This application is claims priority to Application No. MX/a/2014/015894 filed in Mexico on Dec. 18, 2014 under 35 U.S.C. § 119. The entire contents of this application is hereby incorporated by reference.
The present invention relates to dairy and milk treatment industries for obtaining lactose-free milk and assessment of byproduct in particular, particularly to milk treatment industry through different separation means such as micro and nanofiltration equipment.
After some time, it has been observed men and women who have trouble digesting lactose, disaccharide consisting of glucose and galactose. This situation can cause mild digestive problems, but also stronger problems. It has been attempted to solve this problem in several ways.
Furthermore, it is a high percentage tendency of the population, as can be seen in soft drinks by reducing carbohydrate intake in general and sugars in particular.
An alternative is to provide the person who has lactose intolerance a non-bender lactose enzyme, externally and by oral ingestion prior to the consumption of any dairy product. This solution is cumbersome and requires some planning and discipline by consumer. These features are not in target audience of a product to be marketed massively.
Other option is to apply lactase enzyme into milk fluid as a process for obtaining a product for direct consumption or for preparation of various milk derivatives to ensure low-lactose content.
These processes using lactase into the product provides a sweetness increased by the amount of galactose obtained, resulting an undesirable product by consumer.
U.S. Pat. No. 5,334,399 refers a solution to solve the problem adding potassium chloride to the product where enzymatic hydrolysis was performed. It is a practical solution, but often not allowed for breach of official standards in some countries.
Moreover, said procedure does not allow the assessment of an unwanted component which remains in said product and a process to remove said component to contain more advantages.
Some of said processes use equipment with membranes (filters) of different size (pore size) for different filtration processes such as ultrafiltration. Depending on the pore size, filter becomes more selective as follows:
1. Microfiltration. Used to retain particles according to their size such as bacteria and spores. Let through proteins, fat, sugars, amino acids, minerals and water.
2. Ultrafiltration. Used to retain particles according to their size such as proteins and fat. Let through sugars, amino acids, minerals and water.
3. Nanofiltration. Used to retain particles according to their size such as sacarose or granulated sugar. Let through minerals and water.
4. Reverse osmosis. Let through water and simple minerals.
Thus, it is not possible to determine a milk treatment process for lactose-free milk with similar organoleptic properties such as ultrapasteurized milk without lactose-free process.
A process known currently comprising the steps of:
Equipment use membranes capable to perform microfiltration, ultrafiltration, nanofiltration and reverse osmosis processes to separate milk components.
The process for producing lactose-free or low-lactose milk is as follows:
UF and NF processes can perform a partial or even near elimination of lactose content where also part of minerals are lost. This mixture then is subjected to an enzymatic hydrolysis process using β-galactosidase enzyme to reduce lactose content generating glucose and galactose.
Also can perform reconstitution of milk using UF retentate adding water to protein desired level or including reverse osmosis process to concentrate minerals of NF permeate and used for milk reconstitution.
This process provides milk with strange organoleptic characteristics for a normal milk without considering this situation, besides de possibility of using operations which increase the production process.
Any invention that refers the necessary steps (micro, ultra or nano filtration and reverse osmosis) to achieve a lactose-free process for a delactosed or lactose-free milk with a sensory profile equivalent to a pasteurized milk (lactose milk), a partial removal of lactose by physical means and then removing the remaining lactose using lactase enzyme (β-galactosidase enzyme) and obtaining a fully lactose as byproduct, it contributes a non-existent technical knowledge to the state of the art for its protection by a patent.
Patent No. CA2701066, Vernazza, Francesco, refers to a method to obtain low-fat milk comprising at least two steps: first step milk is subjected to an ultrafiltration process to produce an ultrafiltration permeate and retentate after said process and; a second step wherein said ultrafiltration permeate is subjected to a nanofiltration process to produce a nanofiltration permeate and a nanofiltration concentrate after said process. Nanofiltration permeate is continuously recycled directly to the nanofiltration operation to dilute retentate from ultrafiltration and to obtain low-fat milk therefrom. This method does not consider physicochemical conditions to achieve milk with specific organoleptic characteristics.
Mexican patent No. PA/a/2004/011243, Janne Sahlstein, refers to a procedure for producing lactose-free milk products. Process of said invention is characterized by subjecting whole milk to ultrafiltration (UF), nanofiltration (NF) and reverse osmosis concentration, followed by the addition of salt to the UF retentate. Disadvantages of said method is the addition of salt to ultrafiltration retentate adding concentration by reverse osmosis becoming said method more expensive.
Mexican patent No. PA/a/2005/002049 refers to a method for separating milk components, comprising the steps of: passing milk in one-direction-flow through a filtration apparatus; a first step of milk filtration by ultrafiltration means for producing a first liquid filtered and a first concentrated, wherein lactose content of first filtered does not exceed 5.5% by weight; a second step of milk filtration by nanofiltration of first liquid filtered by nanofiltration means for producing a second liquid filtered and a second concentrated, wherein lactose content of second filtered does not exceed 0.15% by weight; a third step of milk filtration by reverse osmosis of second liquid filtered for producing a third liquid filtered and a third concentrated, wherein lactose content of third concentrated does not exceed 0.06% by weight; and wherein first filtered, second filtered and third filtered are removed from filtration apparatus through a first output, a second output and a third output respectively. Said patent contains reverse osmosis.
U.S. Pat. No. 8,445,052, Holst et. al., refers to a process for producing lactose-free or substantially lactose-free milk, preferably without adding water, and the resultant product. Said process comprising the steps of: a) ultrafiltration of original milk for obtaining a first permeate and a first retentate; b) nanofiltration of said first permeate for obtaining a second permeate and a second retentate; mixing first retentate with second permeate for obtaining a mixture; and d) hydrolyze remaining lactose in said mixture for obtaining a hydrolyzed milk. Process provides a lactose-free product with original milk flavor. Said process does not consider the composition of fats, proteins and carbohydrates of original milk.
Processes present in state of the art have the following disadvantages: only used UF retentate and mixing directly retentate with soft water to achieve desired fat and protein levels, making these levels higher to obtain products with good sensory profile.
Also is a complicated and higher cost of operation process due to the application of 3 filtration steps: UF, NF and reverse osmosis.
Also adding flavor to achieve a product that according to Mexican standards, said product not categorized as milk but as flavored milk.
Also incorporate the use of more proteins, up from 3.5% being unaffordable for Mexican market.
Also are methods or processes with lower yields due to the water removal in product and does not return said water in filtration process.
Also said methods or processes use external salts for recovering of lost minerals which increases cost of product.
Also not considered recovery of mineral salts and possible aromatic compound total or partially responsible of milk flavor.
One of the purposes of this invention is to provide a delactosed or lactose-free milk with sensory profile equivalent to a normal pasteurized milk.
Another purpose of this invention is to provide the above quality using essential separation steps to reduce product costs.
Another purpose of this invention is to determine the effect of milk natural components concentration on organoleptic properties to achieve the first purpose of this invention.
Another purpose is to determine percentage between retentate and permeate to get a sensory profile equivalent to a normal pasteurized milk.
Further purposes and qualities will be detailed through the present invention.
In other words, the process object of this invention begins with standardization of milk to be treated.
Raw milk is standardized to the required fat level, setting a value from 1.4 to 2.2%, preferably from 1.5 to 2.1, even more preferably from 1.6 to 2.0%, even more preferably from 1.7 to 1.9% of butterfat. Meanwhile, protein level after standardization is as follows: a value from 2.9 to 3.7%, preferably from 3.0 to 3.6%, even more preferably from 3.1 to 3.5%, even more preferably from 3.2 to 3.4%.
Later, milk is subjected to UF process wherein a “milk-concentrate” retentate is obtained (from 4.7 to 5.3%, preferably from 4.8 to 5.2%, even more preferably from 4.9 to 5.1%), said retentate subsequently will be mixed with the permeate resulting from NF process. This concentration must be reached in retentate in ultrafiltration step to obtain level of lactose in reconstituted milk.
In the process of this invention, proportions in UF step are: 55 to 63%, preferably from 56 to 62%, even more preferably from 57 to 61%, even more preferably from 58 to 60% of retentate and; from 37 to 45%, preferably from 38 to 44%, even more preferably from 39 to 43%, even more preferably from 40 to 42% of permeate.
Permeate obtained in UF is subjected to NF process to obtain a retentate (water, lactose and minerals) and a permeate (water and minerals).
For NF step, process of this invention stablishes the following proportions: from 30 to 38%, preferably from 31 to 37%, even more preferably from 32 to 36%, even more preferably from 33 to 35% of retentate and; from 62 to 70%, preferably from 63 to 69%, even more preferably from 64 to 68%, even more preferably from 65 to 67% of permeate.
Diafiltration process is used primarily to streamline the recovery of minerals salts and aromatic compounds that provide flavor, it begins when lactose level is critical (lactose crystallization in membranes) in NF retentate, keeping lactose levels closed to said level avoiding diluted over the retentate.
In diafiltration only enough water is used to restore water lost during the process, such that by mixing UF retentate and NF permeate is obtained the same milk volume which it started only by obtaining a lower yield for protein adjustment necessary to provide better sensory profile. Mixing obtained from UF retentate and NF reconstituted milk permeate is then subjected to UHT process and then adding thereto enzyme needed by container to hydrolyze remaining lactose.
The use of UF permeate of milk causes a limitation in NF retentate concentration (between lactose and calcium), due to risk of crystallization on membrane, therefore it is recommended maintain a retentate concentration between 9 and 10° Bx, preferably from 10 to 11° Bx, even more preferably from 11 to 12° Bx, even more preferably from 12 to 13° Bx while diafiltration process is performed.
To generate a similar sweetness such as pasteurized milk during enzymatic hydrolysis, such step also part of process of this invention, in UF and NF steps should be removed from 35 to 40%, preferably from 36 to 39%, even more preferably from 37 to 38%; reconstituted milk should be from 2.7 to 3.5%, preferably from 2.8 to 3.4%, even more preferably from 2.9 to 3.3% and even more preferably from 3.0 to 3.2% of lactose.
Another parameter defining process of this invention is the proportion obtained from retentate and permeate in UF and NF processes. Said process has the following proportions: proportions in UF process are: from 55 to 63%, preferably from 56 to 62%, even more preferably from 57 to 61%, even more preferably from 58 to 60% of retentate; from 37 to 45%, preferably from 38 to 44%, even more preferably from 39 to 43%, even more preferably from 40 to 42% of permeate. For NF process: from 32 to 36%, preferably from 33 to 35% of retentate; from 62 to 70%, preferably from 63 to 69%, even more preferably from 64 to 68%, even more preferably from 65 to 67% of permeate.
A detailed description of the invention is next, relying on examples for this purpose is carried out.
Line (3a) carries permeate of permeate tank to NF equipment (4). Line (3b) carries permeate with addition of water stored into retentate-diafiltration water mixture tank (7). Tank (9) contains water that is injected to NF retentate.
A portion of the non-recirculated retentate is carried to the tank (8) wherein concentrated solution is concentrated.
NF permeate is carried to mixing tank (5) wherein UF retentate is mixing with said NF permeate to get delactosed milk which is carried to tank (6), said delactosed milk receives enzymatic cleavage of lactose step.
The first step in the process of this invention is to standardization of milk to be treated. Said standardization is accomplished with two milk components, fat concentration and protein concentration.
Raw milk is standardized to required fat level, i.e., setting a value from 1.4 to 2.2%, preferably from 1.5 to 2.1, even more preferably from 1.6 to 2.0%, even more preferably from 1.7 to 1.9% of butterfat.
Protein level after standardization is as follows: a value from 2.9 to 3.7%, preferably from 3.0 to 3.6, even more preferably from 3.1 to 3.5%, even more preferably from 3.2 to 3.4%.
Next step is ultrafiltration to get a UF permeate and a UF retentate. Permeate is carried to nanofiltration (NF) step. UF retentate is mixing with NF permeate. UF permeate is subjected to NF process to get a retentate (water, lactose and minerals) and permeate (water and minerals).
Use of skim milk (2 g/L).
Total solids concentration (SC) up to 12.8% (8.26%
Reconstitution of milk using retentate and soft water
Heat treatment of milk-UHT Process-
Enzymatic hydrolysis (using β-galactosidase) of
Product obtained has a milky and sweet diluted profile
Raise the profile increasing fat level to 1.6%.
In this example, skim milk has a butterfat content of 2 g/L. No nanofiltration has used and enzymatic hydrolysis of lactose remaining was less than 1%.
The result was undesirable because the product was very sweet and diluted.
Use of skim milk (2 g/L).
Concentration (SC) up to 12.98% (8.14% protein)
Reconstitution of milk using retentate and soft water
Standardization up to 1.6% of butterfat (BF)
Heat treatment of milk-UHT Process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has a dairy profile, more tan P1
Explore the possibility of reducing the use of soft
In this example, skim milk had the same butterfat content on treated milk of 2 g/L. concentration through UF has noticeably same concentrations of milk compounds.
Product is less sweet than example 1, and has a dairy profile, however, has a thin consistency.
Use of skim milk (2 g/L).
Concentration (SC) up to 9.51% (4.2% protein) using
Using UF permeate for processing by NF.
Concentration of NF retentate up to 13.5° Bx max
It is feasible to perform NF process using UF permeate
To perform test using UF and NF processes.
In this example, butterfat content on treated milk is the same, but concentration on final solids and protein is lower such that is less water with ultrafiltration step, because a nanofiltration step is applied to permeate.
It is feasible performed NF process using UF permeate and using less soft water for reconstitution of milk.
Use of skim milk (2 g/L).
Concentration (SC) up to 14.32% (8.58% protein)
Using UF permeate for processing by NF.
Concentration of NF retentate up to 12% of lactose.
Reconstitution of milk using UF retentate, NF permeate
NO standardization is performed at a level of 1.6%
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained improves dairy profile using these
Establish minimum amount of remaining lactose in
To identify the feasibility of using skim milk of
To determine whether additional homogenization
The result is still not acceptable, the product is diluted and sweetness is poor.
Use of skim milk (16 g/L).
Pasteurization and homogenization of milk
Concentration up to 16.11% SC (8.7% protein) using
UF permeate processing through NF.
NF retentate concentration up to 9.18% of lactose.
Reconstitution of milk using UF retentate, NF permeate
PH adjustment using lactic acid, because acidity is
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has a better dairy profile, however
Pasteurization and homogenization process does
There are major benefits using skim milk but:
Develop a specific curve on Milkoscan to obtain reliable
Explore the possibility of incorporating diafiltration
Use of skim milk (2 g/L).
Concentration up to 10.54% SC (4.69% protein) using
Processing UF permeate through NF and diafiltration.
Concentration of NF retentate using diafiltration
Reconstitution of milk using UF retentate and NF
Standardization performed a level of 1.6% of butter-
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has a better dairy profile with a
Proper functioning of generated curve for this
Feasible and beneficial the use of diafiltration process
To perform the process using semiskim milk.
To use curve generated in Milkoscan for raw milk.
To use diafiltration process in NF step.
Product obtained has a better dairy profile, however, sweetness is lower than a pasteurized milk.
Use of skim milk (16 g/L).
Retentate concentration up to 14.96% SC (6.23%
UF permeate processing using NF and diafiltration.
Reconstitution of milk using UF retentate plus NF
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has better texture, dairy profile
To improve sweetness level through optimize lactose
To achieve lower ° Bx width variation during diafiltration
Following was obtained:
Product obtained has better texture, dairy profile and same sweetness as pasteurized milk versus P6, but still has opportunity to optimize texture and sweetness.
Use of semi skim milk (16 g/L).
Retentate concentration up to 13.05% SC (5.02%
UF permeate processing using NF and diafiltration.
Final concentration of NF retentate using diafiltration
Reconstitution of milk using UF retentate plus NF
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has better dairy profile and same
To achieve lower ° Bx width variation and close
To decrease ° Bx width variation during diafiltration
Explore a reconstitution of milk to higher protein
Results obtained as follows:
Product obtained has better dairy profile and same sweetness as pasteurized milk, optimizing texture but still has opportunity to optimize versus pasteurized milk.
To decrease ° Bx width variation during diafiltration process but still close said variation.
Use 1.4% of fat milk because fat is increased in
Retentate concentration up to 14.14% SC (5.81%
UF permeate processing using NF and diafiltration.
Final concentration of NF retentate using diafiltration
Two reconstitutions of at different levels of protein
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Products obtained have better dairy profile, better
It is a better control of ° Bx amplitude.
To perform reconstitutions of milk at different protein
Products obtained have better dairy profile, better than 3.5% of protein and slight lack of texture.
Use 1.4% of fat milk.
Retentate concentration up to 14.07% SC (5.63%
UF permeate processing using NF and diafiltration.
Final concentration of NF retentate using diafiltration
Three reconstitutions of at different levels of protein
Heat treatment of milk-UHT process-
Enzymatic hydrolysis of lactose remaining less than
Product obtained has better dairy profile due to the
Difference in protein is low between 3.2 and 3.5%
Best products are from 3.2 to 3.5% of protein with
Profiles of these products are similar sweetness
To perform product with 3.3% of protein and 1.8%
Protein difference is not as marked between 3.2 and 3.5% comparing fat between 1.6 and 1.8% found.
Use 1.4% of fat.
Retentate concentration up to 14.66% SC (5.7%
UF permeate processing using NF and diafiltration.
Final concentration of NF retentate using diafiltration
Two reconstitutions of at different levels of protein
Heat treatment of milk - UHT process-
Enzymatic hydrolysis of lactose remaining less than
Both products are similar sensory to a pasteurized
Best method known for applicant for carrying out the invention is that resulting from the present description.
This invention has been sufficiently described so that a person with ordinary skills in present state of the art can reproduce and obtain results mentioned in said invention. If any person may be able to make modifications not described in said invention, said modifications in a lactose-removing milk process for lactose-free milk production and byproduct use, said modifications must be within scope of invention.
Number | Date | Country | Kind |
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MX/a/2014/015894 | Dec 2014 | MX | national |
Number | Name | Date | Kind |
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20050196508 | Wang | Sep 2005 | A1 |
20050214409 | Tossavainen | Sep 2005 | A1 |
20070166447 | Ur-Rehman | Jul 2007 | A1 |
20100055286 | Tikanmaki | Mar 2010 | A1 |
20100055289 | Kallioinen | Mar 2010 | A1 |
20100215828 | Tossavainen | Aug 2010 | A1 |
20110059220 | Tossavainen | Mar 2011 | A1 |
20130230623 | Sibakov | Sep 2013 | A1 |
Entry |
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“How Do We Eliminate Lactose . . . ?” 2019. http://organicvalley.custhelp.com/app/answers/detail/a_id/201/kw/lactose%20free. |
Number | Date | Country | |
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20160174586 A1 | Jun 2016 | US |