EP4307909A1 - Procédés de production de produits laitiers appauvris en perchlorate - Google Patents

Procédés de production de produits laitiers appauvris en perchlorate

Info

Publication number
EP4307909A1
EP4307909A1 EP22716342.5A EP22716342A EP4307909A1 EP 4307909 A1 EP4307909 A1 EP 4307909A1 EP 22716342 A EP22716342 A EP 22716342A EP 4307909 A1 EP4307909 A1 EP 4307909A1
Authority
EP
European Patent Office
Prior art keywords
perchlorate
milk
preferred
milk product
ppb
Prior art date
Legal status (The legal status 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 status listed.)
Pending
Application number
EP22716342.5A
Other languages
German (de)
English (en)
Inventor
Jan-Michael Steils
Matthias PARUSEL
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hipp and Co
Original Assignee
Hipp and Co
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 Hipp and Co filed Critical Hipp and Co
Publication of EP4307909A1 publication Critical patent/EP4307909A1/fr
Pending legal-status Critical Current

Links

Classifications

    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00—Milk preparations; Milk powder or milk powder preparations
    • A23C9/14—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment
    • A23C9/142—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by dialysis, reverse osmosis or ultrafiltration
    • A23C9/1427—Milk preparations; Milk powder or milk powder preparations in which the chemical composition of the milk is modified by non-chemical treatment by dialysis, reverse osmosis or ultrafiltration by dialysis, reverse osmosis or hyperfiltration, e.g. for concentrating or desalting
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C7/00—Other dairy technology
    • A23C7/04—Removing unwanted substances other than lactose or milk proteins from milk
    • 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
    • A23L33/40—Complete food formulations for specific consumer groups or specific purposes, e.g. infant formula

Definitions

  • the invention relates to a process for the manufacture of a perchlorate depleted milk product comprising the step of subjecting a perchlorate containing milk product and/or a milk product assumed to contain perchlorate to a nanofiltration step thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein the nanofiltration step makes use of a ceramic nanofiltration membrane.
  • the invention further relates to a process for the manufacture of a milk-based infant formula comprising said process for the manufacture of a perchlorate depleted milk product. Also provided herein is a process for the manufacture of a milk-based infant formula comprising a perchlorate depleted milk product.
  • the present invention further relates to a process for the manufacture of an infant formula base comprising the step of composing an infant formula base from the perchlorate depleted retentate fraction obtained by the processes of the invention.
  • the invention also relates to the use of the produced perchlorate depleted retentate fraction for the manufacture of an infant formula base or an infant formula from said perchlorate depleted milk product.
  • the invention further relates to the use of a nanofiltration membrane for the manufacture of a perchlorate depleted retentate fraction and a system for the manufacture of an infant formula base or a milk-based infant formula comprising a nanofiltration module.
  • Perchlorate (CI0 4 ), the anion of a salt of the perchloric acid (HCI0 4 ), is a contaminant which has been found in drinking water, groundwater and surface water. It is primarily associated with release from defense and military operations, fireworks, certain fertilizers, plant food and by using chlorine-containing substances for cleaning or disinfecting. Perchlorate can also occur naturally in nitrogen-rich mineral deposits. Although it is a strong oxidant, perchlorate is very persistent in the environment and salts of perchlorate are extremely soluble.
  • the first entry pathway is likely to be the contact of food with water, which has previously been treated with chlorine- containing biocidal products for disinfection purposes, while the second entry pathway is via feed and drinking water of the animals.
  • There are health concerns associated to perchlorate since at high concentrations it was demonstrated to affect the thyroid gland by inhibiting the uptake of iodine by the sodium iodide symporter (NIS). Iodine deficiency can lead to developmental delays in fetuses and infants.
  • NIS sodium iodide symporter
  • Iodine deficiency can lead to developmental delays in fetuses and infants.
  • the Environmental Protection Agency established a dietary reference dose (RfD) for perchlorate at 0.0007 mg/kg body weight/day to account for perchlorate exposure from both food and water.
  • Perchlorate is measured in environmental water samples primarily by ion exchange chromatography. This contaminant can be removed from water, for example by employing anion exchange or membrane filtration. Biological and chemical processes are also effective in removing this species from water (Srinivasan et al. 2009 Int J Environ Res Public Health, 6(4):1418-1442).
  • CN106324144 discloses a method for detecting chlorate, perchlorate and bromate from milk powder and infant formula milk powder by hydrophilic interaction chromatography-tandem mass spectrometry.
  • WO2013/068653 discloses a combination of microfiltration, ultrafiltration and nanofiltration that enables milk to be split into a casein fraction, a whey protein fraction and a lactose fraction. These fractions can be combined in a desired manner and in appropriate proportions to provide an infant formula base in which the amino acid composition is close to that of human milk.
  • nanofiltration is merely applied as follow-up step after micro- and ultrafiltration, and the document does not aim to, nor address, the depletion of dangerous contaminants from milk such as perchlorate.
  • CN 101589739 discloses methods for removing melamine from dairy products using nanofiltration. However, this document is silent regarding the use of nanofiltration for the depletion of perchlorate from dairy products. Moreover, CN 101589739 does not specify the used nanofiltration membrane and is equally silent regarding the production of organic dairy products from organic perchlorate depleted milk.
  • the present invention is based at least partly on the surprising finding that a nanofiltration process that makes use of a ceramic nanofiltration membrane is suitable to reliably deplete perchlorate from perchlorate containing milk products or milk products assumed to be contaminated with perchlorate.
  • a nanofiltration process that makes use of a ceramic nanofiltration membrane is suitable to reliably deplete perchlorate from perchlorate containing milk products or milk products assumed to be contaminated with perchlorate.
  • the perchlorate content basically remains unchanged in the obtained retentate fraction. That means the perchlorate content is reduced in relation to the dry mass increase by loss of aqueous fluid. Accordingly, when adjusting the dry mass of the obtained milk product concentrate to the dry mass content of the perchlorate containing milk product before nanofiltration in order to assess perchlorate reduction, it could be observed that the perchlorate content was reduced by about 40% or even more. Moreover, other valuable ions like magnesium and calcium as well as proteins and lactose were largely retained by the ceramic nanofiltration membrane (see Example 1 and Tables 1A to 1G).
  • the methods and processes of the present invention surprisingly allow to safely and reliably reducing perchlorate by about 40% or more from perchlorate containing milk products when referring to the initial dry mass content using a ceramic nanofiltration membrane.
  • the produced perchlorate depleted retentate fraction can then be further used for composing an infant formula base or the production of an infant formula.
  • the present invention provides for an easy applicable, as well as energetically and economically convenient decontamination procedure for the manufacture of milk-based (infant) edibles such as milk based infant formula, which are essentially free of perchlorate.
  • the present invention refers to a method or process for the manufacture of a perchlorate depleted milk product, comprising the step of subjecting a perchlorate containing milk product and/or a milk product assumed to contain perchlorate to a nanofiltration step thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein said nanofiltration step makes use of a ceramic nanofiltration membrane.
  • said method or process further comprises evaluating the perchlorate content in said retentate fraction and/or said permeate fraction, and optionally supplying a manufacturing process of a milk based formula with said perchlorate depleted retentate fraction.
  • said perchlorate containing milk product and or milk product assumed to contain perchlorate contains 2 ppb or more than 2 ppb perchlorate when the dry mass of said milk product is between about 5% and about 13%.
  • said perchlorate containing milk product and or milk product assumed to contain perchlorate contains 2 ppb or more than 2 ppb perchlorate when the dry mass of said milk product is about 6% or about 9%.
  • said ceramic nanofiltration membrane used according to the methods and processes of the invention has a molecular weight cut-off between about 150-1000 Da, more preferred between about 200 and 750 Daltons, even more preferred between 200 and 450 Daltons, still more preferred between about 200 and 250.
  • Said ceramic nanofiltration membrane is preferably characterized by lactose and protein rejection. It is further envisaged that said ceramic nanofiltration membrane is made out of titanium dioxide or silicon dioxide, preferably titanium dioxide.
  • the ceramic nanofiltration membrane is characterized in that it deplete at least 35%, more preferred at least 39% of the contained perchlorate by a nanofiltration step as defined herein.
  • the ceramic nanofiltration membrane is characterized in that it deplete at least 40%, preferably at least 46% of the contained chlorate and/or at least 30%, preferably at least 35% of the contained bromide, preferably by a nanofiltration step as defined herein. It is further envisaged that the ceramic nanofiltration membrane is characterized by a magnesium rejection by at least 80% and/or a calcium rejection by at least 80%, preferably by a nanofiltration step as defined herein.
  • the perchlorate containing milk product and/or milk product assumed to contain perchlorate is milk or whey.
  • said milk is skim milk, low-fat milk or whole milk.
  • Said whey is preferably sweet whey or sour whey. It is envisaged that said milk or whey is pretreated. It is further envisaged that said milk or whey is milk or whey concentrate. It is further envisaged that said perchlorate containing milk product and/or milk product assumed to contain perchlorate is an organic milk product. Most preferred, the perchlorate containing milk product and/or milk product assumed to contain perchlorate is organic skim milk, organic whole milk, organic low-fat milk or organic whey.
  • perchlorate depleted milk product As described herein, it is envisaged that said perchlorate containing milk product and/or milk product assumed to contain perchlorate contains 2 ppb or more than 2 ppb chlorate and/or 2 ppb or more than 2 ppb bromide when the dry mass of the milk product is between about 5% and about 13%.
  • the perchlorate depleted retentate fraction obtained by the method or process for the manufacture of a perchlorate depleted milk product as described herein can optionally be contacted with a perchlorate free solvent and subjected to a further nanofiltration step, preferably as defined herein.
  • the perchlorate containing permeate fraction obtained by the method or process of the present invention is discarded, i.e. can be used for nonfood applications or the perchlorate containing permeate fraction can be purified for further production steps.
  • the perchlorate depleted retentate fraction obtained by the method or process of the present invention is preferably further processed.
  • the processes or methods of the present invention further comprise a demineralization step. It is also envisaged that said perchlorate depleted retentate fraction is diluted.
  • the method or process of the present invention for the manufacture of a perchlorate depleted milk product is for the manufacture of a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13%. More preferred, the method or process of the present invention for the manufacture of a perchlorate depleted milk product is for the manufacture of a perchlorate depleted milk product containing less than 2 ppb perchlorate, less than 2 ppb chlorate and less than 2 ppb bromide when the dry mass of the milk product is between about 5% and about 13%.
  • the methods or processes for the manufacture of a perchlorate depleted milk product of the present invention comprise at least the step of formulating said perchlorate depleted milk product into a milk based infant formula.
  • another aspect of the present invention relates to a process for the manufacture of a milk-based infant formula, comprising the processes for the manufacture of a perchlorate depleted milk product of the present invention as described herein above.
  • Also provided by the present invention is a method or process for the manufacture of a milk-based infant formula from a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13%, comprising the processes for the manufacture of a perchlorate depleted milk product as defined herein.
  • the present invention provides a process for the manufacture of a milk-based infant formula from a perchlorate depleted milk product containing less than 2 ppb perchlorate, less than 2 ppb chlorate and less than 2 ppb bromide when the dry mass of the milk product is between about 5% and about 13%, comprising the process for the manufacture of a perchlorate depleted milk product as defined herein.
  • said manufacturing process comprises at least the step of formulating said perchlorate depleted milk product into a milk-based infant formula.
  • said milk-based infant formula is spray dried or processed to powder. It is envisaged that said milk-based infant formula is packed in portions of 11 to 25 g or 300 to 800g. Further, said milk-based infant formula can be produced as a liquid infant formula. It is envisaged that said milk-based infant formula is packed into portions of 90 to 1000ml.
  • the present invention also refers to a method or process for the manufacture of an infant formula base comprising the step of composing said infant formula base from the perchlorate depleted retentate fraction obtained by the processes and methods of the present invention.
  • a process for the manufacture of an infant formula base from a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13% comprising the process for the manufacture of a perchlorate depleted milk product as defined herein.
  • said infant formula base is dried into a powder. More preferably, said infant formula base is spray dried or processed to powder. It is further envisaged that said infant formula base is formulated to an infant formula having an energy content of about 60 to 80 kcal/100 ml as consumed, preferably of about 62 to 75 kcal/100ml as consumed.
  • the present invention relates to the use of a ceramic nanofiltration membrane as defined according to the methods and processes of the invention for the manufacture of a perchlorate depleted retentate fraction from a perchlorate containing milk product and/or milk product assumed to contain perchlorate.
  • the present invention also relates to the use of a ceramic nanofiltration membrane as defined according to the methods and processes of the invention for the manufacture of an infant formula base comprising a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13%.
  • a ceramic nanofiltration membrane as defined according to the methods and processes of the invention for the manufacture of a milk-based infant formula comprising a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13%. It is further envisaged in this respect that the perchlorate depleted milk product from which the infant formula base or the milk-based infant formula is produced contains less than 2 ppb chlorate and less than 2 ppb bromide when the dry mass of the milk product is between about 5% and about 13%.
  • the present invention also refers to a system for the manufacture of an infant formula base or a milk-based infant formula comprising a nanofiltration module that is suitable for subjecting a perchlorate containing milk product and/or a milk product assumed to contain perchlorate to a nanofiltration step thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein said nanofiltration step makes use of a ceramic nanofiltration membrane as defined herein.
  • Figure 1 shows a general schematic overview of the workflow applicable for the manufacture of a perchlorate depleted skim milk concentrate and perchlorate depleted skim milk, and a perchlorate depleted infant formula.
  • Figure 2 shows a detailed overview of the workflow applicable for the manufacture of perchlorate depleted skim milk.
  • Figure 3 shows a detailed overview of the workflow applicable for the manufacture of perchlorate depleted skim milk powder, a perchlorate depleted infant formula base and a perchlorate depleted infant formula from perchlorate depleted skim milk concentrate.
  • Figure 4 shows a general schematic overview of the workflow applicable for the manufacture of perchlorate depleted whey and a perchlorate depleted infant formula.
  • Figure 5 shows a detailed overview of the workflow applicable for the manufacture of perchlorate depleted whey powder, a perchlorate depleted infant formula base and a perchlorate depleted infant formula from perchlorate depleted whey concentrate.
  • the present inventions is inter alia based on the surprising finding that nanofiltration that makes use of a ceramic nanofiltration membrane can be used to deplete milk products of water-soluble inorganic contaminants such as perchlorate while other nutritionally valuable components like magnesium, calcium, protein and lactose are largely retained in the nanofiltration retentate.
  • the amount of perchlorate in various milk products like skim milk and whey could be reliably and efficiently reduced by at least 35%, preferably by about 40% or more when applying nanofiltration techniques described herein.
  • the processes for the manufacture of perchlorate deplete milk product of the present invention allows for the manufacture of milk- based (infant) formula complying, in respect of the perchlorate content, with toxicological limits recommended so far by the WHO and EFSA.
  • Most commonly used processes for the manufacture of milk based infant formula and other milk-based or milk containing edibles are downdraft evaporators. These devices increase the dry mass to up to about 25%, thereby concentrating the milk raw material. However, this process also results in concentrating contaminants like perchlorate on the dry matter (or dry mass). This is a disadvantage in the current state of the art as well as the fact that processing of milk in such downdraft evaporators is a highly energy-intensive method.
  • skimmed milk concentrate with a dry mass of about 22% is mixed with highly demineralized whey raw materials and lactose, as well as other substances. Demineralizing of said whey raw materials to 90% also represents a very complex and cost intensive process.
  • the inventors devised the use of nanofiltration that makes use of a ceramic nanofiltration membrane as a new method to easily obtain/produce perchlorate depleted milk products, thereby also removing other minerals.
  • the invention describes that perchlorate, but also other unwanted compounds such as chlorate and bromide can be depleted when subjecting a perchlorate containing milk product that also contains chlorate and/or bromide to nanofiltration as described herein.
  • the invention describes partial desalination of the perchlorate containing milk product in that positive and negative monovalent ions of the salts present in the perchlorate containing milk product like sodium, potassium and chloride are depleted when subjecting the perchlorate containing milk product to nanofiltration as described herein.
  • nanofiltration means that, overall, the total salt content of the perchlorate-depleted milk or of the milk- based infant formula can be better adjusted. This is advantageous, for example, for the production of additives, which have to be later on included in milk-based infant formulas. Since said required additives can contain higher salt content, this in turn means, for example in the case of whey powders, possibly a further energy and cost savings.
  • Nanofiltration in general terms is a membrane filtration process used most often with low total dissolved solids water such as surface water and fresh groundwater, with the purpose of softening the filtrate (polyvalent cation removal) and removal of disinfection by product precursors such as natural organic matter and synthetic organic matter in the filtrate (Roy et al. 2017 Desalination. 420: 241-257; Letterman et al. 1999 Water Quality and Treatment 5 th Ed ISBN 0-07-001659-3).
  • nanofiltration relies on the use of membranes made of a synthetic, porous material, which acts like a shield, preventing particles of a defined size from passing as pressure forces the feed through the membranes.
  • feed refers to any substance (water, milk) that is subjected to a membrane processing.
  • the nanofiltration membrane is created from ceramic materials as described elsewhere herein.
  • the inventors applied a ceramic nanofiltration membrane to a milk product, in particular skim milk and whey, to receive a skim milk or whey concentrate for the milk based infant formula production and analyzed the out- coming retentate fraction (skim milk or whey concentrate).
  • a ceramic nanofiltration membrane to a milk product, in particular skim milk and whey, to receive a skim milk or whey concentrate for the milk based infant formula production and analyzed the out- coming retentate fraction (skim milk or whey concentrate).
  • the inventors were surprisingly able to increase the dry matter of perchlorate containing skim milk from between about 8% to 10% to between about 16% to 20%, and simultaneously achieving a reduction of perchlorate of at least 45% in the perchlorate containing skim milk when referring to the initial dry mass content.
  • perchlorate (CI0 4 ) can be efficiently depleted from a perchlorate containing milk product or a milk product assumed to contain perchlorate and is not rejected from a ceramic nanofiltration membrane, while also other smaller ions like magnesium and calcium are surprisingly retained in high percentages. This finding is very surprising, since perchlorate (CI0 4 ) has the largest atomic volume per mole (74.7 qcm/mol) and the largest molecular weight (99.449 Dalton) of all ions in the milk (see Table 2).
  • the methods of the present invention based on subjecting a perchlorate containing milk product to a nanofiltration step comprising a ceramic nanofiltration membrane provide for a favorable method for the manufacture of a perchlorate depleted milk product, which can be used for the manufacture of a (infant) formula or a formula base with reduced perchlorate levels.
  • the methods of the present invention can address the provision of an effective and energy saving reduction of perchlorate contamination from milk products.
  • the invention relates to a process for the manufacture of a perchlorate depleted milk product, comprising the step of subjecting a perchlorate containing milk product and/or milk product assumed to contain perchlorate to a nanofiltration step thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein the nanofiltration step makes use of a ceramic nanofiltration membrane.
  • the present invention refers to a process for the manufacture of a perchlorate depleted milk product, comprising the step of subjecting a perchlorate containing milk product and/or milk product assumed to contain perchlorate to a nanofiltration step to obtain a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein the nanofiltration step makes use of a ceramic nanofiltration membrane.
  • the present invention refers to a process for the manufacture of a perchlorate depleted milk product, comprising the step of subjecting a perchlorate containing milk product and/or milk product assumed to contain perchlorate to a nanofiltration step to obtain a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein said nanofiltration step makes use of a ceramic nanofiltration membrane and said nanofiltration is conducted with predetermined process parameters that are suitable to deplete at least 35%, preferably at least 39% of the contained perchlorate in the perchlorate containing milk product when referring to the initial dry mass content.
  • the perchlorate content is reduced in relation to the dry mass increase by loss of aqueous fluid.
  • said method also comprises evaluating the perchlorate content in said retentate and/or permeate fraction as described elsewhere herein. Further, it is envisaged that a manufacturing process of a milk based infant formula with said perchlorate depleted retentate fraction is supplied.
  • a perchlorate depleted milk product in particular refers to a milk product as defined elsewhere herein wherein the perchlorate initially contained in said milk product or assumed to be initially contained in said milk product is significantly reduced in quantity or even completely removed when referring to the initial dry mass content.
  • “Significantly reduced in quantity” with reference to the remaining content of perchlorate in said milk after applying nanofiltration means that the content of perchlorate is decreased by at least 35%, preferably at least 39%, more preferred at least 45 %, when compared to the initial amount of perchlorate in said milk product, i.e. is reduced by an amount between 35% and 100% when conducting a nanofiltration step that makes use of a ceramic nanofiltration membrane as defined elsewhere herein.
  • it is preferred that the content of perchlorate is reduced by an amount between 45% and 85%, more preferred between 65% and 85%.
  • the perchlorate content of said milk after applying the nanofiltration technique described elsewhere herein can be reduced by at least 35%, more preferred by at least 40%, even more preferred by at least 45%, still more preferred by at least 50%, still more preferred by at least 55%, still more preferred by at least 60%, still more preferred by at least 65%, still more preferred by at least 70%, still more preferred by at least 75%, still more preferred by at least 80%, still more preferred by at least 85%, still more preferred by at least 90%, still more preferred by at least 95%, still more preferred by at least 98%, still more preferred by at least 99%. Most preferred the perchlorate content of said milk after applying nanofiltration is reduced by 100%.
  • the content of perchlorate is decreased by at least 35%, preferably by at least 39%. More preferred the content of perchlorate is decreased by at least 45%. Even more preferred the content of perchlorate is decreased by at least 50%.
  • a “perchlorate depleted milk product” also refers to a milk product in which the absolute amount of perchlorate is determined.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 13%.
  • a perchlorate depleted milk product containing less than 2 ppb of perchlorate has a dry mass between 5% and 14%, preferably between 5% and 13%.
  • a perchlorate depleted milk product containing less than 2 ppb of perchlorate has a dry mass between 5% and 7%.
  • a perchlorate depleted milk product of the invention containing less than 2 ppb of perchlorate has a dry mass between 8% and 10%.
  • perchlorate depleted milk product of the invention containing less than 2 ppb of perchlorate has a dry mass between 8% and 13%.
  • a dry mass of the milk product between about 5% and about 13% as used in the context of the present invention means that the dry mass of the milk product is in the range of about 5% and about 13%, i.e.
  • a dry mass of a milk product between about 5% and about 13% as used in the context of the present invention further includes the concrete numbers of 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12% and 13% and any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 7%, i.e. about 5%, about 6% or about 7% or any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between 5% and 7%, i.e. 5%, 6% or 7% or any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 10%, i.e. about 8%, about 9% or about 10% or any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between 8% and 10%, i.e. 8%, 9% or 10% or any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 13%, i.e. about 8%, about 9%, about 10%, about 11%, about 12% or about 13% or any number in between.
  • a “perchlorate depleted milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between 8% and 13%, i.e. 8%, 9%, 10%, 11%, 12% or 13% or any number in between.
  • a “perchlorate depleted milk product” contains less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 7% as defined herein is whey.
  • said perchlorate depleted milk product containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 7% is produced from a perchlorate containing milk product and/or milk product assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 5% and about 7%.
  • a “perchlorate depleted milk product” contains less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 10% as defined herein is skim milk.
  • said perchlorate depleted milk product containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 10% is produced from a perchlorate containing milk product and/or milk product assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 8% and about 10%.
  • a “perchlorate depleted milk product” containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 13% as defined herein is whole milk or low-fat milk.
  • said perchlorate depleted milk containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate depleted) milk product is between about 8% and about 13% is produced from perchlorate containing milk and/or milk assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 8% and about 13%.
  • the “perchlorate depleted milk product” as described herein above contains less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01
  • the “perchlorate depleted milk product” manufactured according to the processes of the present invention comprises no detectable amount of perchlorate, i.e. the content of perchlorate has been nearly completely removed.
  • the perchlorate depleted retentate fraction obtained after nanofiltration, i.e. one nanofiltration step, can be contacted with perchlorate free solvent defined elsewhere herein to achieve to the same dry mass content of the initial “perchlorate containing milk product” or “milk product assumed to contain perchlorate” as defined elsewhere herein to compare the perchlorate content before and after nanofiltration.
  • the perchlorate content can be measured in the retentate fraction and reduction of the content of perchlorate by nanofiltration can be calculated based on the dry mass increase.
  • a reduction of the perchlorate content in the retentate fraction after subjecting a perchlorate containing milk product to nanofiltration as described herein refers to the fact that the dry mass of the perchlorate depleted retentate fraction is recalculated to refer to the initial dry mass content before nanofiltration.
  • a “perchlorate containing milk product” subjected to nanofiltration refers to milk containing 2 ppb or more than 2 ppb perchlorate when the dry mass of the (perchlorate containing) milk product is between about 5% and about 13%, preferably about 6% or about 9%.
  • a dry mass of a milk product between about 5% and about 13% as used in the context of the present invention means that the dry mass of the milk product is in the range of about 5% and about 13%, i.e.
  • a dry mass of a milk product between about 5% and about 13% as used in the context of the present invention further includes the concrete numbers of 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12% and 13% and any number in between.
  • a “perchlorate containing milk product” subjected to nanofiltration is considered as containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between about 5% and about 7%, i.e.
  • a “perchlorate containing milk product” subjected to nanofiltration is considered as containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between 5% and 7%, i.e. 5%, 6% or 7% or any number in between.
  • a “perchlorate containing milk product” subjected to nanofiltration is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between about 8% and about 10%, i.e.
  • a “perchlorate depleted milk product” subjected to nanofiltration is considered as containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between 8% and 10%, i.e. 8%, 9% or 10% or any number in between.
  • a “perchlorate containing milk product” is considered as containing less than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between about 8% and about 13%, i.e.
  • a “perchlorate depleted milk product” subjected to nanofiltration is considered as containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between 8% and 13%, i.e. 8%, 9%, 10%, 11%, 12% or 13% or any number in between.
  • a “perchlorate containing milk product” containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between about 5% and about 7% as defined herein is whey.
  • a “perchlorate containing milk product” containing 2 ppb or more than 2 ppb of perchlorate when the dry mass of the (perchlorate containing) milk product is between about 8% and about 10% as defined herein is skim milk.
  • milk product assumed to contain perchlorate means that perchlorate is not necessarily determined or measured in said milk product before subjecting the milk product to nanofiltration, but is supposed to be 2 ppb or more than 2 ppb when the dry mass of the “milk product assumed to contain perchlorate” is between about 5% and about 13%, preferably about 6% or about 9%.
  • the amount of perchlorate contained in said “perchlorate containing milk product” or said “milk product assumed to contain perchlorate” may e.g.
  • milk product assumed to contain perchlorate also refers to a milk product originating from milk that comes from a dairy farm that practices grazing livestock. Hence, the fact that the milk product is “assumed to contain perchlorate” can be equated with a certain security that this milk product is a “perchlorate containing milk product”, but without the necessity of measuring the actual perchlorate content in said milk product.
  • nanofiltration making use of a ceramic nanofiltration membrane can be conducted with (predetermined) process parameters depleting at least 35%, preferably at least 39%, even more preferred at least 45%, of the contained perchlorate in one nanofiltration step.
  • the reduction of perchlorate is related to the dry matter, in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step.
  • the depletion of at least 35% means that 65% or less than 65% of the contained perchlorate is rejected by the ceramic nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • rejection means that a compounds is refrained from passing through the ceramic nanofiltration membrane described elsewhere herein, i.e. the quantity of the compound is maintained when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate. “Maintained” means that basically the same amount of the compounds is present in the obtained perchlorate depleted retentate fraction when referring to the same dry mass as the “perchlorate containing milk product” or “milk product assumed to contain perchlorate”.
  • a rejection means that at least 95%, more preferred at least 95.5%, even more preferred at least 96%, still more preferred at least 96.5%, still more preferred at least 97%, still more preferred at least 97.5%, still more preferred at least 98%, still more preferred at least 98.5%, still more preferred at least 99%, still more preferred at least 99.2%, still more preferred at least 99.3%, still more preferred at least 99.4%, still more preferred at least 99.5%, still more preferred at least 99.6%, still more preferred at least 99.7%, still more preferred at least 99.8%, still more preferred at least 99.9% of the compound are refrained from passing through the ceramic nanofiltration membrane. Most preferred a rejection means that 100% of the compound are refrained from passing through the ceramic nanofiltration membrane.
  • a perchlorate depletion of at least 35% means that the contained perchlorate is depleted by 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at least 35% of the contained perchlorate in one nanofiltration step.
  • the applied (predetermined) process parameters deplete at least 35%, more preferred at least 39%, still more preferred at least 40%, still more preferred at least 45%, still more preferred at least 50%, still more preferred at least 55%, still more preferred at least 60%, still more preferred at least 65%, still more preferred at least 70%, still more preferred at least 75%, still more preferred at least 80%, still more preferred at least 85%, still more preferred at least 90%, still more preferred at least 95%, still more preferred at least 97%, still more preferred at least 98%, still more preferred at least 99% of the contained perchlorate in one nanofiltration step. Most preferred the perchlorate content of said milk product after applying nanofiltration is reduced by 100%.
  • predetermined process parameters reduce the perchlorate content in relation to the dry mass increase by loss of aqueous fluid.
  • said process parameters are suitable to (roughly) double the dry mass of the starting raw material while the perchlorate content remains basically unchanged.
  • Predetermined process parameters means in this respect that said nanofiltration parameters are defined beforehand and are known to be applicable to achieve the objective for which they are applied.
  • said predetermined process parameters can be used as reference or standard nanofiltration parameters to significantly remove the perchlorate content from a milk product containing perchlorate or a milk product assumed to contain perchlorate, namely depleting at least 35% of the contained perchlorate in milk in one passage.
  • said predetermined process parameters can be conducted without the need to determine the perchlorate content in the milk subjected to nanofiltration, or in the permeate and/or retentate fraction.
  • said predetermined process parameters automatically result in a perchlorate depleted milk product as defined elsewhere herein, i.e.
  • said predetermined process parameters can be the ones summarized in Example 1. Parameters useful in this respect as predetermined nanofiltration process parameters to deplete at least 35%, preferably ate least 39%, more preferred at least 45% of the contained perchlorate are described elsewhere herein.
  • the perchlorate containing milk product and/or milk product assumed to contained perchlorate as defined elsewhere herein contains chlorate and/or bromide, i.e. is a chlorate and/or bromide containing milk product and/or milk product assumed to contain chlorate and/or bromide.
  • the “perchlorate containing” milk product as defined herein contains 2 ppb or more than 2 ppb chlorate and/or 2 ppb or more than 2 ppb bromide when the dry mass of said milk product is between about 5% and about 13% as defined elsewhere herein, preferably about 6% or about 9%.
  • a “perchlorate containing milk product” also refers to a milk product that is additionally chlorate and/or bromide containing. Accordingly, the context of the present invention also the absolute amount of chlorate and/or bromide may be determined in a “perchlorate containing milk product” and/or a “perchlorate depleted milk product”.
  • a “perchlorate depleted milk product” manufactured according to the processes of the present invention is considered as containing less than 2 ppb of chlorate when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 13% as defined elsewhere herein, preferably about 6% or about 9%.
  • the “perchlorate depleted milk product” contains less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb chlorate,
  • the “perchlorate depleted milk product” manufactured according to the processes of the present invention comprises no detectable amount of chlorate, i.e. the content of chlorate has been nearly completely removed.
  • the “perchlorate depleted milk” manufactured according to the processes of the present invention is considered as containing less than 2 ppb of bromide when the dry mass of the (perchlorate depleted) milk product is between about 5% and about 13% as defined elsewhere herein, preferably about 6% or about 9%.
  • the “perchlorate depleted milk product” contains less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb bromide
  • the chlorate and/or bromide depleted (perchlorate depleted) retentate fraction obtained after nanofiltration i.e. one nanofiltration step that makes use of a ceramic nanofiltration membrane as defined elsewhere herein
  • perchlorate, chlorate and bromide free solvent defined elsewhere herein can be contacted with perchlorate, chlorate and bromide free solvent defined elsewhere herein to achieve to the same dry mass content of the initial “perchlorate containing milk product” or “milk product assumed to contain perchlorate” that also contains chlorate and/or bromide, as defined elsewhere herein to compare the chlorate and/or bromide content before and after nanofiltration.
  • the chlorate and/or bromide content can be measured in the retentate fraction and reduction of the content of chlorate and/or bromide by nanofiltration can be calculated based on the dry mass increase.
  • the perchlorate containing milk product and/or milk product assumed to contained perchlorate as defined elsewhere herein also contains chlorate and/or bromide.
  • the nanofiltration according to the processes of the present invention that makes use of a ceramic nanofiltration membrane is further envisaged to be conducted with (predetermined) process parameters depleting at least 40%, preferably at least 46% of the contained chlorate and/or at least 30%, preferably at least 35% of the contained bromide in one nanofiltration step. Specifically, said (predetermined) process parameters reduce the chlorate and bromide content in relation to the dry mass increase by loss of aqueous fluid.
  • the reduction of the chlorate and bromide is related to the dry matter, in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step. That means, the reduction is calculated when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate, i.e. they are considered to have the same dry mass.
  • said (predetermined) process parameters can be used as reference or standard nanofiltration parameters to significantly remove in addition to the perchlorate content from a milk product containing perchlorate or milk product assumed to contain perchlorate, also at least 40% of the contained chlorate and/or at least 30%, preferably at least 35% of the contained bromide in said milk product in one passage or nanofiltration step.
  • said process parameters can be conducted without the need to determine the chlorate and/or bromide content in the milk product subjected to nanofiltration, or in the permeate and/or retentate fraction.
  • said predetermined process parameters can be the ones summarized in Examples 1.
  • a depletion of at least 40% of the contained chlorate means that 60% or less than 60% of the contained chlorate is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 40% means that the contained chlorate is depleted by 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at least 40% of the contained chlorate in one nanofiltration step.
  • a depletion of at least 30% of the contained bromide means that 70% or less than 70% of the contained bromide is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 30% means that the contained bromide is depleted by 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at 30% of the contained bromide is depleted in one nanofiltration step.
  • the perchlorate containing milk product and/or milk product assumed to contained perchlorate as defined elsewhere herein contains lactose and protein.
  • the absolute amount of lactose and protein may be determined in “perchlorate containing milk product", “milk product assumed to contain perchlorate” and “perchlorate depleted milk product” using for example a method in accordance with the Official Collection of Methods for Sampling and Examining Foods ( ⁇ 64 of the German Food and Feed Code (LFGB).
  • the amount of lactose is determined according to the enzymatic method L 01.00-17 2016-10 for the determination of lactose in milk and milk products according to DIN 10344).
  • the amount of protein is determined according to the Kjeldahl method L 01.00-10 2016-03 and the calculation of the raw protein content according to DIN EN ISO 8968-1.
  • a “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 44 g/kg and 49 g/kg lactose, preferably, between 45 g/kg and 49 g/kg, even more preferred between 46 g/kg and 48 g/kg or between
  • a “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 45 g/kg and 49 g/kg lactose, preferably between 46 g/kg and 48 g/kg lactose when the dry mass of the perchlorate containing milk product is between about 8% and about 13% as defined elsewhere herein, preferably between about 8% and about 10%.
  • a “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 44 g/kg and 49 g/kg lactose, preferably between 45 g/kg and
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 5 g/kg and 42 g/kg protein, preferably between 5 g/kg and 20 g/kg or between 30 g/kg and 42 g/kg protein when the dry mass of the perchlorate containing milk product is between about 5% and about 13 as defined elsewhere herein, preferably about 6% or about 9%.
  • a “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 30 g/kg and 42 g/kg, preferably between 34 g/kg and 38 g/kg protein when the dry mass of the perchlorate containing milk product is between about 8% and about 13% as defined elsewhere herein, preferably between about 8% and about 10%.
  • a “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” contains between 5 g/kg and 20 g/kg, preferably between 6 g/kg and 12 g/kg protein when the dry mass of the perchlorate containing milk product is between about 5% and about 7% as defined elsewhere herein.
  • the nanofiltration according to the processes of the present invention that makes use of a ceramic nanofiltration membrane can further be conducted with (predetermined) process parameters leading to lactose and protein rejection in one nanofiltration step.
  • predetermined process parameters can be the ones summarized in Example 1.
  • the “rejection” of lactose and protein as described herein means that the quantity of lactose and protein is (roughly) doubled in relation to the dry mass increase by loss of aqueous fluid in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step.
  • the rejection of lactose an protein in one nanofiltration step means that the same content of lactose and protein is present when determined in the “perchlorate containing milk product” or “milk product assumed to contain perchlorate” as in the “perchlorate depleted milk product” when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate.
  • the term “rejection” means that at least 95%, more preferred at least 95.5%, even more preferred at least 96%, still more preferred at least 96.5%, still more preferred at least 97%, still more preferred at least 97.5%, still more preferred at least 98%, still more preferred at least 98.5%, still more preferred at least 99%, still more preferred at least 99.2%, still more preferred at least 99.3%, still more preferred at least 99.4%, still more preferred at least 99.5%, still more preferred at least 99.6%, still more preferred at least 99.7%, still more preferred at least 99.8%, still more preferred at least 99.9% of the compound, here lactose and protein, are refrained from passing through the nanofiltration membrane.
  • a rejection means that 100% of the compound, herein lactose and protein, are refrained from passing through the nanofiltration membrane.
  • the quantity of the compound, herein protein and lactose is maintained when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate.
  • the content of lactose and protein is determined in a perchlorate containing milk product (before nanofiltration) and after in the perchlorate depleted milk product subjected to nanofiltration (i.e.
  • nanofiltration making use of a ceramic nanofiltration membrane can be conducted with (predetermined) process parameters characterized by magnesium rejection by at least 80%, preferably by at least 92% and/or calcium rejection by at least 80%, preferably by at least 89% in one nanofiltration step.
  • said (predetermined) process parameters reject at least 80%, preferably at least 92% of the magnesium content and/or 80%, preferably at least 89% of the calcium content when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate, i.e. they have the same dry mass.
  • the rejection of magnesium and/or calcium is related to the dry matter, in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step.
  • process parameters can be conducted without the need to determine the magnesium and/or calcium content in the milk product subjected to nanofiltration, or in the permeate and/or retentate fraction.
  • said predetermined process parameters can be the ones summarized in Example 1.
  • a magnesium rejection by at least 80% means that 20% or less than 20% of the contained magnesium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the rejection of at least 80% means that the contained magnesium is rejected by 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters reject at least 80% of the contained magnesium in one nanofiltration step. More preferred at least 85%, even more preferred at least 90%, still more preferred at least 92%, still more preferred at least 95%, still more preferred at least 97%, still more preferred at least 98%, still more preferred at least 99% of the contained magnesium is rejected in one nanofiltration step. Most preferred 100% of the contained magnesium is rejected in one nanofiltration step.
  • a calcium rejection by at least 80% means that 20% or less than 20% of the contained calcium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the rejection of at least 80% means that the contained calcium is rejected by 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters reject at least 80% of the contained calcium in one nanofiltration step. More preferred at least 85%, even more preferred at least 90%, still more preferred at least 92%, still more preferred at least 95%, still more preferred at least 97%, still more preferred at least 98%, still more preferred at least 99% of the contained calcium is rejected in one nanofiltration step.
  • Most preferred 100% of the contained calcium is rejected in one nanofiltration step.
  • the nanofiltration according to the processes described herein can further be used for simultaneous desalination of the perchlorate containing milk product, i.e.
  • the nanofiltration according to the processes described herein can be conducted with (predetermined) process parameters characterized by an up to 41%, preferably up to 50% or more reduced content of sodium and/or an up to 41% or more reduced content of potassium in one nanofiltration step.
  • said (predetermined) process parameters reduce up to 50% or more of sodium and/or up to 41% ore more of potassium when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate, i.e. they have the same dry mass.
  • the reduction of sodium and/or potassium is related to the dry matter, in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step.
  • process parameters can be conducted without the need to determine the sodium and/or potassium content in the milk product subjected to nanofiltration, or in the permeate and/or retentate fraction.
  • said predetermined process parameters can be the ones summarized in Example 1.
  • a sodium and/or potassium rejection by up to 50% means that 50% or more than 50% of the contained sodium and/or potassium are rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the rejection of 50% or more than 50% means that the contained sodium and/or potassium is rejected by 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at least 50% of the contained sodium and/or potassium in one nanofiltration step, preferably 55%.
  • the nanofiltration according to the processes described herein can be conducted with (predetermined) process parameters depleting at least 40%, preferably at least 45%, more preferred at least 50%, even more preferred at least 52%, still more preferred at least 56%, still more preferred at least 63%, still more preferred at least 68% of the contained chloride in one nanofiltration step.
  • said (predetermined) process parameters reduce at least 52%, preferably at least 56%, more preferred at least 63%, even more preferred at least 68% of the contained chloride in one nanofiltration step of the contained chloride when the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate, i.e. they have the same dry mass.
  • the depletion of chloride is related to the dry matter, in a process where the dry matter of the perchlorate containing milk product and/or milk product assumed to contained perchlorate is roughly doubled by concentration in one nanofiltration step.
  • said process parameters can be conducted without the need to determine the chloride content in the milk product subjected to nanofiltration, or in the permeate and/or retentate fraction.
  • said predetermined process parameters can be the ones summarized in Example 1.
  • a chloride depletion of at least 52% means that 48% or less than 48% of the contained chloride is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 52% means that the contained chloride is depleted by 52%, 53%, 55%, 56%, 60%, 63%, 64%, 65%, 68%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at least 40% of the contained chloride in one nanofiltration step.
  • the content of perchlorate in a “perchlorate containing milk product”, “milk product assumed to contain perchlorate” and a “perchlorate depleted milk product” can be easily analyzed by those skilled in the art using known methods like, ion chromatography (IC), high performance liquid chromatography (HPLC), ion chromatographic-mass spectrometry (IC-MS) or liquid chromatographic-mass spectrometry (LC-MS), just to name some.
  • IC ion chromatography
  • HPLC high performance liquid chromatography
  • IC-MS ion chromatographic-mass spectrometry
  • LC-MS liquid chromatographic-mass spectrometry
  • the content of perchlorate in a “perchlorate containing milk product”, “milk product assumed to contain perchlorate” and a “perchlorate depleted milk product” is analyzed using the QuPPe-AO-Method (Quick Polar Pesticides Method) as described by the EU Reference Laboratories for Residues of Pesticides requiring Single Residue Methods (EURL-SRW), CVUA Stuttgart, Schaflandstr. 3/2, DE-70736 Fellbach, Germany that involves extraction with acidified methanol and LC-MS/MS measurement, and is known to those skilled in the art.
  • QuPPe-AO-Method QuPPe-AO-Method
  • ppb means “parts per billion” and is the number of units of mass of a contaminant per 1000 million units of total mass (1 ppb equals 1*1 O 9 or 0.000000001). Also pg/L (micrograms per liter) or pg/kg (micrograms per kilogram) can be used to define the amount of a contaminant. In this respect, 1 ppb corresponds to an amount of 0.001 mg/kg contaminant. It should be noted that in the dairy industry the mass unit kg is used and not the volume unit liters. If a liter is specified, the user must pay attention to conversion factors. Regardless of the unit indicated, the method for each unit of mass or volume can be specified taking into account the conversion factors. Both in terms of dry matter and on fresh mass.
  • milk product refers in its broadest sense to a compound originating from milk, i.e. a milk-related product that can contain many or all ingredients of milk. “Originating from” means that milk is the original basis of said milk product which may have been processed or pretreated in order to obtain said milk product.
  • said milk product is preferably milk or whey.
  • milk refers to an opaque white fluid rich in fat, protein and milk sugar, and comprising partially dissolved minerals and vitamins, secreted by female mammals for the nourishment of their young.
  • said milk is skim milk, low-fat milk or whole milk.
  • skim milk has a typical dry mass of about 8% to about 10%, preferably about 9%, and a fat content of ⁇ 0.1%.
  • Low-fat or fat-reduced milk has a dry mass of about 8% to about 13% and a fat content between 0.1 and 3% (see Chemie und Physik der Milch, Naturstoff Rohstoffmaschine, 4 th edition 2016, Behrs Verlag, ISBN: 978-3- 95468-037-5).
  • the term “whole milk” also comprises raw milk, i.e. milk naturally produced by a mammal that did not undergo any modification or treatment procedure.
  • “skim milk” as used herein refers to whole milk which has been deprived of the milk fat using so called milk separators. What remains is the skimmed milk. Skim milk or skimmed milk usually contains less than 0.1% fat independently of original fat content of the whole milk. “Low-fat milk” refers to whole milk with reduced fat content obtained by centrifugal separation, which removes some of the fat globules or cream to lower the fat content. “The term “skim milk concentrate” as used herein refers to the material retrieved after nanofiltration when subjecting perchlorate containing skim milk to nanofiltration defined elsewhere herein.
  • the term “skim milk concentrate” corresponds to the “retentate fraction” as defined elsewhere herein when skim milk has been subjected to nanofiltration.
  • the term “whole milk concentrate” as used herein refers to the material retrieved after nanofiltration when subjecting perchlorate containing whole milk to nanofiltration defined elsewhere herein. Accordingly, the term “whole milk concentrate” corresponds to the “retentate fraction” as defined elsewhere herein when whole milk has been subjected to nanofiltration.
  • “low-fat milk concentrate” as used herein refers to the material retrieved after nanofiltration when subjecting perchlorate containing low-fat milk to nanofiltration defined elsewhere herein.
  • low-fat milk concentrate corresponds to the “retentate fraction” as defined elsewhere herein when low-fat milk has been subjected to nanofiltration.
  • whey refers to the serum or watery part of milk that is separated from the coagulable part or curd. “Whey” refers to milk that has been processed by curdling or straining.
  • Whey also refers to a fluid that is rich in lactose, minerals, and vitamins and contains proteins, soluble proteins and less than ⁇ 0.1% of fat, further on ingredients like alpha-lactalbumin, alpha-lactoglobin, lactoferrin, immunoglobulins and including lactose as a pre-cursor substance for the probiotic galactooligosaccharides.
  • Whey has a typical dry mass of about 5% to about 7%, preferably about 6%, and a fat content of ⁇ 0.1% (see Technologie der Milch für, Edgar Spreer, BehrsVerlag, ISBN 978-3-89947-841-9, 10 th completely revised edition 2011, unchanged reprinting 2015).
  • “Whey” is preferably sweet whey or sour whey.
  • the term “whey”, as used herein, can also refer to the permeate of microfiltration of milk, which can be used analog as whey.
  • Permeate from milk filtration (MF) of skim milk is the fraction that contains an decreased solids mass percentage or dry mass, as defined elsewhere herein, (as compared to the original milk) of b-casein.
  • Whey protein is the collection of globular proteins isolated from whey consisting of a-lactalbumin, b-lactoglobulin, serum albumin, immunoglobulins, Lactoferrin, and traces of glycol-macropeptides of casein.
  • whey concentrate refers to the material retrieved after nanofiltration when subjecting perchlorate containing whey to nanofiltration defined elsewhere herein. Accordingly, the term “whey concentrate” corresponds to the “retentate fraction” as defined elsewhere herein when whey has been subjected to nanofiltration.
  • the milk product according to the present invention may further be pre-treated before subjected to nanofiltration.
  • pre-treated refers to any industrial process applied before subjecting the milk product to nanofiltration, for example pasteurization (heat- treatment) or microfiltration to reduce microorganisms.
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” according to the invention may be pre-treated milk or whey that has undergone heat and durability treatment, or milk or whey that has undergone only moderate heat and durability treatment.
  • the milk product is an organic milk product such as organic milk, preferably organic skim milk, organic whole milk or organic whey.
  • fat-containing milk products such as whole milk or low-fat milk may be pre-treated by means of homogenization.
  • the dry mass of the perchlorate containing milk product such as milk or whey can be increased by a nanofiltration step to a dry mass of for example 16%, then transported and subjected to a second nanofiltration step to increase the dry mass to 32%.
  • the dry mass content of the milk concentrate or the obtained whey concentrate can be reduced by dilution for further processing steps and for adjusting the dry mass of the obtained milk or whey concentrate to the dry mass content of the perchlorate containing milk or whey before the first nanofiltration step in order to assess the amount of perchlorate reduction.
  • the milk product can be dried and dissolved again with water before subjected to nanofiltration.
  • a powdered milk product or dried milk product is a manufactured dairy product made by evaporating milk to dryness.
  • One purpose of drying milk is to preserve it since milk powder has a far longer shelf life than liquid milk and does not need to be refrigerated, due to its low moisture content.
  • Another purpose is to reduce its bulk for economy of transportation.
  • a powdered milk product or dried milk product is preferably made by skim milk, but can also made by concentrated milk, ultrafiltered milk, diafiltered milk, micro-filtered milk or pasteurized skim milk or skim milk with extended shelf live or skim milk processed with high temperature heating, low temperature and long-time heating, high temperature and short-time heating, ultra-high temperature heating.
  • a powdered milk product or dried milk product is preferably whey powder but can also be made by sweet whey or sour whey, whey of caseinate or permeate of microfiltration with whey protein. But it can also made by concentrated whey, ultrafiltered whey, diafiltered whey, micro-filtered whey, demineralized whey by ion exchange or electro dialysis or pasteurized whey or whey with extended shelf live or whey processed with high temperature heating, low temperature and long-time heating, high temperature and short-time heating, ultra-high temperature heating.
  • the perchlorate containing milk product to be subjected to nanofiltration can also be a perchlorate containing dried milk product or a perchlorate containing powdered milk product, and/or a dried or powdered milk product assumed to contain perchlorate, such as dried or powdered milk or whey.
  • a dried milk product or a powdered milk product cannot directly be subjected to nanofiltration and has to be solved again prior to the nanofiltration step as described herein above.
  • the dried milk product or powdered milk product is diluted with a perchlorate-free solvent described elsewhere herein to at least 2.5% dry matter to be subjected to nanofiltration.
  • a "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration in the context of the present invention refers to liquid milk, i.e. milk having a dry mass of at least 2.5% and not more than 20%.
  • the "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration according to the present invention comprises between about 5% and about 13% dry matter as defined elsewhere herein. More preferred, the "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration according to the present invention comprise between about 5% and about 7% dry matter as defined elsewhere herein.
  • the "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration according to the present invention comprise between about 8% and about 10% dry matter as defined elsewhere herein.
  • the "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration according to the present invention comprise between about 8% and about 13% dry matter as defined elsewhere herein.
  • the "perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” subjected to nanofiltration according to the present invention is about 6% or about 9% dry matter as defined elsewhere herein.
  • a “perchlorate depleted milk product” manufactured by the processes of the present invention refers to both liquid and dry milk. Therefore, in the context of the present invention the perchlorate containing milk product and the perchlorate depleted milk product as defined elsewhere herein which are subjected to nanofiltration according to the present invention comprise at least 2.5% dry matter.
  • the obtained retentate fraction can then again be solved or contacted with the perchlorate-free solvent described elsewhere herein and subjected to a further nanofiltration step as described elsewhere herein.
  • said contacting with the perchlorate-free solvent and subsequent nanofiltration are repeated as often as necessary, i.e.
  • the retentate fraction has a dry mass between about 5% and about 13% as defined elsewhere herein, preferably a dry mass between about 5% and about 7%, a dry mass between about 8% and about 10% or a dry mass between about 8% and 13% as defined elsewhere herein, more preferred a dry mass of about 6% or about 9% as defined elsewhere herein.
  • the perchlorate content is reduced to less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb, specifically when the retentate fraction
  • the nanofiltration step(s) according to the present invention can also reduce the content of other unwanted compounds such as chlorate and bromide.
  • the perchlorate-free solvent is also free of chlorate and bromide.
  • the chlorate and bromide content of said the retentate fraction is reduced to less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01
  • the perchlorate depleted retentate fraction comprises no detectable amount of perchlorate after being contacted with the perchlorate-free solvent and subsequent repeated nanofiltration step(s). More preferred, the perchlorate depleted retentate fraction comprises no detectable amount of perchlorate, chlorate and bromide after being contacted with the perchlorate-free solvent that is also chlorate- and bromide-free and subsequent repeated nanofiltration step(s).
  • the nanofiltration conditions/parameters applied in a further nanofiltration step or further nanofiltration steps can be the same as in the previous nanofiltration step, or can vary between the single nanofiltration steps.
  • the same parameters set for the first nanofiltration are also used for the subsequent nanofiltration step.
  • a “perchlorate containing milk product” can also be diluted prior to be subjected to nanofiltration.
  • Such diluted milk product comprises at least 2.5% dry mass in total.
  • the milk product is diluted in the perchlorate-free solvent described elsewhere herein.
  • perchlorate-free solvent as used in the context of the invention is preferably essentially free of perchlorate. Essentially free means in this respect that the solvent comprises less than 0.1 ppb of perchlorate.
  • the “perchlorate-free solvent” comprises less than 0.09 ppb, more preferred less than 0.08 ppb, even more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb, still more preferred less than 0.009 ppb, still more preferred less than 0.008 ppb, still more preferred less than 0.007 ppb, still more preferred less than 0.006 ppb, still more preferred less than 0.005 ppb, still more preferred less than 0.004 ppb, still more preferred less than 0.003 ppb, still more preferred less than 0.002 ppb, still more preferred less than 0.001 ppb.
  • the “perchlorate-free solvent” comprising 0 ppb perchlorate.
  • the “perchlorate-free solvent” as used in the context of the invention is also essentially free of chlorate and bromide. Essentially free means in this respect that the solvent comprises less than 0.1 ppb of chlorate.
  • the “perchlorate-free solvent” comprises less than 0.09 ppb, more preferred less than 0.08 ppb, even more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb, still more preferred less than 0.009 ppb, still more preferred less than 0.008 ppb, still more preferred less than 0.007 ppb, still more preferred less than 0.006 ppb, still more preferred less than 0.005 ppb, still more preferred less than 0.004 ppb, still more preferred less than 0.003 ppb, still more preferred less than 0.002 ppb, still more preferred less than 0.001 ppb of chlorate, and less than 0.1 ppb, more preferred, less than 0.09 ppb, more preferred less than 0.08 ppb, even more preferred less than 0.07
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” in the context of the present invention may refer to all possible forms of (processed or pretreated) milk, such as whole milk, low-fat or skim milk, cream, ultrafiltered milk, diafiltered milk, micro-filtered milk, milk recombined from milk powder, organic milk, as well as whey, or a combination or dilution of any of these.
  • the milk from which said milk product originates from may be obtained from cow, sheep, goat, camel, horse, donkey or any other mammal producing milk suitable for human nourishment.
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” is milk such as skim milk, whole milk or low-fat milk.
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” is whey.
  • the milk product according to the present invention is preferably an organic milk product.
  • the milk from which the milk product originated is organic milk from livestock raised according to methods and/ or organic farming law.
  • the understanding of “organic milk” in the context of the present invention entirely refers to the criteria as defined in the Regulation (EG) No.
  • organic milk is milk from cows that are not prophylactically treated with antibiotics, that are not given prophylactic growth or reproduction hormones and that receive at least 50% of their food from their own farm or from pasture.
  • Organic milk may also comprise a combination of milk from different animal origins specified above.
  • Said “perchlorate containing milk product” or “milk product assumed to contain perchlorate” preferably originates from milk from dairies.
  • the milk is preferably skimmed prior to nanofiltration, which means it is depleted of fats, and preferably, it is deprived of fats to contain less than 0.1% of the original fat content.
  • the “perchlorate containing milk product” and/or “milk product assumed to contain perchlorate” is preferably organic skim milk, organic whole milk, organic low-fat milk or organic whey.
  • perchlorates are of primary commercial interest: ammonium perchlorate (NH 4 CI0 4 ), perchloric acid (HCI0 4 ), potassium perchlorate (KCI04), and sodium perchlorate (NaCI0 4 ), which can all result in increased environmental perchlorate exposure.
  • perchlorate (CI0 4 ) is the anion resulting from the dissociation of perchloric acid (HCI0 4 ) and its salts upon their dissolution in water, and has a molecular weight of 0.09944KDa.
  • Perchlorate (CI0 4 ) has the largest atomic volume per mole (74.7 qcm/mol) and the largest atomic mass (99.449 Dalton) of all ions in the milk (see Table 2). Many perchlorate salts are also soluble in non-aqueous solutions (Vogt et al. 2002, Wiley- VCH. doi: 10.1002/14356007. a06_483).
  • molecular weight refers to the mass of a molecule and is calculated as the sum of the relative atomic masses of each constituent element multiplied by the number of atoms of that element in the molecular formula.
  • Kilodalton refers to the unified atomic mass unit or Dalton (symbol: u, or Da or AMU), which is a standard unit of mass that quantifies mass on an atomic or molecular scale (atomic mass).
  • Dalton symbol: u, or Da or AMU
  • One unified atomic mass unit is approximately the mass of one nucleon (either a single proton or neuron) and is numerically equivalent to 1g/mol.
  • Water soluble contaminants are chemical substances (also called solute) which have the ability to dissolve in a solvent.
  • water soluble contaminants are chemicals substances able to dissolve in water.
  • Some ionic compounds (salts) dissolve in water, because of the attraction between positive and negative charges.
  • a salt's positive ions e.g. Ag +
  • the salt's negative ions e.g. Cl
  • an ionic contaminant may be water-soluble and can be found in milk.
  • Example of the water soluble contaminants that could be additionally depleted from the milk using the process and method described herein are, for example diethanolamin, triethanolamin and other surfactants, bromide, and chlorate.
  • the methods of the present invention are suitable for the depletion of chlorate and/or bromide as described elsewhere herein.
  • the perchlorate containing milk product and/or milk product assumed to contain perchlorate as defined elsewhere herein is subjected to nanofiltration making use of a ceramic nanofiltration membrane to obtain a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product defined elsewhere herein, i.e. the perchlorate penetrates through the ceramic nanofiltration membrane into the permeate fraction.
  • the perchlorate- depleted milk product defined elsewhere herein is retained in the retentate fraction.
  • a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product is obtained by said process.
  • the term “subjected to a nanofiltration step” as used in the context of the present invention refers to the fact that nanofiltration that makes use of a nanofiltration module comprising a ceramic nanofiltration membrane as described elsewhere herein is used to deplete perchlorate from a perchlorate containing milk product and/or a milk product assumed to contain perchlorate to reduce unwanted impurities, specifically perchlorate.
  • nanofiltration technology
  • nanofiltration comprising a ceramic nanofiltration membrane as described elsewhere is applied to said perchlorate containing milk product and/or milk product assumed to contain perchlorate, thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product.
  • NF nanofiltration
  • Membrane filtration processing as applied in the context of the present invention refers to a technique that allows the concentration and separation of substances with the use of pressure and specially designed semi-permeable membranes.
  • particles are separated on the basis of their molecular size and shape and concentration, depending on the product properties e.g. pH, ionic strength, viscosity, surface activity, chemical and physical characteristics.
  • a semipermeable membrane is a type of membrane that will allow certain molecules or ions to pass through it by diffusion or occasionally by more specialized processes. How the membrane is constructed to be selective in its permeability will determine the rate and the permeability.
  • nanofiltration when applied to a milk product as defined herein, gives a minimum reduction of perchlorate of at least 35%, preferably of at least 39%, even more preferred of at least 45%, without the need for further testing.
  • value-determining substances such as lactose (0.342297 kDa) are retained in the retentate, while not valuable compounds like perchlorate, diethanolamine, triethanolamine, bromide and chlorate are additionally depleted from the retentate fraction.
  • the nanofiltration step makes use of a ceramic nanofiltration membrane.
  • the methods and processes for the manufacture of a perchlorate depleted milk product make use of a ceramic nanofiltration membrane. “Make use” means that a ceramic nanofiltration membrane is applied for the nanofiltration step to which the perchlorate containing milk product and/or a milk product assumed to contain perchlorate is subjected.
  • the term “ceramic” refers to inorganic and non-metallic materials that receive their material properties through a special temperature treatment such as firing or sintering and generally retain their shape at room temperature.
  • ceramic also includes technical ceramics, which can be divided into silicate ceramics, oxide ceramics and non-oxide ceramics a described for example by the “Ceramic associations for technical ceramics” (http://www.keramvious.de).
  • Silicate ceramics can be subdivided into alkali aluminium silicates, magnesium silicates, alkaline earth aluminium silicates and zircon porcelains, porous aluminium silicates, magnesium silicates and mullite ceramics with a low alkali content.
  • Oxide ceramics can be subdivided into ceramic materials with a high aluminium content and oxide ceramic materials of other types.
  • Non-oxide ceramics can be divided into carbides, as well as nitrides and "non-oxide ceramic insulating materials”.
  • the classes described above are subdivided by DIN EN 60672 into C classes 100-900.
  • the best-known materials of the silicate ceramics include, for example, porcelain, steatite, cordierite and mullite.
  • Representatives of oxide ceramics are, for example, aluminum oxide, magnesium oxide, zirconium oxide, silicon oxide and titanium oxide.
  • ceramic nanofiltration membranes are preferably out of the elements aluminum (Al), carbon (C), oxygen (O), nitrogen (N), titanium (Ti), zirconium (Zr), silicon (Si) and magnesium (Mg) and their combinations.
  • the ceramic nanofiltration membrane is made out of oxide ceramics.
  • the ceramic nanofiltration membrane is made out of aluminum trioxide (Al 2 0 3 ), magnesium oxide (MgO), titanium dioxide (Ti0 2 ), titanium trioxide (Ti 2 0 3 ), zirconium dioxide (Zr0 2 ), zirconiumtrioxide (Zr 2 0 3 ), silicon dioxide (Si0 2 ) or titanium dioxide (Ti0 2 ).
  • the ceramic nanofiltration membrane is made out of silicon dioxide or titanium dioxide, more preferred of titanium dioxide.
  • Ceramic nanofiltration membranes used in the context of the methods and processes of the present invention can be ceramic membranes of various forms such as plates, discs, both single layer or with channels or tubes, single or multichannel tubes or spiral wound membranes.
  • the membranes can be set alone, in parallel and/or lined up.
  • the elements can be used for cross-flow, dead end or laminar flow filtration. Typically, one or multiple elements are combined in one stainless steel case to form a module that is used for the nanofiltration process. Contrary to synthetic nanofiltration membranes, ceramic nanofiltration membranes are generally without charge.
  • Ceramic nanofiltration membranes applicable in the context of the present invention may have a mean pore size between 0.1 and 10 nm, preferably a mean pore size between 0.5 and 3 nm.
  • the mean pore size is between 0.7 and 1.1 nm. It is particularly envisaged to make use of a ceramic nanofiltration membrane having a molecular weight cut-off about between about 150 and 1000 Daltons. More preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 750 Daltons. Even more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 300 and 600 Daltons. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 450 Daltons. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 250 Daltons.
  • the used ceramic nanofiltration membrane has a molecular weight cut-off at about 200 Da or about 450 Daltons, with about 200 Da being preferred.
  • About means in this respect that the cut-off may vary by 5%, but also includes the concrete number, e.g., about 450 Da includes 450 Da and about 200 Da includes 200 Da.
  • the molecular weight cut-off or MWCO refers to the lowest molecular weight solute (in Daltons) in which 90% of the solute is retained by the membrane, or the molecular weight of the molecule that is 90% retained by the membrane.
  • Ceramic nanofiltration membranes applicable in the context of the present invention may have variable lengths of up to 10 m or even more. However, also shorter membrane as described for example in Example 1 are applicable.
  • the ceramic nanofiltration membrane may in principle operate at a pH range from about 0 to 14 at temperatures below ( ⁇ ) 20°C.
  • the ceramic nanofiltration membrane operates at a pH range of the perchlorate containing milk product as described elsewhere herein.
  • the transmembrane pressure (maximum operating pressure) during nanofiltration with a ceramic nanofiltration membrane can be up to 40bar.
  • the maximum operating temperature with other fluids than milk products can be up to 200°C.
  • the ceramic nanofiltration membrane used is able to deplete perchlorate (0.09944 kDa) from the perchlorate containing milk product and/or the milk product assumed to contain perchlorate described elsewhere herein.
  • the perchlorate will pass through the ceramic nanofiltration membrane, leaving a retentate fraction depleted in perchlorate and a permeate fraction containing perchlorate.
  • the ceramic nanofiltration membrane used in the context of the present invention is characterized in that it depletes at least 35%, preferably at least 39%, even more preferred at least 45% from perchlorate containing milk product by a nanofiltration step as specified elsewhere herein.
  • the nanofiltration membrane When subjecting the milk product described elsewhere herein to a nanofiltration step making use of a ceramic nanofiltration membrane, the nanofiltration membrane gives a minimum reduction of perchlorate of at least 35%, preferably at least 39%, even more preferred at least 45% in the above mentioned process without the need for further testing.
  • the ceramic nanofiltration membrane is particularly able to deplete perchlorate from the milk product at the pH value and conductivity characteristic of said milk product, i.e. preferably at a pH value between 3.5 and 9.
  • the ceramic nanofiltration membrane is particularly able to deplete perchlorate from the milk at the pH value and conductivity characteristic of milk, i.e. preferably at a pH value between 5 and 9, more preferred at a pH between 6 and 8.
  • the ceramic nanofiltration membrane is also particularly able to deplete perchlorate from whey at the pH value and conductivity characteristic of whey, i.e. preferably at a pH value between 3.5 and 6.5, wherein the pH of sweet whey is at or above 5.6 and the pH of sour whey is below 5.6.
  • pH refers to the measure of how acidic or alkaline a substance is. pH is a scale of acidity or in other words a measure of the concentration of protons (H + ) in a solution.
  • the conductivity is suggested between 3 and 7 of the filtered material.
  • Electrode conductivity refers to the measure of a material's ability to allow the transport of an electric charge. Electrical conductivity is measured in siemens per meter, it is the ratio of the current density to the electric field strength. It is equivalent to the electrical conductance measured between opposite faces of a 1 -metre cube of the material under test. The symbol for electrical conductivity is k (kappa), and also o (sigma) or g (gamma). Electrical conductance is an electrical phenomenon where a material contains movable particles with electric charge (such as electrons), which can carry electricity. When a difference of electrical potential is placed across a conductor, its electrons flow, and an electric current appears.
  • a conductor such as a metal has high conductivity, and an insulator like glass or a vacuum has low conductivity.
  • a semiconductor has a conductivity that varies widely under different conditions. Electrical conductivity is the reciprocal (or inverse) of electrical resistivity.
  • a pH value between 6 and 8 and a conductivity between 4.5-6.5 mS/cm are preferred.
  • ceramic nanofiltration membranes have no charge or membrane tension.
  • a ceramic nanofiltration membrane refers to any a ceramic membrane which is suitable for nanofiltration of perchlorate from a perchlorate containing milk product. Further, the ceramic nanofiltration membrane used according to the present invention retains monovalent salts.
  • the ceramic nanofiltration membrane used in the processes of the present invention is an single module Inopor® nanofiltration membrane of type EKR made of titanium oxide with a molecular weight cut off of 450 Dalton, an average pore size of 0.9 nm, an outer module diameter of 10 millimeter, a module length of 1200 millimeter and a filtration area of 0.0264m 2 per test run, or a ceramic nanofiltration membrane that has similar filtration characteristics (see Example 1).
  • the ceramic nanofiltration membrane used in the processes of the present invention is an single module Inopor® nanofiltration membrane of type EKR made of titanium oxide with a molecular weight cut off of 200 Dalton, an outer module diameter of 10 millimeter, a module length of 1200 millimeter and a filtration area of 0.0264m 2 per test run, or a ceramic nanofiltration membrane that has similar filtration characteristics (see Example 1).
  • the used ceramic nanofiltration membrane is characterized by lactose and protein rejection in one nanofiltration step as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the used nanofiltration membrane can be characterized by magnesium rejection by at least 80%, preferably at least 92% and/or calcium rejection by at least 80%, preferably at least 89% as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the used nanofiltration membrane can be further characterized by depleting at least 40%, more preferred at least 46% of the contained chlorate and/or at least 30%, preferably at least 35% of the contained bromide in one nanofiltration step as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the used nanofiltration membrane can be further characterized in that it depletes at least 35%, preferable at least 39%, more preferred at least 45% of the contained perchlorate as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the used nanofiltration membrane can be characterized by an up to 41%, preferably up to 50% or more reduced content of sodium and/or an up to 41% or more reduced content of potassium as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the used nanofiltration membrane can be characterized by depleting at least 40%, preferably at least 45%, more preferred at least 50%, even more preferred at least 52%, still more preferred at least 56%, still more preferred at least 63%, still more preferred at least 68% of the contained chloride in one nanofiltration step as defined elsewhere herein for the conduction of predetermined process parameters, which is fully applicable for specifying the used nanofiltration membrane.
  • the nanofiltration membrane applied in the context of the processes of the present invention and characterized by perchlorate depletion, preferred lactose and protein rejection, preferred magnesium and/or calcium rejection, preferred sodium and/or potassium reduction and preferred chloride depletion as defined herein above is a ceramic nanofiltration membrane having a molecular weight cut-off between about 200 and 250 Daltons, preferably at about 200 Da.
  • the processes for the manufacture of a perchlorate depleted milk product can be applied to various types of perchlorate containing milk products, such as perchlorate containing milk and perchlorate containing whey (see Example 1 and Tables 1A to 1G).
  • the present invention also refers to a process for the manufacture of a perchlorate depleted milk, preferably perchlorate depleted skim milk, or a perchlorate depleted whey (from said perchlorate containing milk or whey), comprising the steps as described elsewhere herein.
  • perchlorate containing skim milk contains 2 ppb or more than 2 ppb perchlorate when the dry mass of the skim milk is between about 8% and about 10% as defined elsewhere herein.
  • perchlorate depleted skim milk contains less than 2 ppb perchlorate when the dry mass of the skim milk is between about 8% and about 10%.
  • perchlorate containing whey contains 2 ppb or more than 2 ppb perchlorate when the dry mass of the whey is between about 5% and about 7%.
  • perchlorate depleted whey contains less than 2 ppb perchlorate when the dry mass of the whey is between about 5% and about 7%.
  • the lactose and protein content of said skim milk after applying the nanofiltration technique described herein is maintained by 95%, more preferred by 95.5%, even more preferred by 96%, still more preferred by 96.5%, still more preferred by 97.0%, still more preferred by 97.5%, still more preferred by 98%, still more preferred by 98.5%, still more preferred by 99%, still more preferred by 99.2%, still more preferred by 99.3%, still more preferred by 99.4%, still more preferred by 99.5%, still more preferred by 99.6%, still more preferred by 99.7%, still more preferred by 99.8%, still more preferred by 99.9%.
  • lactose and protein content of said skim milk after applying the nanofiltration technique described elsewhere herein is maintained by 100%.
  • lactose and protein contained in a perchlorate containing skim milk and/or skim milk assumed to contain perchlorate means that the content of lactose and protein is determined in the perchlorate containing skim milk (before nanofiltration) and after in perchlorate depleted skim milk subjected to nanofiltration (i.e. after nanofiltration) both refer to the same dry mass, i.e.
  • the dry mass of the perchlorate depleted skim milk is recalculated to the dry mass of the perchlorate containing skim milk (before nanofiltration), and the lactose and protein content values are compared as described elsewhere herein.
  • the nanofiltration membrane is characterized by magnesium rejection by at least 80%, preferably at least 95% and/or calcium rejection by at least 80%, preferably at least 89%, preferably by a nanofiltration step as defined herein.
  • a magnesium rejection by at least 80% means that 20% or less than 20% of the contained magnesium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • a magnesium rejection by at least 80% means that 20% or less than 20% of the contained magnesium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the rejection of at least 80% means that the contained magnesium is rejected by 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane rejects at least 80% of the contained magnesium in one nanofiltration step.
  • a calcium rejection by at least 80% means that 20% or less than 20% of the contained calcium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the rejection of at least 80% means that the contained calcium is rejected by 80%, 85%, 90%, 92%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane rejects at least 80% of the contained calcium in one nanofiltration step. More preferred at least 85%, even more preferred at least 90%, still more preferred at least 92%, still more preferred at least 95%, still more preferred at least 97%, still more preferred at least 98%, still more preferred at least 99% of the contained calcium is rejected in one nanofiltration step. Most preferred 100% of the contained calcium is rejected in one nanofiltration step.
  • the nanofiltration membrane is characterized in that it depletes at least 40%, preferably at least 46%, more preferred at least 50% of the contained chlorate and/or at least 45%, preferably at least 53% of the contained bromide, preferably by a nanofiltration step as defined herein.
  • a depletion of at least 50% of the contained chlorate means that 50% or less than 50% of the contained chlorate is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 50% means that the contained chlorate is depleted by 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane depletes at least 50% of the contained chlorate in one nanofiltration step.
  • a depletion of at least 45% of the contained bromide means that 45% or less than 45% of the contained bromide is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 45% means that the contained bromide is depleted by 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane depletes at least 45% of the contained bromide in one nanofiltration step.
  • the nanofiltration membrane is characterized in that it depletes at least 45% of the contained perchlorate, preferably by a nanofiltration step as defined herein.
  • a depletion of at least 45% of the contained perchlorate means that 55% or less than 55% of the contained perchlorate is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 45% means that the contained perchlorate is depleted by 45%, 50,%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane depletes at least 45% of the contained perchlorate in one nanofiltration step.
  • the used ceramic nanofiltration membrane has a molecular weight cut-off between about 150 and 1000 Da, preferably between about 200 and about 750 Da, more preferred between about 300 and 600 Da, still more preferred at about 450 Da. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 450 Daltons. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut off between about 200 and 250 Daltons.
  • the used ceramic nanofiltration membrane has a molecular weight cut-off at about 200 Da or about 450 Daltons, with about 200 Da being preferred.
  • the nanofiltration membrane is characterized by lactose and protein rejection as described elsewhere herein.
  • the lactose and protein content of said whey after applying the nanofiltration techniques described herein is maintained by 95%, more preferred by 95.5%, even more preferred by 96%, still more preferred by 96.5%, still more preferred by 97%, still more preferred by 97.5%, still more preferred by 98%, still more preferred by 98.5%, still more preferred by 99%, still more preferred by 99.2%, still more preferred by 99.3%, still more preferred by 99.4%, still more preferred by 99.5%, still more preferred by 99.6%, still more preferred by 99.7%, still more preferred by 99.8%, still more preferred by 99.9%.
  • lactose and protein content of said milk after applying the nanofiltration technique described elsewhere herein is maintained by 100%.
  • lactose and protein contained in perchlorate containing whey and/or whey assumed to contain perchlorate are maintained means that the content of lactose and protein is determined in perchlorate containing whey (before nanofiltration) and after in perchlorate depleted whey subjected to nanofiltration (i.e. after nanofiltration) both having the same dry mass, and these values are compared as described elsewhere herein.
  • the nanofiltration membrane is characterized in that it rejects at least 80%, preferably at least 92% of the contained magnesium and/or calcium, preferably by a nanofiltration step as defined herein.
  • a rejection of at least 80% of the contained magnesium and calcium means that 20% or less than 20% of the contained magnesium and calcium is depleted by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the nanofiltration membrane is characterized by magnesium and calcium rejection.
  • rejection as used in this regard has been specified elsewhere herein.
  • the magnesium and calcium content of said whey after applying the nanofiltration technique described herein is maintained by 95%, more preferred by 95.5%, even more preferred by 96%, still more preferred by 96.5%, still more preferred by 97%, still more preferred by 97.5%, still more preferred by 98%, still more preferred by 98.5%, still more preferred by 99%, still more preferred by 99.2%, still more preferred by 99.3%, still more preferred by 99.4%, still more preferred by 99.5%, still more preferred by 99.6%, still more preferred by 99.7%, still more preferred by 99.8%, still more preferred by 99.9%. Most preferred the magnesium and calcium content of said whey after applying the nanofiltration technique described elsewhere herein is maintained by 100%.
  • magnesium and calcium contained in perchlorate containing whey and/or whey assumed to contain perchlorate means that the content of magnesium and calcium is determined in perchlorate containing whey (before nanofiltration) and after in perchlorate depleted whey subjected to nanofiltration (i.e. after nanofiltration) both having the same dry mass, and these values are compared as described elsewhere herein.
  • the nanofiltration membrane is characterized in that it depletes at least 40%, more preferred at least 45%, even more preferred at least 46%, still more preferred at least 68%, still more preferred at least 71% of the contained chlorate and/or at least 30%, preferably at least 35% of the contained bromide, preferably by a nanofiltration step as defined herein.
  • a depletion of at least 45% of the contained chlorate means that 55% or more than 55% of the contained chlorate is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 45% means that the contained chlorate is depleted by 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane depletes at least 45% of the contained chlorate in one nanofiltration step.
  • the depletion of at least 35% means that the contained bromide is depleted by 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied (predetermined) process parameters deplete at least 35% of the contained bromide in one nanofiltration step.
  • the nanofiltration membrane is characterized in that it depletes at least 35%, preferably at least 39%, more preferred at least 52%, even more preferred at least 59% of the contained perchlorate, preferably by a nanofiltration step as defined herein.
  • a depletion of at least 35% of the contained perchlorate means that 65% or less than 65% of the contained perchlorate is rejected by the nanofiltration membrane used in the context of the invention, i.e. one nanofiltration step.
  • the depletion of at least 35% means that the contained perchlorate is depleted by 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 98%, 99% or even 100%.
  • the applied nanofiltration membrane depletes at least 35% of the contained perchlorate in one nanofiltration step.
  • the used ceramic nanofiltration membrane has a molecular weight cut-off between about 150 and 1000 Da, preferably between about 200 and about 750 Da, more preferred between about 300 and 600 Da, still more preferred at about 450 Da. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 450 Daltons. Still more preferred, the used ceramic nanofiltration membrane has a molecular weight cut-off between about 200 and 250 Daltons. It is also particularly envisaged that the used ceramic nanofiltration membrane has a molecular weight cut-off at about 200 Da or about 450 Daltons, with about 200 Da being preferred.
  • the nanofiltration process may comprise crossflow filtration, which is a type of filtration (using a particular unit operation).
  • cross-flow membrane filtration is used to mean a class of filtration that typically produces two effluent streams, permeate and retentate.
  • Cross-flow filtration gets its name because the majority of the feed flow travels tangentially across the surface of the filter, rather than into the filter.
  • the nanofiltration process may be a continuous process.
  • the nanofiltration process according to the invention can be used for feeds containing a high proportion of small particle size solids (where the permeate is of most value) because solid material can quickly block (blind) the filter surface.
  • Transmembrane pressure is a measure of pressure difference between two sides of a membrane. With crossflow filtration the tangential motion of the bulk of the fluid across the membrane causes trapped particles on the filter surface to be rubbed off. This means that a crossflow filter can operate continuously at relatively high solids loads without blinding.
  • perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration results in perchlorate-depleted retentate fraction and a perchlorate containing permeate fraction of said milk product.
  • the “permeate fraction” as described in the context of the invention designates the liquid passing through the nanofiltration membrane defined herein, while the “retentate fraction” or “concentrate” or “skim milk concentrate” or “whey concentrate” designates the fraction not passing through the nanofiltration membrane.
  • the term “permeate” therefore is used to mean, in relation to a filtration process, that liquid product of filtration of said milk product which contains only those milk product components that are able to pass through the filtration membrane.
  • the permeate fraction is therefore remaining fluid that has become enriched with compounds that could permeate the membrane.
  • the "retentate” is used to mean, in relation to a filtration process, the product of filtration of said milk product which is the concentrated milk product feed and which contains all the components typically found in said milk product, but with an increased solids mass percentage (as compared to the original milk product) of protein, fat, and minerals (ash).
  • cross-flow membrane filtration is used to mean a class of filtration that typically produces two effluent streams, permeate and retentate.
  • the retentate fraction of the milk product of the present invention will contain, after nanofiltration, less than 4 ppb perchlorate when the retentate fraction has a dry mass of about 10% to about 26%, i.e. the retentate fraction is perchlorate depleted. Therefore, the retentate fraction comprises the perchlorate-depleted milk product as defined elsewhere herein.
  • the retentate fraction also contains lactose.
  • the permeate fraction of the present invention will contain, after nanofiltration, 2 ppb or more than 2 ppb perchlorate, i.e. is perchlorate containing.
  • the permeate fraction typically comprises a perchlorate-containing aqueous salt solution.
  • the retentate fraction and/or the permeate fraction as defined herein and obtained by the process described herein are analyzed to evaluate the perchlorate content.
  • Methods for analyzing or measuring the content of perchlorate in a solution are known to those skilled in the art and are also described elsewhere herein.
  • evaluation of the perchlorate contained in the permeate and/or retentate fractions can be carried out by using ion chromatography-suppressed conductivity (IC-CD) and/or ion chromatography-electrospray mass spectrometry (IC-MS), as described inter alia by Kirk et al.
  • IC-CD ion chromatography-suppressed conductivity
  • IC-MS ion chromatography-electrospray mass spectrometry
  • Evaluation of perchlorate content of the permeate and/or retentate fraction can also be measured by using hydrophilic interaction chromatography-tandem mass spectrometry, as described by the patent application CN106324144. In the context of the present invention, evaluation of perchlorate content may be carried out before and/or after the step of nanofiltration.
  • a perchlorate free solvent refers to any solvent applicable to liquefy or dilute milk and includes, but is not limited to, water, perchlorate depleted milk, a buffer, a mixture or any combination thereof.
  • the milk diluted with any perchlorate free solvent comprises at least 2.5% dry mass in total.
  • the “perchlorate-free solvent” is preferably water. As described elsewhere herein, the perchlorate free solvent is preferably also free of chlorate and bromide.
  • the retentate fraction is subjected to (a) further step(s) of nanofiltration, as mentioned also elsewhere herein.
  • subsequent nanofiltration steps may include the same or varied parameters, which may dependent on the origin of the perchlorate containing milk product or milk product assumed to contain perchlorate subjected to nanofiltration.
  • the nanofiltration step(s) as often as necessary to reach a final concentration/level of perchlorate, i.e. as often as to reduce the perchlorate content down to less than 2 ppb, when the retentate fraction has a dry mass between about 5% and about 13% as defined elsewhere herein, preferably about 6% or about 9%.
  • the perchlorate content is reduced to less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb, specifically when the retentate fraction has
  • the perchlorate retentate fraction comprises no detectable amount of perchlorate after said contacting with the perchlorate-free solvent and subsequent repeated nanofiltration steps. It is also envisaged in this respect to repeat the nanofiltration step(s) as often as necessary to reach a final concentration/level of chlorate and/or bromide, i.e. as often as to reduce the chlorate and/or bromide content down to less than 2 ppb, when the retentate fraction has a dry mass between about 5% and about 13% as defined elsewhere herein, preferably about 6% or about 9%.
  • the perchlorate content is reduced to less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb, specifically when the retentate fraction has
  • the nanofiltration step as described herein is repeated at least one time, more preferred between two and fifty times.
  • the perchlorate containing milk product and/or milk product assumed to contain perchlorate according to the present invention is subjected to 1 , 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, 25, 30, 35, 40, 45, 50 or even more nanofiltration steps in total.
  • the nanofiltration step is repeated until the most preferred value of less than 0.001 ppb perchlorate is reached.
  • the nanofiltration step is repeated until the most preferred value of less than 0.001 ppb chlorate and/or bromide is reached.
  • one nanofiltration step can comprise usage of several nanofiltration membranes/modules stacked in parallel.
  • the nanofiltration steps can be consecutively applied to further deplete or reduce perchlorate from the retentate fraction obtained in the previous nanofiltration step.
  • the amount of nanofiltration steps applied depends on the initial amount/content of perchlorate in the milk product subjected to nanofiltration, i.e. the more perchlorate is contained in the milk product or is assumed to be contained in the milk product subjected to nanofiltration, the more nanofiltration steps are applied.
  • the perchlorate depleted retentate fraction obtained by the processes of the present invention i.e. by subjecting the perchlorate containing milk and/or the milk assumed to contain perchlorate to a nanofiltration step, is contacted with a perchlorate free solvent and additionally or alternatively to a further nanofiltration step subjected to one or more steps of diafiltration.
  • Diafiltration is a dilution process that involves removal or separation of components (permeable molecules like salts, small proteins, solvents etc.) of a solution based on their molecular size by using micro-molecule permeable filters in order to obtain pure solution.
  • the retentate fraction is being mixed with a perchlorate free solvent and subjected to continuous diafiltration.
  • the retentate fraction may be subjected to one or more diafiltration cycles wherein the nanofiltration retentate is combined with a diafiltration liquid, which is the perchlorate free solvent defined elsewhere herein, and the combination of nanofiltration retentate and diafiltration liquid is subjected to subsequent nanofiltration and concentration steps.
  • diafiltration liquid is added to the nanofiltration sample feed reservoir, preferably at the same rate as filtrate is generated.
  • discontinuous diafiltration the solution is first diluted and then concentrated back to the starting volume.
  • the "diafiltration volume” (or “diavolume”) is defined herein as the volume of filtrate recovered in comparison to the amount of NF- retentate.
  • the volume of filtrate removed is equal to the volume of retentate when diafiltration operations began, 1 diavolume has been processed. Accordingly, the term “diafiltration cycle” refers to the processing, i.e. removal and collection, of 1 diavolume from the NF sample feed reservoir.
  • Suitable liquids to be used as the diafiltration liquid in accordance with the present invention include water and aqueous solutions.
  • the diafiltration liquid is water or an aqueous fraction of the milk product.
  • the diafiltration liquid does not comprise the perchlorate containing permeate fraction.
  • the permeate fraction derived from the first nanofiltration step is not subjected to further processing.
  • the permeate fraction derived after nanofiltration applied as first purification method is preferably discarded.
  • the permeate fraction obtained from the nanofiltration step is not further used in the process for the manufacture of a perchlorate-depleted milk product and/or for the manufacture of a milk based infant formula (base).
  • the permeate fraction can be further processed and may afterwards return into the manufacture process.
  • the permeate can be subjected to reverse osmosis.
  • Reverse osmosis is a water treatment method traditionally known for removing salt from seawater or for purifying drinking water by membrane processing defined elsewhere herein.
  • reverse osmosis can be applied to the permeate fraction described herein, in order to obtain clean water from said permeate fraction.
  • Said clean water can be used for other application, e.g. can be used as washing water or as perchlorate free solvent which is applied in the context of the invention as described elsewhere herein.
  • the permeate can be subjected to diafiltration.
  • the described process for the manufacture of perchlorate depleted milk i.e. the described nanofiltration steps and techniques, can also be applied as intermediate step of reverse osmosis.
  • the present invention also envisages to further process the perchlorate depleted retentate fraction obtained by the processes for the manufacture of a perchlorate depleted milk product as defined elsewhere herein. It may be desirable to dry or otherwise condense the retentate fraction(s) that have been obtained by the methods described herein for ease of preservation, storage and transportation. To this aim, processing of the retentate fraction may comprise admixing, drying, and evaporation or condensed by reverse osmosis.
  • the obtained retentate fraction is processed to powder, i.e. is evaporated to dryness.
  • the drying process may be carried out by any method known to those skilled in the art, preferably by spray drying or freeze drying.
  • Spray-drying refers to any process involving breaking up liquid mixtures into small droplets (atomization) and rapidly removing solvent from the mixture in a spray-drying apparatus where there is a strong driving force for evaporation of solvent from the droplets.
  • Spray-drying in accordance with the present invention can suitably be done by spraying the perchlorate-depleted retentate into an atmosphere at a temperature of 120-230 °C, with a product temperature of about 60-90°C.
  • Freeze-drying or “lyophilization” is any method of cold-drying, which involves the freezing of the UF retentate liquid followed by the removal or evaporation, by sublimation, of the water.
  • Admixing refers to the process of mixing the retentate fraction with a drink or food product. Admixing may for example include mixing of the retentate fraction with whey powder, lactose, mineral and trace elements, vitamins, fat mixtures, special protein compositions, fatty acids, starch and amino acids, just to name some. The further processing of the perchlorate depleted retentate fraction may also include supplementation with a suitable fat source and other necessary components, such as trace elements and vitamins, set by the EU food legislation.
  • the perchlorate depleted retentate fraction obtained can also be further processed the way it is diluted by a diluting agent.
  • the diluting agent may include water and minerals, or purified water, or milk.
  • the diluting agent must be suitable for consumption.
  • the diluting agent is an agent upon which addition to the retentate fraction will result in a perchlorate depleted milk product as defined elsewhere herein.
  • the present invention also relates to a perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product as described elsewhere herein.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass of the retentate fraction is between about 10% and about 26%.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass of the retentate fraction is between about 10% and about 14%. It is further envisaged that said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass of the retentate fraction is between about 16% and about 20%.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass of the retentate fraction is between about 16% and about 26%.
  • a dry mass between about 10% and about 26% of the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product includes a dry mass of about 10%, about 11%, about 12%, about 13%, about 14%, about 15%, about 16%, about 17%, about 18%, about 19%, about 20%, about 21%, about 22%, about 23%, about 24%, about 25% or about 26% and any number in between.
  • a dry mass of a milk product between about 10% and about 26% as used in the context of the present invention further includes the concrete numbers of 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25% or 26% and any number in between.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between about 10% and about 14%, i.e. about 10%, about 11%, about 12%, about 13% or about 14% or any number in between.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between 10% and 14%, i.e. 10%, 11%, 12%, 13% or 14% or any number in between.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between about 16% and about 20%, i.e.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between 16% and 20%, i.e. 16%, 17%, 18%, 19% or 20% or any number in between.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between about 16% and about 26%, i.e. about 16%, about 17%, about 18%, about 19% or about 20%, about 21%, about 22%, about 23%, about 24%, about 25% or about 26% or any number in between.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by a perchlorate content of less than 4 ppb when the dry mass is between 16% and 26%, i.e. 16%, 17%, 18%, 19%, 20% 21%, 22%, 23%, 24%, 25% or 26% or any number in between.
  • a perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product containing less than 4 ppb of perchlorate when the dry mass of the perchlorate depleted retentate fraction is between about 10% and about 14% as defined herein is whey.
  • said perchlorate depleted retentate fraction containing less than 4 ppb of perchlorate when the dry mass of the said perchlorate depleted retentate fraction is between about 10% and about 14% is produced from perchlorate containing whey and/or whey assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 5% and about 7%.
  • said perchlorate depleted retentate fraction containing less than 4 ppb of perchlorate when the dry mass of the said perchlorate depleted retentate fraction is between about 16% and about 20% is produced from perchlorate containing skim milk and/or skim milk assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 8% and about 10%.
  • a perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product containing less than 4 ppb of perchlorate when the dry mass of the perchlorate depleted retentate fraction is between about 16% and about 26% as defined herein is whole milk or low-fat milk.
  • said perchlorate depleted retentate fraction containing less than 4 ppb of perchlorate when the dry mass of the said perchlorate depleted retentate fraction is between about 16% and about 26% is produced from perchlorate containing whole milk or low-fat milk and/or whole milk or low-fat milk assumed to contain perchlorate containing 2 ppb or more than 2 ppb perchlorate when the dry mass is between about 8% and about 13%.
  • a content of less than 4 ppb of perchlorate when the dry mass of the produced retentate fraction is between about 10% and about 26% as defined elsewhere herein means in this respect that the content of perchlorate is preferably less than 4.0 ppb, more preferred less than 3.5 ppb, even more preferred less than 3.0 ppb, still more preferred less than 2.5 ppb, still more preferred less than 2.0 ppb, still more preferred less than 1.8 ppb, still more preferred less than 1.5 ppb, still more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 pp
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product comprises no detectable amount of perchlorate.
  • Said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is preferably characterized by a chlorate content of less than 4 ppb and/or a bromide content of less than 4 ppb when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%.
  • Less than 4 ppb means in this respect that the content of chlorate and/or bromide is preferably less than 4.0 ppb, more preferred less than 3.5 ppb, even more preferred less than 3.0 ppb, still more preferred less than 2.5 ppb, still more preferred less than 2.0 ppb, still more preferred less than 1.8 ppb, still more preferred less than 1.5 ppb, still more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9 ppb, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product as described elsewhere herein is characterized by a sodium content of 250 to 900 mg/kg and/or a potassium content of 900 to 3000 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%.
  • the sodium content of said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is between 250 and 900 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%. It is also preferred that the potassium content of said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is between 900 and 3000 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product as described elsewhere herein is characterized by a magnesium content of 50 to 400 mg/kg and/or a calcium content of 200 to 4000 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%.
  • the magnesium content of said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is between 80 and 400 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%. It is also preferred that the calcium content of said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is between 900 and 4000 mg/kg when the dry mass of the retentate fraction is between about 10% and about 26% as defined elsewhere herein, preferably about 12% or about 18%.
  • the calcium content of the perchlorate depleted retentate fraction is between 900 and 4000 mg/kg, preferably, between 1200 and 2800 mg/kg when the dry mass of the retentate fraction is between about 16% and about 20% as defined elsewhere herein, preferably about 18%.
  • the calcium content of the perchlorate depleted retentate fraction is between 200 and 1200 mg/kg, preferably, between 350 and 800 mg/kg when the dry mass of the retentate fraction is between about 10% and about 14%, preferably about 12%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk is produced from perchlorate containing whole milk or low-fat milk, it is particularly envisaged that the calcium content of the perchlorate depleted retentate fraction is between 900 and 4000 mg/kg, preferably, between 1200 and 2800 mg/kg when the dry mass of the retentate fraction is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product of the present invention is characterized by a perchlorate content of less than 4 ppb when the dry mass of the milk is between about 16% and about 20% as defined elsewhere herein, preferably about 18%.
  • said perchlorate depleted retentate fraction is characterized by a chlorate content of less than 4 ppb and/or a bromide content of less than 4 ppb when the dry mass of the milk is between about 16% and about 20% as defined elsewhere herein, preferably about 18%.
  • said perchlorate depleted retentate fraction is characterized by a sodium content of 300 to 800mg/kg, preferably of 400 to 500mg/kg and/or a potassium content of 1200 to 2800 mg/kg, preferably of 1600 to 2200 mg/kg when the dry mass of the retentate fraction is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • said perchlorate depleted retentate fraction is characterized by a magnesium content of 80 to 400 mg/kg, preferably of 100 to 250 mg/kg and/or a calcium content of 900 to 4000 mg/kg, preferably of 1200 to 2800 mg/kg when the dry mass of the retentate fraction is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk of the present invention is characterized by a perchlorate content of less than 4 ppb when the dry mass of the milk is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • said perchlorate depleted retentate fraction is characterized by a chlorate content of less than 4 ppb and/or a bromide content of less than 4 ppb when the dry mass of the milk is between about 16% and about 26%.
  • said perchlorate depleted retentate fraction is characterized by a sodium content of 300 to 800 mg/kg, preferably of 400 to 500 mg/kg and/or a potassium content of 1200 to 2800 mg/kg, preferably of 1600 to 2200 mg/kg when the dry mass of the retentate fraction is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • said perchlorate depleted retentate fraction is characterized by a magnesium content of 80 to 400 mg/kg, preferably of 100 to 250 mg/kg and/or a calcium content of 900 to 4000 mg/kg, preferably of 1200 to 2800 mg/kg when the dry mass of the retentate fraction is between about 16% and about 26% as defined elsewhere herein, preferably about 20%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk of the present invention is characterized by a perchlorate content of less than 4 ppb when the dry mass of the milk is between about 10% and about 14% as defined elsewhere herein, preferably about 12%.
  • said perchlorate depleted retentate fraction is characterized by a chlorate content of less than 4 ppb and/or a bromide content of less than 4 ppb when the dry mass of the milk is between about 10% and about 14% as defined elsewhere herein, preferably about 12%.
  • said perchlorate depleted retentate fraction is characterized by a chlorate content of less than 4 ppb and/or a bromide content of less than 4 ppb when the dry mass of the milk is between about 10% and about 14% as defined elsewhere herein, preferably about 12%. It is further envisaged that said perchlorate depleted retentate fraction is characterized by a sodium content of 250 to 900 mg/kg, preferably of 300 to 500 mg/kg and/or a potassium content of 900 to 3000 mg/kg, preferably of 1500 to 2300 mg/kg when the dry mass of the retentate fraction is between about 10% and about 14% as defined elsewhere herein, preferably about 12%.
  • said perchlorate depleted retentate fraction is characterized by a magnesium content of 50 to 300 mg/kg, preferably of 60 to 150 mg/kg and/or a calcium content of 200 to 1200 mg/kg, preferably of 350 to 800 mg/kg when the dry mass of the retentate fraction is between about 10% and about 14% as defined elsewhere herein, preferably about 12%.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product of the present invention is characterized by an at least 35%, preferably at least 39%, more preferred at least 45% reduced content of perchlorate compared to the content of perchlorate in the perchlorate containing milk product and/or milk product assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • “Recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate” means in this respect that the dry mass of the perchlorate depleted retentate fraction refers to the initial dry mass content of the perchlorate containing milk product and/or milk product assumed to contain perchlorate, i.e. they are considered to have the same dry mass.
  • the perchlorate depleted retentate fraction is characterized by a 50% reduced content of perchlorate when referring to the initial dry mass of in the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by no change in the content of lactose and protein compared to the content of lactose and protein in the perchlorate containing milk product and/or milk product assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by an at least 40%, preferably at least 46% reduced content of chlorate and/or an at least 30%, preferably at least 35% reduced content of bromide compared to the content of chlorate and bromide in the perchlorate containing milk product and/or milk product assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product is characterized by an at least 80%, preferably at least 92% maintained content of magnesium and/or an at least 80%, preferably at least 89% maintained content of calcium compared to the content of magnesium and calcium in the perchlorate containing milk product and/or milk product assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk is characterized by an up to 40%, preferably up to 50% or more reduced content of sodium and/or an up to 41% or more reduced content of potassium compared to the content of content of sodium and/or potassium in the perchlorate containing milk and/or milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk and/or milk assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk is characterized by an at least 40%, preferably at least 45%, more preferred at least 50%, even more preferred at least 52%, still more preferred at least 56%, still more preferred at least 63%, still more preferred at least 68% reduced content of chloride compared to the content of chloride in the perchlorate containing milk product and/or milk product assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing milk product and/or milk product assumed to contain perchlorate subjected to nanofiltration.
  • the perchlorate depleted retentate fraction is produced from milk such as skim milk
  • the perchlorate depleted retentate fraction is characterized by an at least 45% reduced content of perchlorate compared to the content of perchlorate in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from skim milk is characterized by no change in the content of lactose and protein compared to the content of lactose and protein in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from skim milk is characterized by an at least 40%, preferably at least 46%, more preferred at least 50% reduced content of chlorate and/or an at least 45%, preferably at least 53% reduced content of bromide compared to the content of chlorate and bromide in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • the perchlorate depleted retentate fraction produced from skim milk is characterized by an at least 80%, preferably at least 95% maintained content of magnesium and/or an at least 80%, preferably at least 89% maintained content of calcium compared to the content of magnesium and calcium in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • the perchlorate depleted retentate fraction produced from skim milk is characterized by an up to 41%, preferably up to 46% or more reduced content of sodium and/or an up to 41% or more reduced content of potassium compared to the content of content of sodium and/or potassium in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from skim milk is characterized by an at least 40%, preferably at least 45%, more preferred at least 50%, even more preferred at least 52%, still more preferred at least 56%, still more preferred at least 57% reduced content of chloride compared to the content of chloride in the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk and/or skim milk assumed to contain perchlorate subjected to nanofiltration.
  • the perchlorate depleted retentate fraction is produced from whey, it is particularly envisaged that the perchlorate depleted retentate fraction is characterized by an at least 35%, preferably at least 39%, more preferred at least 52%, even more preferred at least 59% reduced content of perchlorate compared to the content of perchlorate in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from whey is characterized by no change in the content of lactose and protein compared to the content of lactose and protein in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration. It is further envisaged that said perchlorate depleted retentate fraction produced from whey is characterized by a magnesium and calcium rejection of at least 80%, preferably at least 92%.
  • a rejection of at least 80% compared to the content of magnesium and calcium in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from whey is characterized by no change of magnesium and/or calcium compared to the content of magnesium and calcium in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from whey is characterized by an at least 40%, preferably at least 45%, more preferred at least 68%, even more preferred at least 71% reduced content of chlorate and/or an at least 30% preferably at least 35% reduced content of bromide compared to the content of chlorate and bromide in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration.
  • said perchlorate depleted retentate fraction produced from whey is characterized by an up to 25%, preferably up to 47%, more preferred up to 54% or more reduced content of sodium and/or an up to 25%, preferably up to 34%, more preferred up to 40% or more reduced content of potassium.
  • said perchlorate depleted retentate fraction produced from whey is characterized by an at least at least 50%, preferably at least 55%, more preferred at least 60%, even more preferred at least 63%, still more preferred at least 68% reduced content of chloride compared to the content of chloride in the perchlorate containing whey and/or whey assumed to contain perchlorate when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey and/or whey assumed to contain perchlorate subjected to nanofiltration.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product as defined herein is preferably produced from perchlorate containing milk, preferably skim milk or raw milk, or whey and/or milk or whey assumed to contain perchlorate.
  • the perchlorate depleted retentate fraction defined herein is produced from a perchlorate containing organic milk product and/or an organic milk product assumed to contain perchlorate.
  • the perchlorate depleted retentate fraction defined herein is produced from perchlorate containing organic milk and/or organic milk assumed to contain perchlorate, such as organic skim milk and/or organic skim milk assumed to contain perchlorate, or organic raw milk and/or organic raw milk assumed to contain perchlorate. It is further envisaged that the perchlorate depleted retentate fraction defined herein is produced from perchlorate containing organic whey and/or organic whey assumed to contain perchlorate.
  • organic when used in combination with milk has been defined elsewhere herein.
  • the perchlorate depleted retentate fraction produced by the processes or methods for the manufacture of a perchlorate depleted milk product preferably refers to an organic perchlorate depleted retentate fraction.
  • the perchlorate depleted retentate fraction as defined elsewhere herein is used for the manufacture of milk- based products.
  • milk-based product refers to food consisting between 1 and 100% of milk, milk components or milk single ingredients as defined or named elsewhere herein.
  • said milk-based products are yogurt, clabbered milk, curd and cheese, to name some, that can be produced from the perchlorate depleted retentate fraction of the present invention.
  • said milk products or milk-based products produced from the perchlorate depleted retentate fraction of the present invention are organic milk products or organic milk-based products.
  • the present invention also refers to the use of a ceramic nanofiltration membrane as defined elsewhere herein for the manufacture of a perchlorate depleted retentate fraction.
  • the present invention refers to the use of a ceramic nanofiltration membrane as defined elsewhere herein for the manufacture of a perchlorate depleted retentate fraction from a perchlorate containing milk product and/or milk product assumed to contain perchlorate as defined elsewhere herein.
  • a ceramic nanofiltration membrane as defined elsewhere herein for the manufacture of an infant formula base comprising a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13%.
  • said infant formula base comprises the perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk is between about 5% and about 13% as defined elsewhere herein.
  • a ceramic nanofiltration membrane as defined elsewhere herein for the manufacture of a milk-based infant formula comprising a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk product is between about 5% and about 13% as defined elsewhere herein.
  • said perchlorate depleted milk product comprised by said infant formula base or said milk-based infant formula contains less than 2 ppb chlorate and/or less than 2 ppb bromide when the dry mass of the milk product is between about 5% and about 13%.
  • the infant formula base comprises a perchlorate depleted retentate fraction comprising less than 4 ppb when the dry mass of the perchlorate depleted retentate fraction is between about 10% and about 26%.
  • infant formula base comprising the perchlorate depleted retentate fraction as defined elsewhere herein.
  • infant formula base in the context of the present invention refers to a product which is highly similar to human milk, and in which the concentration of different components can be easily adjusted as desired, and in which the concentration of the proteins a-lactalbumin and b-casein in particular can be optimized in an advantageous manner (see Figure 3).
  • an “infant formula base” of the present invention is preferably a milk-based infant formula base.
  • “Milk-base” means that the infant formula comprises between 15 and 40% of a milk product, preferably milk or whey, especially an organic milk product as defined elsewhere herein, wherein the organic milk product has undergone one of the processes for the manufacture of a perchlorate depleted milk product as described elsewhere herein.
  • the infant formula base of the present invention can undergo further manufacturing processes for the production of a milk-based infant formula described elsewhere herein.
  • the milk-based infant formula base may be supplemented by casein, by acid casein, caseinate, whey, whey protein fractions or fats.
  • minerals and oligoelements may be further added to the infant formula base obtained by the processes of the invention.
  • the infant formula base may be further supplemented.
  • Infant formulas may comprise partially and extensively hydrolyzed proteins in or only intact proteins.
  • any infant formula, including PHF should simulate human milk as closely as possible.
  • Whey protein typically composes about 60% of the protein in human milk, while casein typically composes about 40% (Lonnerdal et al. 1985, Am. J. Clin. Nutr.
  • the milk based infant formula obtained may be only whey protein.
  • the milk-based infant formula obtained may be casein based.
  • the infant formula base may be further supplemented with a suitable fat source and other necessary components, such as trace elements and vitamins.
  • the milk-based infant formula achieved is an infant formula which meets the requirements set by the EU food legislation.
  • the infant formula base may be dried to partial hydrolysates or into a powder by spray-drying. Suitable drying techniques applicable in this respect are described elsewhere herein.
  • spray-dried hydrolysate can be incorporated into an infant formula.
  • the retentate fraction obtained and processed according to the methods described herein can be used as it is and/or blended with other ingredients to make an infant formula base.
  • liquid partial hydrolysates can be concentrated by evaporation and then spray dried. Again, the spray-dried hydrolysate can be incorporated into an infant formula base.
  • the infant formula base having the described depleted perchlorate content can be further formulated to an infant formula using any of the methods of infant formulation known in the art.
  • the infant formula base according to the present invention is formulated to an infant formula having an energy content of about 60 to about 80 kcal/100 ml as consumed, preferably of about 62 to 75 kcal/100ml as consumed.
  • the infant formula base may be produced by the method as described in Example 2.
  • the present invention also relates to a process for the manufacture of a milk-based infant formula comprising a perchlorate depleted milk product manufactured according to the processes described herein, i.e. containing less than 2 ppb perchlorate when the dry mass of the perchlorate depleted milk product is between about 5% and about 13%.
  • said milk-based infant formula is manufactured from the perchlorate depleted milk product manufactured according to the processes described herein.
  • said process for the manufacture of a milk-based infant formula comprising a perchlorate depleted milk product manufactured according to the processes described herein, comprises a perchlorate depleted milk containing less than 2 ppb chlorate and/or less than 2 pbb bromide when the dry mass of the perchlorate depleted milk product is between about 5% and about 13% as defined elsewhere herein.
  • the manufactured milk-based infant formula can also be spray dried or processed to powder as described elsewhere herein.
  • the present invention also refers to the use of a perchlorate depleted retentate fraction produced according to the processes of the present invention for the manufacture of a milk-based infant formula.
  • Said perchlorate depleted milk product or retentate fraction can be obtained by any of the process for the manufacture of a perchlorate depleted milk product of the present invention described elsewhere herein.
  • a milk-based infant formula comprising the perchlorate depleted retentate fraction as defined elsewhere herein and/or the (milk-based) infant formula base defined elsewhere herein.
  • the milk based infant formula may be produced by the method as described in Example 3.
  • the infant formula is essentially milk-based, i.e. comprises the perchlorate depleted milk product as defined elsewhere herein after being subjected to the methods of the present invention used to deplete perchlorate.
  • the milk-based infant formula is obtained by a process comprising the step of subjecting a perchlorate containing milk product and/or milk product assumed to contain perchlorate to a nanofiltration step to obtain a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product.
  • said process comprises evaluating the perchlorate content in said retentate fraction and/or said permeate fraction.
  • the milk-based infant formula is produced by supplying a manufacturing process of a milk-based infant formula with said perchlorate depleted retentate fraction, i.e.
  • the milk-based infant formula is therefore manufactured using the perchlorate depleted retentate fraction defined elsewhere herein. “Supplying a manufacturing process” mean in this respect that any industrial process for the production of an infant formula known to those skilled in the art can be applied.
  • the present invention further refers to a milk-based infant formula whose milk-based ingredients consist of the perchlorate depleted retentate fraction as defined elsewhere herein and/or of the milk-based infant formula base as defined elsewhere herein.
  • milk- base ingredients refers to the total amount of milk components comprised by the perchlorate depleted retentate fraction.
  • said milk-based infant formula is spray dried or processed to powder as described elsewhere herein.
  • the process for the manufacture of a milk-based infant formula as defined herein may also comprise the step of spray drying said infant formula or processing said infant formula to powder.
  • the milk-based infant formula is liquid.
  • infant formula refers to any composition which can be fed to a newborn or a toddler.
  • infant preferably refers to any child in the age of up to 12 months which is in accordance with Commission Directive 2006/141 /EC.
  • Infant formulae means foodstuffs intended for particular nutritional use by infants during the first months of life and satisfying by themselves the nutritional requirements of such infants until the introduction of appropriate complementary feeding.
  • follow-on formulae means foodstuffs intended for particular nutritional use by infants when appropriate complementary feeding is introduced and constituting the principal liquid element in a progressively diversified diet of such infants.
  • milk-based refers to the fact that the infant formula comprises between 15 and 40% of a milk product, preferably milk or whey, especially an organic milk product defined elsewhere herein, wherein the organic milk product has undergone one of the processes for the manufacture of perchlorate depleted milk product as described elsewhere herein.
  • the milk-based infant or follow-on formulae is preferably designed for feeding infants under 12 months of age, i.e. is usually prepared for bottle-feeding or cup feeding from milk powder (mixed with water) or liquid (with or without additional water).
  • Said milk-based infant formula can exemplarily have a composition as shown in any of Tables 3A- E.
  • said infant formulae are preferably fed to infants under 12 months of age, said infant formula aims at simulating human milk, i.e. its suitability as a complete or partial substitute for human milk in cases where women are unable to feed their child with their own milk or cannot supply enough milk, or when breastfeeding is contraindicated.
  • the milk-based infant formula can be part of other foods suitable for consumption by infants, such as milk pudding, fruit puree and milk-cereal puree comprising said milk-based infant formula.
  • milk-based infant formula products are also included by the present invention.
  • the milk-based infant formula can be packed into portions.
  • said milk-based infant formula is packed in portions of 11 to 50 g. More preferred, said milk-based infant formula is packed in portions of 11-25 g, even more preferred in portion of 11 to 14 g or 18 to 25 g.
  • said milk-based infant formula is packed in portions of 300 to 800 g. More preferred, said milk-based infant formula is packed in portions of 500 to 800 g. It is particularly preferred that said infant formula is packed into portions of 500 g, 600 g or 800 g.
  • the process for the manufacture of a milk-based infant formula as defined herein may also comprise the step of packing said infant formula in portions of 11 to 25 g or 300 to 800g.
  • a liquid infant formula is packed in portions of 90 to 1000 ml, preferably of 90-450 ml. It is particularly preferred that said liquid infant formula is packed into portions of 90 ml, 200 ml, 450 ml or 1000 ml.
  • the process for the manufacture of a milk-based infant formula as defined herein may also comprise the step packing said infant formula in portions of 80 to 1000ml.
  • the present invention also refers to an assortment consisting of at least two infant formulas as defined elsewhere herein.
  • the term “assortment” as used herein refers to a shipping unit, i.e. the arrangement of said infant formulas to be transported and/or purchased.
  • said assortment consists of 2 to 200 infant formulas as defined elsewhere herein. More preferred, said assortment consists of 10 to 200 infant formulas as defined elsewhere herein. Equally preferred, said assortment consists of 4 to 48 infant formulas as defined elsewhere herein. More preferred, said assortment consists of 4 to 12 or 12 to 24, preferably 24 infant formulas as defined elsewhere herein. Still more preferred, said assortment consists of 2 to 8 infant formulas as defined elsewhere herein.
  • said assortment consists of 4 to 8 infant formulas as defined elsewhere herein. Most preferred, said assortment consists of 4 infant formulas as defined elsewhere herein. Equally preferred, said assortment consists of 6 infant formulas as defined elsewhere herein. Equally preferred, said assortment consists of 8 infant formulas as defined elsewhere herein. In this respect it is particular envisaged that an assortment consisting of formulas packed in portions of 500 g, 600g or 800g consists of 4 infant formulas. It is further particularly envisaged that an assortment consisting of formulas packed in portions of 11 to 50 g, such as 11-25 g, more preferred 11 to 14 g or 18 to 25 g, consists of 10 to 200 infant formulas.
  • an assortment consisting of formulas packed in portions of 200 ml or 100 ml consists of 6 infant formulas. It is further particularly envisaged that an assortment consisting of formulas packed in portions of 450 ml consists of 8 infant formulas. It is further particularly envisaged that an assortment consisting of formulas packed in portions of 90 ml consists of 24 infant formulas.
  • said assortment is placed on a tray. Said tray is preferably suitable for transporting or storing said assortment. Preferably, said tray is made out of cardboard or wood. It is also envisaged that said assortment placed on said tray is covered with foil, preferably a plastic foil.
  • the process for the manufacture of a milk-based infant formula as defined herein may also comprise the step of preparing an assortment as defined herein above.
  • infant formulae are usually based predominantly on an amino acid composition similar to that of human milk.
  • Infant formula bases are generally characterized in that a protein composition is prepared by subjecting milk that has not undergone heat treatment or milk that has undergone moderate heat treatment or pasteurization, or microfiltration and bactofugation, to membrane processing as described elsewhere herein, in order to obtain a perchlorate depleted retentate fraction, concentrating the retentate and optionally demineralizing the concentrated retentate for example by electrodialysis as described elsewhere herein.
  • the infant formula can be produced by mixing perchlorate depleted milk powder and dry ingredients together, or by dissolving perchlorate depleted milk powder and dry ingredients in water followed by a spray drying step.
  • said infant formula does not comprise yoghurt.
  • the process of the manufacture of the infant formula preferably comprises at least the step of formulating the perchlorate depleted milk product of the present invention into a milk-based infant formula.
  • “Formulating” means in this respect that all essential components needed to manufacture said milk-based infant formula are brought together under conditions known to those skilled in the art to result in an eatable formula.
  • Formulating said milk-based infant formula may also comprise diverse follow-up treatments such as diluting, drying and/or sterilizing said formula as described elsewhere herein.
  • said milk-based infant formula comprises a perchlorate depleted milk product containing less than 2 ppb perchlorate when the dry mass of the milk is between about 5% and about 13%, preferably about 6% or about 9%.
  • the milk-based infant formula comprises a perchlorate depleted milk product containing less than 1.8 ppb, more preferred less than 1.5 ppb, even more preferred less than 1.3 ppb, still more preferred less than 1.0 ppb, still more preferred less than 0.9, still more preferred less than 0.8 ppb, still more preferred less than 0.7 ppb, still more preferred less than 0.6 ppb, still more preferred less than 0.5 ppb, still more preferred less than 0.4 ppb, still more preferred less than 0.3 ppb, still more preferred less than 0.2 ppb, still more preferred less than 0.1 ppb, still more preferred less than 0.09 ppb, still more preferred less than 0.08 ppb, still more preferred less than 0.07 ppb, still more preferred less than 0.06 ppb, still more preferred less than 0.05 ppb, still more preferred less than 0.04 ppb, still more preferred less than 0.03 ppb, still more preferred less than 0.02 ppb, still more preferred less than 0.01 ppb,
  • the milk-based infant formula comprises a perchlorate depleted milk product containing no detectable amount of perchlorate, i.e. the content of perchlorate has been nearly completely removed.
  • said milk-based infant formula well complies with the perchlorate content as suggested by EFSA as TDI.
  • the processes of the present invention may further comprise partial reduction of monovalent salts from the perchlorate depleted retentate, and/or of water soluble contaminants, such as diethanolamine, triethanolamine, bromide and chlorate as described elsewhere herein.
  • water soluble contaminants such as diethanolamine, triethanolamine, bromide and chlorate as described elsewhere herein.
  • nanofiltration may be most efficient way to deplete milk products of water soluble contaminants.
  • Demineralization process is commonly used in the dairy and food industry, and it aims to maintain lactose and proteins of the milk while decreasing the mineral content (up to -90%).
  • Demineralized end product which can subsequently be crystallized and dried up, is largely used as base ingredient in nutrition for infancy, as a substitute for breast milk.
  • the term "demineralization” is used to mean, in relation to a purification process, the removal of ionized minerals and salts (both organic and inorganic) from the retentate fraction.
  • Demineralization of the retentate refers to removal of ions, e.g. calcium and other ions, from the retentate.
  • a further possible step for the manufacture processes of the present invention is de-ashing, separation of carbohydrates and proteins, or lactose demineralization.
  • de-ashing refers to a procedure in which interfering inorganic (i.e., ash-forming) components are removed from a sample.
  • ash forming compounds comprise minerals.
  • a combination of the above described processes is used to obtain end products with desired specifications and characteristics.
  • the present invention relates to a system for the manufacture of an infant formula base or a milk-based infant formula as defined herein.
  • Said system may contain a device which is able to regulate the perchlorate depletion.
  • said system may comprise a nanofiltration module that is suitable for subjecting a perchlorate containing milk product and/or milk product assumed to contain perchlorate to a nanofiltration step as defined elsewhere herein, thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product.
  • Said nanofiltration module comprises a ceramic nanofiltration membrane as defined elsewhere herein.
  • the present invention also refers to a system for the manufacture of an infant formula base or a milk-based infant formula comprising a nanofiltration module that is suitable for subjecting a perchlorate containing milk product and/or a milk product assumed to contain perchlorate to a nanofiltration step thereby obtaining a perchlorate depleted retentate fraction and a perchlorate containing permeate fraction of said milk product, wherein said nanofiltration step makes use of a ceramic nanofiltration membrane as defined elsewhere herein.
  • the obtained retentate fraction is characterized by a perchlorate content of less than 4 ppb when the dry mass of the retentate fraction is between about 10% and about 26%.
  • said system may comprise: (a) a milk source, (b) one or more filtration modules, for example, cross-flow filtration modules, which are communicatively connected to the milk source for generating one or more filtration fractions, thereby providing for a retentate fraction and a permeate fraction as defined elsewhere herein, and (c) one or more fluid delivery means connected to each of the cross-flow filtration modules, for creating a sufficient flow of milk through the filtration modules to effect separation of milk fractions and (d) one or more means downstream of each filtration modules for sequentially capturing one or more fractions generated by the filtration module.
  • the system can also comprise one or more dilution or drying modules for providing infant formulae with desired specifications and characteristics.
  • Example 1 Manufacture of a perchlorate depleted milk product
  • nanofiltration membranes from Inopor® For the manufacture of a perchlorate depleted milk product from dairy raw materials, ceramic nanofiltration membranes from Inopor® have been tested.
  • the nanofiltration membranes were used as single module with a molecular weight cut off of 450 Dalton and an average pore size of 0.9 nm, or a molecular weight cut off of 200 Dalton for the milk raw materials skim milk and whey. This resulted in a filtration area of 0.0264m 2 per test run.
  • the membranes were not conditioned but rinsed with reverse osmosis water before the trial.
  • the stainless steel nanofiltration unit When using the 450 Dalton membrane, the stainless steel nanofiltration unit was equipped with a single module membrane of type EKR made of titanium oxide with an outer module diameter of 10 millimeter and a module length of 1200 millimeter. When using the 200 Dalton membrane, the stainless steel nanofiltration unit was equipped with a single module membrane of type EKR made of titanium oxide with an outer module diameter of 10 millimeter and a module length of 1200 millimeter.
  • the perchlorate containing milk was pumped at a maximum pressure of 15 bar into the nanofiltration module to separate the perchlorate containing milk into perchlorate depleted retentate and a perchlorate containing permeate.
  • Raw milk having a dry matter of about 12% to about 14% was stored at 4°C. Afterwards, raw milk was preheated at 50 to 60°C and fat was separated at 50 to 60°C and 4000rpm to obtain perchlorate containing skim milk with a dry mass of about 8% to about 10% and a fat content of ⁇ 0.1%. Perchlorate content was measured in 5 kg of skimmed milk with a dry mass of 9%, and 25 ppb of perchlorate was detected. After perchlorate content evaluation, perchlorate containing skim milk was pasteurized at 72 to 75°C for 15 to 30 sec, then cooled down below 10°C and conducted to nanofiltration.
  • 1.5 kg of pretreated skim milk was fed on a dairy plant manufactured by the company PS Rothtechnik GmbH (Basel, Switzerland) with a nanofiltration membrane (Nanofiltration Inopor® Nano 450 Dalton cut-off and average pore size 0.9 nm, or Nanofiltration Inopor® Nano 200 Dalton cut-off with a filtration area of 0.0264 m 2 per module.
  • the nanofiltration unit was equipped with one of the two nanofiltration membranes as described herein above.
  • 1.5 kg skim milk were fed to the nanofiltration unit for maximum 5 hours at a maximum pressure of 15 bar and a temperature below 25°C, which led to the production of 0.5 kg skim milk concentrate with a dry mass of 18% and a perchlorate content of 27 ppb, respectively.
  • the amount of permeate was also about 0.5 kg, the rest of the material was lost in the system.
  • the content of perchlorate, chlorate and bromide was analysed using the QuPPe-AO-Method (Quick Polar Pesticides Method) that involves extraction with acidified methanol and LC-MS/MS measurement.
  • Other ions like magnesium, calcium, sodium, potassium and chloride were analyzed using ion chromatography. The respective results are summarized in Tables 1A-1D below. Perchlorate containing permeate was discarded.
  • the obtained perchlorate depleted retentate fraction (or skim milk concentrate) was stored at 4°C and subsequently dried via spray drying to provide skim milk powder depleted of perchlorate or further manufactured to obtain a perchlorate depleted infant formula base.
  • Tables 1A-1D when roughly doubling the dry mass of the perchlorate containing starting material the perchlorate content basically remained unchanged, i.e. was reduced by about 45%.
  • other ions like magnesium and calcium as well as proteins and lactose were largely retained by the nanofiltration membrane.
  • Tables 1A-1D show that compounds like chlorate and/or bromide are depleted by at least 46% and about 53%, respectively, from the perchlorate containing skim milk when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk. Further, a reduction of sodium by up to 45% and of potassium by up to 41%, as well as a depletion of chloride by at least 52% could been observed when the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing skim milk.
  • Perchlorate containing whey with a dry mass of about 6% and a fat content of ⁇ 0.1% was stored at 4°C. Perchlorate content was measured in each 5 kg of whey with a dry mass of 6%, and 32 ppb of perchlorate was detected. After perchlorate content evaluation, perchlorate containing whey was conducted to nanofiltration. 1.5kg of pretreated whey was fed on a dairy plant manufactured by the company PS mittechnik GmbH (Basel, Switzerland) with a nanofiltration membrane (Nanofiltration Inopor® Nano 450 Dalton cut-off and average pore size 0.9 nm, or Nanofiltration Inopor® Nano 200 Dalton cut-off with a filtration area of 0.0264 m 2 per module.
  • the nanofiltration unit was equipped with one of the two nanofiltration membrane as described herein above. 1.5 kg whey were fed to the nanofiltration unit for maximum 5 hours at a maximum pressure of 15 bar and a temperature below 25°C, which led to the production of 0.5 kg whey concentrate with a dry mass of 12% and a perchlorate content of 40 ppb, respectively. The amount of permeate was also about 0.5 kg, the rest of the material was lost in the system. The content of perchlorate, chlorate and bromide was analysed using the QuPPe-AO-Method (Quick Polar Pesticides Method) that involves extraction with acidified methanol and LC-MS/MS measurement. Other ions like magnesium, calcium, sodium or potassium were analyzed using ion chromatography.
  • Tables 1E to 1G show that compounds like chlorate and/or bromide are depleted by at least 46% and about 35%, respectively, from the perchlorate containing whey when the dry mass of the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey. Further, a reduction of sodium by up to 54% and of potassium by up to 40%, as well as a depletion of chloride by at least 63% could been observed when the perchlorate depleted retentate fraction is recalculated to the dry mass of the perchlorate containing whey.
  • Whey (W) and whey concentrate (WC) ceramic membrane 450 Da results
  • Example 2 Manufacture of the infant formula base
  • the infant formula base of the invention was manufactured from the perchlorate depleted retentate fraction (such as skim milk concentrate) obtained according to Example 1 and as depicted in Figures 1-3.
  • skim milk concentrate having a dry mass of about 16 to about 20% or skim milk having a dry mass of about 8 to about 10% was optionally further supplemented and spray dried to obtain an infant formula base useful to produce an infant formula (see Figure 3).
  • the infant formula base of the invention was manufactured from the perchlorate depleted whey concentrate obtained according to Example 1 as depicted in Figures 4 and 5.
  • whey concentrate having a dry mass of about 12% to about 27% or whey having a dry mass of about 5% to about 7% was optionally further supplemented and spray dried to obtain an infant formula base useful to produce an infant formula (see Figure 5).
  • Example 3 Manufacture of an infant formula from the infant formula base
  • an infant formula base obtained according to Example 2 was further admixed with the following ingredients: whey powder, lactose, mineral and trace elements, vitamins, fat mixtures, special protein compositions, fatty acids, starch and/or amino acids. After admixing, the mixture undergoes spray drying.
  • Exemplary infant formulae manufactured according to the present invention are depicted in Tables 3A-E below.

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Abstract

L'invention concerne un procédé de production d'un produit laitier appauvri en perchlorate sur la base d'une nanofiltration de matières premières laitières à l'aide d'une membrane de nanofiltration céramique. L'invention concerne en outre des procédés de préparation d'une base de préparation pour nourrissons et d'une préparation pour nourrissons à base de lait utilisant ledit produit laitier appauvri en perchlorate. L'invention concerne également une fraction de rétentat appauvrie en perchlorate utilisée pour produire un produit laitier appauvri en perchlorate, une base de préparation pour nourrissons ou une préparation pour nourrissons à base de lait, un assortiment comprenant ladite préparation et un système pour la production d'une préparation pour nourrissons à base de lait ou d'une base de préparation pour nourrissons. L'invention concerne également l'utilisation d'une membrane de nanofiltration céramique pour la production d'une fraction de rétentat appauvrie en perchlorate à partir d'un produit laitier contenant du perchlorate, une base de préparation pour nourrissons comprenant un produit laitier appauvri en perchlorate et une préparation pour nourrissons comprenant un produit laitier appauvri en perchlorate.
EP22716342.5A 2021-03-17 2022-03-17 Procédés de production de produits laitiers appauvris en perchlorate Pending EP4307909A1 (fr)

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ES2226466T3 (es) 1998-11-24 2005-03-16 Societe Des Produits Nestle S.A. Procedimiento de preparacion de una composicion proteinica y de una formula infantil que la contiene.
CN101589739B (zh) 2009-07-01 2011-05-04 济南大学 一种乳制品脱除三聚氰胺的综合处理方法
FI125332B (fi) 2011-11-11 2015-08-31 Valio Oy Menetelmä maitotuotteen valmistamiseksi
CN106324144B (zh) 2016-09-19 2018-06-26 山东省食品药品检验研究院 亲水作用色谱-串联质谱法检测乳粉及婴幼儿配方乳粉中氯酸盐、高氯酸盐和溴酸盐的方法

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