du complexe de fer adsorbé sur la silice au sel comestible.
PCT/IB2016/051475 2015-03-19 2016-03-16 Composition de sel comestible fortifié WO2016147123A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IN911MU2015 2015-03-19
IN911/MUM/2015 2015-03-19

Publications (3)

Publication Number Publication Date
WO2016147123A2 true WO2016147123A2 (fr) 2016-09-22
WO2016147123A8 WO2016147123A8 (fr) 2016-11-24
WO2016147123A3 WO2016147123A3 (fr) 2017-01-05

Family

ID=56919127

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/IB2016/051475 WO2016147123A2 (fr) 2015-03-19 2016-03-16 Composition de sel comestible fortifié

Country Status (1)

Country Link
WO (1) WO2016147123A2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016199442A (ja) * 2015-04-13 2016-12-01 富田製薬株式会社 ピロリン酸第二鉄含有粉末及びその製造方法

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1996030A1 (fr) * 2006-03-21 2008-12-03 Akzo Nobel N.V. Sel doublement fortifie et son procede de preparation
WO2009074998A2 (fr) * 2007-09-11 2009-06-18 Tata Chemicals Limited Sel enrichi en fer

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016199442A (ja) * 2015-04-13 2016-12-01 富田製薬株式会社 ピロリン酸第二鉄含有粉末及びその製造方法

Also Published As

Publication number Publication date
WO2016147123A8 (fr) 2016-11-24
WO2016147123A3 (fr) 2017-01-05

Similar Documents

Publication Publication Date Title
Voegelin et al. Effect of phosphate, silicate, and Ca on Fe (III)-precipitates formed in aerated Fe (II)-and As (III)-containing water studied by X-ray absorption spectroscopy
Hu et al. Can epicatechin gallate increase Cr (VI) adsorption and reduction on ZIF-8?
Ibrahim et al. Synthesis of rod-like hydroxyapatite with high surface area and pore volume from eggshells for effective adsorption of aqueous Pb (II)
CN102795610B (zh) 无定形磷酸钙纳米球及其制备方法
De Kort et al. Calcium-binding capacity of organic and inorganic ortho-and polyphosphates
AU2012304583A1 (en) Micronutrient supplement
Santoro et al. Inorganic and organic P retention by coprecipitation during ferrous iron oxidation
Pedrosa et al. Controlled phase formation of nanocrystalline iron oxides/hydroxides in solution–An insight on the phase transformation mechanisms
Mittal et al. Influence of calcium depletion on iron-binding properties of milk
WO2009074998A2 (fr) Sel enrichi en fer
Zhang et al. One-pot synthesis of a novel P-doped ferrihydrite nanoparticles for efficient removal of Pb (Ⅱ) from aqueous solutions: performance and mechanism
WO2016147123A2 (fr) Composition de sel comestible fortifié
Ke et al. Encapsulation of scorodite using crystalline polyferric sulfate precipitated from the Fe (II)-SO42−-O2-H2O system
CN109172541B (zh) 一种稳定的纳米凝胶多糖铁的制备方法
Davidson et al. Direct synthesis of Fe rich SBA-15 at low pH by in-situ formation of iron phosphate phase
US9675098B2 (en) Double fortified salt composition containing iron and iodine and process for the preparation thereof
AU2017203415A1 (en) Antimicrobial chemical compositions
CN113272255B (zh) 以羧酸有机化的硅离子复合物及复合物的制备方法和利用其的产品
Sun et al. Preparation of biomimetic‐bone materials and their application to the removal of heavy metals
BR112017023878B1 (pt) Sal de polifosfato de cálcio e método de produção de sal de polifosfato de cálcio em forma de partículas
CN106472958B (zh) 一种高效选择性降低高氟食品中氟离子的方法
Li et al. pH-Dependent improvement of pyrophosphate removal on amorphous ferric hydroxide by incorporating Ca2+
Boukhalfa et al. Sulfate removal from aqueous solutions by hydrous iron oxide macroscopic, thermal and spectroscopic analyses
Shashkova et al. Sorption of Co 2+, Pb 2+, and Sr 2+ Ions on Hydroxyapatite, Synthesized in the Presence of Oxyethylidenediphosphonic Acid
Yi et al. Removal of Zn (II) by magnetic composite adsorbent: synthesis, performance, and mechanism

Legal Events

Date Code Title Description
NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 16764314

Country of ref document: EP

Kind code of ref document: A2