CN117481198A - Membrane separation recombination method for core nutritional ingredients of infant milk product and application of membrane separation recombination method - Google Patents
Membrane separation recombination method for core nutritional ingredients of infant milk product and application of membrane separation recombination method Download PDFInfo
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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
- A23C9/15—Reconstituted or recombined milk products containing neither non-milk fat nor non-milk proteins
- A23C9/1512—Reconstituted or recombined milk products containing neither non-milk fat nor non-milk proteins containing isolated milk or whey proteins, caseinates or cheese; Enrichment of milk products with milk proteins in isolated or concentrated form, e.g. ultrafiltration retentate
-
- 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
- A23C9/15—Reconstituted or recombined milk products containing neither non-milk fat nor non-milk proteins
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Dairy Products (AREA)
Abstract
The invention relates to the technical field of food, and provides a membrane separation and recombination method for core nutritional ingredients of infant milk products and application thereof, wherein the method comprises the following steps: the core nutrition component is formed by taking more than one of dilute cream, casein trapped fluid, whey protein concentrated solution, desalted whey protein concentrated solution, lactose concentrated solution and desalted lactose concentrated solution as main raw materials; the preparation of the raw materials comprises the following steps: degreasing raw milk to obtain skimmed milk and cream; carrying out multistage microfiltration on the skim milk to obtain whey protein permeate and casein retentate; subjecting the whey protein permeate to multistage ultrafiltration to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid to obtain whey protein concentrate; and dehydrating and concentrating the lactose permeate to obtain lactose concentrated solution. The invention utilizes the separation components of raw milk, can realize that 100% of core nutrient is derived from raw milk, avoids adverse effects caused by adding powder ingredients, and simultaneously obviously reduces the contents of furoic acid and lactulose in the product.
Description
Technical Field
The invention relates to the technical field of foods, in particular to a membrane separation and recombination method for core nutritional ingredients of infant milk products and application thereof.
Background
The dairy products have better significance on human bodies, especially on infants and children lacking breast milk, but the existing infant dairy products have certain problems.
At present, the infant or children products mainly realize the adjustment of the component proportion by adding nutrition ingredients, for example, in order to make the infant formula milk powder more approximate to breast milk in the protein composition proportion, main substances such as whey protein powder, desalted whey powder, lactose powder and the like are added to the infant formula milk powder to realize the adjustment of the proportions of casein, whey protein agent and lactose. At present, whey proteins come from imported big powder bags, so that secondary processing of whey protein powder exists, the proteins are heated for many times, the denaturation degree is increased, and digestion and absorption are affected.
However, the fresh milk products for children are only distinguished from milk sources at present, and the processing technology is adjusted, so that the products are limited by raw material sources and are difficult to be adjusted proportionally according to the nutrition requirements of children. And the proportion of the core nutrition components is adjusted by adding whey protein powder and the like.
Disclosure of Invention
In order to overcome the problems of the prior infant products at the present stage, the invention provides a membrane separation recombination method for core nutritional components of infant milk products and application thereof, and the separation and on-demand recombination of milk components are realized by adopting a membrane separation combination technology, so that the thermal denaturation of the infant milk products is reduced, and the fresh activity and flexibility of the infant milk products are improved.
Specifically, the invention provides a membrane separation recombination method for core nutritional ingredients of infant milk products, which comprises the following steps: the core nutrition component is formed by taking more than one of dilute cream, casein trapped fluid, whey protein concentrated solution, desalted whey protein concentrated solution, lactose concentrated solution and desalted lactose concentrated solution as main raw materials;
the preparation method of the raw materials comprises the following steps:
degreasing raw milk to obtain skimmed milk and the cream;
filtering the skim milk by multi-stage microfiltration to obtain whey protein permeate and casein retentate; casein in the casein trapped liquid accounts for not less than 95% of total protein;
filtering the whey protein permeate through multistage ultrafiltration to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid to obtain whey protein concentrate;
and dehydrating and concentrating the lactose permeate to obtain the lactose concentrated solution.
The membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention comprises the following steps:
the fat content of the cream is more than or equal to 25%, the protein content is 2-3%, and the lactose content is 1-4%;
the protein content in the casein trapped fluid is more than or equal to 9.0%, and the lactose content is 1-4%;
the protein content in the whey protein concentrate is more than or equal to 10%, and the lactose content is 1-10%; the mass ratio of the whey protein in the whey protein concentrate to the total solid is more than 90%;
the lactose content in the lactose concentrated solution is more than or equal to 10%, preferably more than or equal to 15%.
The membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention comprises the following steps: the multi-stage microfiltration is a continuous microfiltration system; the continuous microfiltration system mainly comprises 3-5 stages of microfiltration membranes connected in series; the 1 st stage micro-filtration membrane is not washed and filtered, and the water adding amount of any stage micro-filtration membrane except the 1 st stage micro-filtration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
According to the membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention, the continuous microfiltration system mainly consists of 3-level ceramic membranes or organic roll-type membranes which are connected in series;
the membrane aperture of the microfiltration membrane is 0.1-0.2 mu m;
the water adding amount during the washing and filtering of the 2 nd-stage microfiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage microfiltration membrane; the water adding amount during washing and filtering of the 3 rd stage microfiltration membrane is 60-80% of the intercepting liquid flow and/or the penetrating liquid flow of the 3 rd stage microfiltration membrane.
The membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention comprises the following steps: the multistage ultrafiltration is a continuous ultrafiltration system; the continuous ultrafiltration system mainly comprises 3-5 stages of ultrafiltration membranes which are connected in series; the 1 st-stage ultrafiltration membrane is not washed and filtered, and the water consumption of any one of the ultrafiltration membranes except the 1 st-stage ultrafiltration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
According to the membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention, the membrane pore size of the ultrafiltration membrane is as follows: 1000D to 50000D, preferably 5000D to 20000D;
the water adding amount during washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd-stage ultrafiltration membrane is 60-80% of the trapped fluid flow and/or the permeate fluid flow of the 3 rd-stage ultrafiltration.
The membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention comprises the following steps: the fat content of the skim milk is less than or equal to 0.08%, preferably less than 0.06%;
the degreasing temperature during degreasing is 45-55 ℃, preferably 50-55 ℃.
The membrane separation and recombination method for the core nutritional ingredients of the infant milk product provided by the invention comprises the following steps: desalting the whey protein concentrate by an ion exchange or electrodialysis technology to prepare the desalted whey protein concentrate; judging the desalination end point according to the conductivity change of the whey protein concentrate;
and/or desalting the lactose concentrated solution by an ion exchange or electrodialysis technology to prepare the desalted lactose concentrated solution; determining a desalination endpoint from the conductivity change of the lactose concentrate;
preferably, the mass ratio of ash in the desalted whey protein concentrate to total solids is less than 0.1%; the mass ratio of ash in the desalted lactose concentrate to the total solid is less than 0.1%.
According to the membrane separation and recombination method for the core nutritional ingredients of the infant milk product, provided by the invention, the electrodialysis technology is used for desalting by adopting a Bipolar (BMED) homogeneous membrane with a membrane pore diameter of 1-10 nm;
the desalination endpoint is reached when the conductivity of the whey protein concentrate and/or the lactose concentrate is 10-15% of the conductivity of the feed solution.
The invention also provides a baby milk product, which comprises liquid milk of a baby formula, powder of a baby formula, fresh milk of a child formula or children protein pudding, wherein more than 95% of the core nutrition components of the baby milk product are from more than one of cream, casein trapped fluid, whey protein concentrated fluid and lactose concentrated fluid by mass percent; preferably, 100% of the core nutritional components are derived from more than one of cream, casein retentate, whey protein concentrate and lactose concentrate;
the cream, the casein retentate, the whey protein concentrate and the lactose concentrate are prepared by the methods described above.
The invention also provides an electronic device comprising a memory, a processor and a computer program stored on the memory and capable of running on the processor, wherein the processor realizes the membrane separation recombination method of the core nutrition components of the infant milk product when executing the program.
The invention provides a membrane separation recombination method of core nutrition components of infant milk products and application thereof, which comprises the steps of degreasing raw milk to obtain skimmed milk and cream, and separating casein and whey protein from the skimmed milk by a multi-stage continuous microfiltration membrane system to obtain high-purity casein concentrate and whey protein permeate; whey protein permeate can flexibly obtain whey protein concentrate and lactose permeate through multistage continuous ultrafiltration and washing filtration; concentrating lactose permeate through nanofiltration/reverse osmosis membrane to obtain lactose concentrate and sterile water; lactose concentrate or desalted lactose concentrate obtained by electrodialysis. Then, the dilute cream, the casein concentrate, the whey protein concentrate (or the desalted concentrated whey protein solution) and the lactose concentrate (or the desalted lactose concentrate) are taken as core raw materials, and the addition (or non-addition) of the separation substances is carried out according to the nutrition requirements of infants and the design scheme of the product so as to meet the flexible proportion of the content and the proportion of core nutrients, particularly, the casein in the casein trapped solution accounts for more than 95% of the total protein mass, the flexible adjustment of the casein/whey protein proportion of 4:6 or 5:5 in the recombinant infant product plays a key role, and in addition, the flexible adjustment of the lactose content and the milk fat content is combined; other nutrients are added or not added, so that the flexible design of infant products can be achieved; the product prepared by the method can realize that 100% of core nutrients are derived from raw cow milk, avoid adverse effects caused by secondary heating of additional powder ingredients, obviously reduce the content of furfuryl amino acid and lactulose in the product, and retain more active substances.
In addition, when the product obtained after the separation of raw milk is used for reconstructing the infant milk product, the method has high utilization rate of raw milk and low water consumption in the separation process. Particularly, the skim milk is filtered through multi-stage microfiltration and the whey protein permeate is filtered through multi-stage ultrafiltration, the first-stage multi-stage microfiltration realizes one-step separation of casein and has high separation degree, the casein in the casein trapped liquid has high purity, the subsequent whey protein concentrate has high yield, the second-stage multi-stage ultrafiltration realizes the high purity of the whey protein in the whey protein concentrate, and on the basis of realizing both the purity and the yield of the casein in the casein trapped liquid and the whey protein in the whey protein concentrate, the integral utilization rate of raw milk is promoted to be more than 67%, the residual fresh cream or micelle casein can be used for preparing cream products and high-protein products, and the water consumption is only 60% of the raw milk treatment capacity.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the following description will briefly explain the drawings used in the embodiments or the description of the prior art, and it is obvious that the drawings in the following description are some embodiments of the invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic flow chart of a membrane separation recombination method of core nutritional ingredients of infant milk products.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The membrane separation and recombination method of the core nutritional ingredients of the infant milk product and the application thereof are described below with reference to fig. 1.
In particular, in a first aspect, the invention provides a membrane separation and recombination method for core nutritional ingredients of infant milk products, comprising the following steps: the core nutrition component is formed by taking more than one of dilute cream, casein trapped fluid, whey protein concentrated solution, desalted whey protein concentrated solution, lactose concentrated solution and desalted lactose concentrated solution as main raw materials;
as shown in fig. 1, the preparation method of the raw materials comprises the following steps:
degreasing raw milk to obtain skimmed milk and the fresh cream;
filtering the skim milk by multi-stage microfiltration to obtain whey protein permeate and casein retentate; casein in the casein trapped liquid accounts for not less than 95% of total protein;
filtering the whey protein permeate through multistage ultrafiltration to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid to obtain whey protein concentrate;
and dehydrating and concentrating the lactose permeate to obtain the lactose concentrated solution.
Considering the requirements of infant milk products on the components of the infant milk products, and improving the proportion of core nutritional components of the cream, the casein trapped fluid, the whey protein concentrated fluid and the lactose concentrated fluid in the infant milk products, the addition of other exogenous nutritional components is reduced, the instability defect and impurities caused by the exogenous nutritional components are reduced, and the invention realizes that the proportion can be improved to more than 90 percent, even up to 100 percent by strictly controlling the following indexes.
In some embodiments of the invention, there is provided:
the fat content of the cream is more than or equal to 25%, the protein content is 2-3%, and the lactose content is 1-4%;
the protein content in the casein trapped fluid is more than or equal to 9.0%, and the lactose content is 1-4%;
the protein content in the whey protein concentrate is more than or equal to 10%, and the lactose content is 1-10%; the mass ratio of the whey protein in the whey protein concentrate to the total solid is more than 90%;
the lactose content in the lactose concentrated solution is more than or equal to 10%, preferably more than or equal to 15%.
Because the raw materials are all liquid, the index disclosed by the invention is very important to the subsequent formula design, for example, the formula design of the core nutritional ingredients of the infant milk product and the addition of the raw materials cannot be carried out when the standard cannot be reached.
In experiments, the raw milk is used as a raw material, and the technological parameter control of degreasing, multistage microfiltration, multistage ultrafiltration and dehydration concentration is particularly important for improving the proportion of the dilute cream, casein trapped liquid, whey protein concentrate and lactose concentrate in the core nutrition components in the membrane separation process of the core nutrition components of the infant milk product.
In some embodiments of the present invention, as shown in fig. 1, it includes: the multi-stage microfiltration is a continuous microfiltration system; the continuous microfiltration system mainly comprises 3-5 stages of microfiltration membranes connected in series; the 1 st stage micro-filtration membrane is not washed and filtered, and the water adding amount of any stage micro-filtration membrane except the 1 st stage micro-filtration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
The series connection of the microfiltration membranes in the invention means that: the trapped fluid of the previous stage of micro-filtration membrane enters the next stage of micro-filtration membrane, and the permeate fluid of each stage of micro-filtration membrane is combined and collected. After the multi-stage microfiltration is finished, the main components of the whey protein permeate are whey protein, lactose and ash, and the main components of the casein retentate are casein, trace lactose and trace ash.
The water can be added in the washing and filtering mode.
The skim milk realizes the efficient separation of casein-whey protein by one step through the continuous micro-filtration system.
In some embodiments of the invention, the continuous microfiltration system consists essentially of a 3-stage ceramic membrane or an organic roll membrane in series;
the membrane aperture of the microfiltration membrane is 0.1-0.2 mu m;
the water adding amount during the washing and filtering of the 2 nd-stage microfiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage microfiltration membrane; the water adding amount during washing and filtering of the 3 rd stage microfiltration membrane is 60-80% of the intercepting liquid flow and/or the penetrating liquid flow of the 3 rd stage microfiltration membrane.
The membrane separation parameters of the multistage microfiltration include:
the temperature is 4-55 ℃, preferably 55 ℃;
VCF (volume ratio of feed liquid to concentrate): 0 to 4, preferably 3.5;
the transmembrane pressure is 0.1-5; preferably 0.1 to 2.
In some embodiments of the present invention, as shown in fig. 1, it includes: the multistage ultrafiltration is a continuous ultrafiltration system; the continuous ultrafiltration system mainly comprises 3-5 stages of ultrafiltration membranes which are connected in series; the 1 st-stage ultrafiltration membrane is not washed and filtered, and the water consumption of any one of the ultrafiltration membranes except the 1 st-stage ultrafiltration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
The ultrafiltration membrane series connection in the invention means that: the trapped fluid of the previous stage ultrafiltration membrane enters the next stage ultrafiltration membrane, and the permeate fluid of each stage of ultrafiltration membrane is combined and collected. After the multi-stage ultrafiltration is finished, the lactose permeate mainly comprises lactose and mineral substances, and the whey protein concentrate mainly comprises whey protein, trace lactose and trace ash.
In some embodiments of the invention, the ultrafiltration membrane has a membrane pore size of: 1000D to 50000D, preferably 5000D to 20000D;
the water adding amount during washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd-stage ultrafiltration membrane is 60-80% of the trapped fluid flow and/or the permeate fluid flow of the 3 rd-stage ultrafiltration.
The membrane separation parameters of the multistage ultrafiltration include:
the temperature is 0-50 ℃, preferably 45-50 ℃;
VCF:0 to 5, preferably 3.5;
the feed pressure was 1-10bar.
In some embodiments of the invention, there is provided: the fat content of the skim milk is less than or equal to 0.08%, preferably less than 0.06%;
the degreasing temperature during degreasing is 45-55 ℃, preferably 50-55 ℃.
The degreasing is performed by a high-speed cream separator.
In some embodiments of the present invention, as shown in fig. 1, it includes: desalting the whey protein concentrate by an ion exchange or electrodialysis technology to prepare the desalted whey protein concentrate; judging the desalination end point according to the conductivity change of the whey protein concentrate;
and/or desalting the lactose concentrated solution by an ion exchange or electrodialysis technology to prepare the desalted lactose concentrated solution; determining a desalination endpoint from the conductivity change of the lactose concentrate;
preferably, the mass ratio of ash in the desalted whey protein concentrate to total solids is less than 0.1%; the mass ratio of ash in the desalted lactose concentrate to the total solid is less than 0.1%.
In some embodiments of the invention, the electrodialysis technique performs desalination using Bipolar (BMED) homogeneous membranes with a membrane pore size of 1-10 nm;
the desalination endpoint is reached when the conductivity of the whey protein concentrate and/or the lactose concentrate is 10-15% of the conductivity of the feed solution.
The conditions of the electrodialysis include:
the membrane pressure is 0.1-0.5 bar, preferably 0.1-0.2 bar;
the temperature is less than 15 ℃.
The dehydration concentration can be performed in a nanofiltration/reverse osmosis membrane concentration mode;
the membrane pore diameter of the reverse osmosis membrane is as follows: 0.1 to 0.7nm, preferably 0.2nm.
The parameters during the reverse osmosis membrane treatment comprise: the pressure is 0 to 20bar, preferably 5 to 10bar.
The lactose permeate is dehydrated by nanofiltration/reverse osmosis membrane, and sterile water can be obtained; the total colony count of the sterile water is less than 10cfu/ml.
In a second aspect, the invention also provides a baby milk product, which comprises liquid milk of a baby formula, powder of a baby formula, fresh milk of a baby formula or children protein pudding, wherein more than 95% of the core nutrition components of the baby milk product are from more than one of cream, casein trapped liquid, whey protein concentrated liquid and lactose concentrated liquid in percentage by mass;
the cream, the casein retentate, the whey protein concentrate and the lactose concentrate are prepared by the methods described above.
Nutrient substances in cow milk can be divided into 3 major categories: milk fat, protein and lactose, which can be effectively separated through the separation process; in the actual formulation process, the milk isolates are not necessarily all used in the selection of the milk isolates, as the nutrients required for the different product formulations are different. The invention can only reach the core nutrition components needed by the infant milk product through the milk isolate, and only a small amount of other nutrients are needed to be added according to different formulas. And the surplus nutrient can be used for producing other products.
The on-line separation and combination of the core nutrients can be realized according to the requirements of the actual product formula to obtain mixed feed liquid; homogenizing, spray drying or pasteurizing or ultra-high temperature sterilizing, cooling, and packaging to obtain the final product.
In a third aspect, the invention also provides an electronic device comprising a memory, a processor and a computer program stored on the memory and executable on the processor, the processor implementing a method for membrane separation and reconstitution of core nutritional ingredients of infant milk products as described above when executing the program.
The specific techniques or conditions are not identified in the examples and are described in the literature in this field or are carried out in accordance with the product specifications. The reagents or equipment used were conventional products available for purchase by regular vendors without the manufacturer's attention.
The membrane separation and recombination method of the core nutritional ingredients of the infant milk product and the application of the membrane separation and recombination method in the infant milk product are described in specific cases below.
Example 1 infant formula liquid milk
A preparation method of infant formula liquid milk comprises the following steps:
(1) Degreasing raw milk by adopting a cream separator to obtain skimmed milk and fresh cream; wherein, the protein in raw milk is 3.0%, the fat is 3.6%, and the lactose is 5.0%; the degreasing temperature was 50 ℃ and the fat content of the skim milk was 0.06%.
The obtained fresh cream has fat content of 30%, protein content of 2.4%, and lactose content of 2.5%.
(2) Separating the skim milk obtained in the step (1) through a ceramic microfiltration membrane connected in series at 3 levels to obtain microfiltration permeate and casein trapped fluid; wherein, the pore diameter of the membrane is 0.1 μm, and the membrane separation parameters are as follows: separation temperature 55 ℃, VCF:3.5, the transmembrane pressure is 1bar, and the water adding amount during the washing and filtering of the 2 nd stage microfiltration membrane is 70% of the intercepting liquid flow of the 2 nd stage microfiltration membrane; the water adding amount during washing and filtering of the 3 rd stage microfiltration membrane is 80% of the intercepting liquid flow rate of the 3 rd stage microfiltration membrane.
The protein content in the obtained casein trapped fluid is 9.0%, the fat content is 0.3%, the lactose content is 1.5%, and the casein accounts for 95% of the total protein.
(3) Concentrating the microfiltration permeate obtained in the step (2) through three-stage series ultrafiltration membranes to obtain lactose permeate and whey protein trapped fluid, and performing reverse osmosis concentration on the whey protein trapped fluid to obtain whey protein concentrate with the protein content of 10%, wherein the fat content of the whey protein concentrate is 0.2%, and the lactose content of the whey protein concentrate is 1.0%.
Wherein, the membrane aperture is: 5000D, separation temperature 50 ℃, VCF:3.5, the water adding amount during the washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60% of the intercepting liquid flow rate of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd level ultrafiltration membrane is 60% of the trapped fluid flow of the 3 rd level ultrafiltration.
(4) And (3) performing reverse osmosis membrane concentration on the lactose permeate liquid obtained in the step (3) to obtain lactose concentrated liquid with lactose content of 10% and sterile water with total colony count of less than 10cfu/ml.
Wherein, the membrane pore diameter of the reverse osmosis membrane is: 0.2nm; the reverse osmosis concentration conditions are as follows: the pressure was 5bar.
(5) And (3) carrying out electrodialysis desalination on the whey protein concentrate obtained in the step (3) and the lactose concentrate obtained in the step (4) by adopting a Bipolar (BMED) homogeneous membrane with a membrane aperture of 1nm until the conductivity of the whey protein concentrate and the lactose concentrate is 10% of the conductivity of the feed liquid, and stopping desalination to obtain desalted whey protein concentrate with ash content less than 0.1% of the total solid mass ratio and desalted lactose concentrate with ash content less than 0.1% of the total solid mass ratio. Wherein, the conditions of electrodialysis desalination are: the membrane pressure was 0.1bar and the temperature 15 ℃.
The amounts of raw milk and water used under the above process, and the yields of the respective components were counted as follows:
(6) Preparation of infant formula liquid milk:
taking 1-stage infant formula liquid milk as an example according to the design requirement of infant formula milk products, preparing 1L infant formula liquid milk, wherein the content of the milk component separated matters is as follows: 60ml of fresh cream, 60ml of casein trapped fluid, 81ml of desalted whey protein concentrate, 700ml of desalted lactose concentrate, 18ml of compound vegetable oil, 100mg of compound mineral substance, 150mg of vitamin, 6mg of taurine and 0.4g of dietary fiber, and finally, preparing the mixture by using milk separation sterile water. In the formula design, 97% of the three main core nutrients are all from the milk separation components, and only a small amount of compound vegetable oil, compound mineral substances, vitamins and other trace nutrients are needed to be added in the formula design process.
(7) After the feed liquid is prepared, the infant formula liquid milk product can be prepared after homogenizing, sterilizing and filling.
The resulting liquid infant formula 1 was compared to a commercially available formula 1, as shown in the following table:
example 2 infant formula powder
A preparation method of infant formula milk powder comprises the following steps:
(1) Degreasing raw milk by adopting a cream separator to obtain skimmed milk and fresh cream; wherein, the protein content in raw milk is 3.0%, the fat content is 3.6%, and the lactose content is 5.0%; the degreasing temperature was 55 ℃ and the fat content of the skim milk was 0.08%.
The obtained fresh cream has fat content of 40%, protein content of 2.4%, and lactose content of 2.5%.
(2) Separating the skim milk obtained in the step (1) through a 3-grade ceramic microfiltration membrane system to obtain microfiltration permeate and casein retentate; wherein, the pore diameter of the membrane is 0.2 mu m, and the membrane separation parameters are as follows: separation temperature 55 ℃, VCF:3.0, transmembrane pressure 1bar; the water adding amount during the washing and filtering of the 2 nd stage microfiltration membrane is 60% of the trapped fluid flow of the 2 nd stage microfiltration membrane; the water adding amount during the washing and filtering of the 3 rd stage microfiltration membrane is 70% of the intercepting liquid flow rate of the 3 rd stage microfiltration membrane.
The protein content in the obtained casein trapped fluid is 12.0%, the fat content is 0.3%, the lactose content is 1.5%, and the casein accounts for 96% of total protein.
(3) Concentrating the microfiltration permeate obtained in the step (2) through three-stage series ultrafiltration membranes to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid through reverse osmosis to obtain whey protein concentrate with the protein content of 15%, wherein the fat content of the whey protein concentrate is 0.2%, and the lactose content of the whey protein concentrate is 1.0%.
Wherein, the membrane aperture is: 5000D, separation temperature 50 ℃, VCF:3.5, the water adding amount during the washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60% of the intercepting liquid flow rate of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd level ultrafiltration membrane is 60% of the trapped fluid flow of the 3 rd level ultrafiltration.
(4) And (3) performing reverse osmosis membrane concentration on the lactose permeate liquid obtained in the step (3) to obtain lactose concentrated liquid with lactose content of 15% and sterile water with total colony count of less than 10cfu/ml.
Wherein, the membrane pore diameter of the reverse osmosis membrane is: 0.2nm; the reverse osmosis concentration conditions are as follows: the pressure was 5bar.
(5) And (3) carrying out electrodialysis desalination on the whey protein concentrate obtained in the step (3) and the lactose concentrate obtained in the step (4) by adopting a Bipolar (BMED) homogeneous membrane with a membrane aperture of 1nm until the conductivity of the whey protein concentrate and the lactose concentrate is 10% of the conductivity of the feed liquid, and stopping desalination to obtain desalted whey protein concentrate with ash content less than 0.1% of the total solid mass ratio and desalted lactose concentrate with ash content less than 0.1% of the total solid mass ratio. Wherein, the conditions of electrodialysis desalination are: the membrane pressure was 0.1bar and the temperature 15 ℃.
The amounts of raw milk and water used under the above process, and the yields of the respective components were counted as follows:
(6) Preparation of infant formula milk powder:
taking 2 segments of infant formula as an example, 1kg of infant formula is prepared according to the design requirement of infant formula, and the content of the milk component separated matters is as follows: 286ml of cream, 398ml of casein trapped fluid, 480ml of desalted whey protein concentrate, 3810ml of desalted lactose concentrate, 114ml of compound vegetable oil, 500mg of compound mineral substance, 800mg of vitamin, 48mg of taurine and 3.0g of dietary fiber, wherein 97% of three main core nutrients in the formula design are all from milk separation components, and only a small amount of compound vegetable oil, compound mineral substance, vitamin and other trace nutrients need to be added in the formula design process.
(7) After the feed liquid is prepared, the infant formula milk powder can be prepared by homogenizing, sterilizing, concentrating, spraying powder, dry-mixing, adding a certain amount of 2mg lactoferrin and 3 hundred million active probiotics.
The obtained 2-stage infant formula was compared with the 2-stage formula on the market, as shown in the following table:
example 3 nutritional formula fresh milk for children
A preparation method of children nutrition-mixed fresh milk comprises the following steps:
(1) Degreasing raw milk by adopting a cream separator to obtain skimmed milk and fresh cream; wherein, the protein content in raw milk is 3.0%, the fat content is 3.6%, and the lactose content is 5.0%; the degreasing temperature was 55 ℃ and the fat content of the skim milk was 0.08%.
The obtained fresh cream has fat content of 30%, protein content of 2.4%, and lactose content of 2.5%.
(2) Separating the skim milk obtained in the step (1) through a 3-grade ceramic microfiltration membrane system to obtain microfiltration permeate and casein retentate; wherein, the membrane aperture is 0.14 μm, the membrane separation parameter is the separation temperature of 50 ℃, VCF:3.0, transmembrane pressure 1bar; the water adding amount during the washing and filtering of the 2 nd stage microfiltration membrane is 70% of the intercepting liquid flow of the 2 nd stage microfiltration; the water adding amount during washing and filtering of the 3 rd stage microfiltration membrane is 80% of the intercepting liquid flow rate of the 3 rd stage microfiltration membrane.
The protein content in the obtained casein trapped fluid is 9.0%, the fat content is 0.3%, the lactose content is 1.5%, and the casein accounts for 95% of the total protein.
(3) Concentrating the microfiltration permeate obtained in the step (2) through three-stage series ultrafiltration membranes to obtain lactose permeate and whey protein trapped fluid, and performing reverse osmosis concentration on the whey protein trapped fluid to obtain whey protein concentrate with the protein content of 10%, wherein the fat content of the whey protein concentrate is 0.2%, and the lactose content of the whey protein concentrate is 1.0%.
Wherein, the membrane aperture is: 10000D, separation temperature 50 ℃, VCF:3.5, the water adding amount during the washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60% of the intercepting liquid flow rate of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd level ultrafiltration membrane is 60% of the trapped fluid flow of the 3 rd level ultrafiltration.
(4) And (3) performing reverse osmosis membrane concentration on the lactose permeate liquid obtained in the step (3) to obtain lactose concentrated liquid with lactose content of 15% and sterile water with total colony count of less than 10cfu/ml.
Wherein, the membrane pore diameter of the reverse osmosis membrane is: 0.2nm; the reverse osmosis concentration conditions are as follows: the pressure was 5bar.
The amounts of raw milk and water used under the above process, and the yields of the respective components were counted as follows:
(5) Preparation of children nutritional formula fresh milk product:
according to the design requirement of the children's prepared fresh milk product, the milk component isolate, the cream, the casein trapped fluid, the whey protein concentrate and the lactose concentrate are added for batching, so that casein in milk can be realized: whey protein ratio is 4:6-2:8, and digestion and absorption of children are facilitated.
Such as 1L low fat, whey protein: the children nutrition prepared fresh milk with the casein ratio of 5:5 is added with the milk component isolates with the contents of respectively: 50ml of cream, 180ml of whey protein concentrate, 200ml of casein retentate, 500ml of lactose concentrate and 70ml of sterile water. In this formulation, 100% of all nutrients are from milk fractions. Realizes the thorough separation and flexible proportioning combination of milk components.
(6) After the feed liquid is prepared, the children nutrition-mixed fresh milk product can be prepared after homogenizing, low-temperature pasteurizing (72 ℃ for 15 s) and filling.
Example 4 children nutritional protein pudding
A preparation method of children nutrition protein pudding comprises the following steps:
(1) Degreasing raw milk by adopting a cream separator to obtain skimmed milk and fresh cream; wherein, the protein content in raw milk is 3.0%, the fat content is 3.6%, and the lactose content is 5.0%; the degreasing temperature was 55 ℃ and the fat content of the skim milk was 0.08%.
The obtained fresh cream has fat content of 30%, protein content of 2.4%, and lactose content of 2.5%.
(2) Separating the skim milk obtained in the step (1) through a ceramic microfiltration membrane connected in series at 3 levels to obtain microfiltration permeate and casein trapped fluid; wherein, the membrane aperture is 0.14 μm, the membrane separation parameter is the separation temperature of 50 ℃, VCF:3.0, transmembrane pressure 1bar; the water adding amount during the washing and filtering of the 2 nd stage microfiltration membrane is 80% of the trapped fluid flow of the 2 nd stage microfiltration membrane; the water adding amount during the washing and filtering of the 3 rd stage microfiltration membrane is 90% of the intercepting liquid flow rate of the 3 rd stage microfiltration membrane.
The protein content in the obtained casein retentate was 9.0%, and casein accounted for 95% of the total protein.
(3) Concentrating the microfiltration permeate obtained in the step (2) through three-stage series ultrafiltration membranes to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid through reverse osmosis to obtain whey protein concentrate with the protein content of 15%, wherein the fat content of the whey protein concentrate is 0.2%, and the lactose content of the whey protein concentrate is 1.0%.
Wherein, the membrane aperture is: 10000D, separation temperature 50 ℃, VCF:3.5, the water adding amount during the washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60% of the intercepting liquid flow rate of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd level ultrafiltration membrane is 60% of the trapped fluid flow of the 3 rd level ultrafiltration.
(4) And (3) performing reverse osmosis membrane concentration on the lactose permeate liquid obtained in the step (3) to obtain lactose concentrated liquid with lactose content of 15% and sterile water with total colony count of less than 10cfu/ml.
Wherein, the membrane pore diameter of the reverse osmosis membrane is: 0.2nm; the reverse osmosis concentration conditions are as follows: the pressure was 5bar.
The amounts of raw milk and water used under the above process, and the yields of the respective components were counted as follows:
(5) Preparation of children nutrition protein pudding:
according to the design requirement of pudding products, the cream, the whey protein concentrate and the lactose concentrate are added for proportioning, and the whey protein content in the final feed liquid is 8%, the lactose content is 3% and the fat content is 3.5%. The content of the milk component separated matters to be added is calculated by 1L of feed liquid: cream 117ml, whey protein concentrate 533ml, lactose concentrate 200ml.
(6) After the feed liquid is prepared, homogenizing, pasteurizing at low temperature (72 ℃ for 15 seconds), hot filling into a hard plastic packaging material, sterilizing for 5 minutes in a water area at 95 ℃, and rapidly cooling to 4 ℃ to prepare the children nutrition protein pudding.
According to the embodiment, the invention can be used for preparing and obtaining each separated product respectively, and can also be used for realizing on-line control according to the formula design and the productivity design, and realizing continuous separation, recombination and product preparation. The invention can obviously reduce adverse effects caused by repeated heating of milk components in the obtained infant milk product, such as increase of lactulose and furoic acid, decrease of active whey protein denaturation and increase of shelf life stability of the infant milk product by carrying out a series of treatments on raw milk and utilizing products under specific processes and flows.
Comparative example 1
The raw milk of example 1 of the present invention was separated, filtered and concentrated by the method of example 1 of patent CN116406702B, wherein the raw milk had a protein content of 3.0%, a fat content of 3.6%, a lactose content of 5.0% and an ash content of 0.6%, and the nutritional ingredients of the components obtained by the method were as shown in the following table:
the amounts of raw milk and water used under the above process, and the yields of the respective components were counted as follows:
(6) Preparation of infant formula liquid milk:
when the cream, the concentrated casein, the concentrated whey protein and the lactose solution obtained in the step (5) are adopted as raw materials and added according to the design requirement of the infant formula to prepare the 1-stage infant formula liquid milk, the fact that a part of desalted whey powder is required to be added to realize whey protein is found that the protein content in the concentrated whey protein solution is relatively low: casein was specified as 6:4. Therefore, the index of the furfuryl amino acid and lactulose in the product is slightly improved.
The liquid infant formula 1 described above was compared to the formula 1 of example 1, market 1, as shown in the following table:
it can be seen that: the core difference between the present patent and example 1 of CN116406702B is that:
according to the invention, the extremely separation of casein-whey protein is realized through a multistage continuous microfiltration system, the proportion of casein in the total protein can reach more than 95%, the casein trapped fluid with higher concentration is obtained, and more importantly, the core nutrients of infant products can be accurately configured in the subsequent recombination, so that the proportion of milk separation components in the core nutrients is improved. The multi-stage continuous ultrafiltration system and the reverse osmosis system are further adopted to realize whey protein concentration, and simultaneously remove a large amount of lactose to obtain high-purity whey protein concentrate, and the whey protein concentrate and the lactose concentrate are desalted to remove ash in the 2 isolates, so that the method is used for preparing infant formulas. The membrane separation process of the invention is mutually matched with each link, thus greatly reducing the water consumption and improving the efficiency of the membrane separation system.
The microfiltration separation adopted in the patent CN116406702B is for separating casein-whey protein, but the separation rate of the whey protein of the present invention cannot be achieved, i.e. the casein content in the trapped fluid cannot reach 95%, in addition, the whey protein concentrate obtained after ultrafiltration of the microfiltration permeate and the skim milk are treated by a cation exchange membrane, the main purpose of the microfiltration separation is to extract lactoferrin in the skim milk, and the method is used for subsequent low-temperature or aseptic treatment, and then recombination is carried out, so as to achieve the purpose of retaining the activities of alpha-lactalbumin, beta-lactoglobulin, immunoglobulin and lactoferrin in the whey; the main purpose of the invention in the formula design process is to prepare infant products, and the total protein proportion and the casein-whey protein proportion are concerned.
From the above description of the embodiments, it will be apparent to those skilled in the art that the embodiments may be implemented by means of software plus necessary general hardware platforms, or of course may be implemented by means of hardware. Based on this understanding, the foregoing technical solution may be embodied essentially or in a part contributing to the prior art in the form of a software product, which may be stored in a computer readable storage medium, such as ROM/RAM, a magnetic disk, an optical disk, etc., including several instructions for causing a computer device (which may be a personal computer, a server, or a network device, etc.) to execute the method described in the respective embodiments or some parts of the embodiments.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A membrane separation and recombination method for core nutritional ingredients of infant milk products, which is characterized by comprising the following steps: the core nutrition component is formed by taking more than one of dilute cream, casein trapped fluid, whey protein concentrated solution, desalted whey protein concentrated solution, lactose concentrated solution and desalted lactose concentrated solution as main raw materials;
the preparation method of the raw materials comprises the following steps:
degreasing raw milk to obtain skimmed milk and the cream;
filtering the skim milk by multi-stage microfiltration to obtain whey protein permeate and casein retentate; casein in the casein trapped liquid accounts for not less than 95% of total protein;
filtering the whey protein permeate through multistage ultrafiltration to obtain lactose permeate and whey protein trapped fluid, and concentrating the whey protein trapped fluid to obtain whey protein concentrate;
and dehydrating and concentrating the lactose permeate to obtain the lactose concentrated solution.
2. The method for membrane separation and recombination of core nutritional components of infant milk products according to claim 1, comprising:
the fat content of the cream is more than or equal to 25%, the protein content is 2-3%, and the lactose content is 1-4%;
the protein content in the casein trapped fluid is more than or equal to 9.0%, and the lactose content is 1-4%;
the protein content in the whey protein concentrate is more than or equal to 10%, and the lactose content is 1-10%; the mass ratio of the whey protein in the whey protein concentrate to the total solid is more than 90%;
the lactose content in the lactose concentrated solution is more than or equal to 10%.
3. Membrane separation and recombination method of core nutritional components of infant milk products according to claim 1 or 2, characterized by comprising: the multi-stage microfiltration is a continuous microfiltration system; the continuous microfiltration system mainly comprises 3-5 stages of microfiltration membranes connected in series; the 1 st stage micro-filtration membrane is not washed and filtered, and the water adding amount of any stage micro-filtration membrane except the 1 st stage micro-filtration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
4. The membrane separation and recombination method for core nutritional ingredients of infant milk products according to claim 3, wherein the continuous microfiltration system mainly consists of 3-grade ceramic membranes or organic roll-type membranes connected in series;
the membrane aperture of the microfiltration membrane is 0.1-0.2 mu m;
the water adding amount during the washing and filtering of the 2 nd-stage microfiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage microfiltration membrane; the water adding amount during washing and filtering of the 3 rd stage microfiltration membrane is 60-80% of the intercepting liquid flow and/or the penetrating liquid flow of the 3 rd stage microfiltration membrane.
5. Membrane separation and recombination method of core nutritional components of infant milk products according to claim 1 or 2, characterized by comprising: the multistage ultrafiltration is a continuous ultrafiltration system; the continuous ultrafiltration system mainly comprises 3-5 stages of ultrafiltration membranes which are connected in series; the 1 st-stage ultrafiltration membrane is not washed and filtered, and the water consumption of any one of the ultrafiltration membranes except the 1 st-stage ultrafiltration membrane during washing and filtering is determined by the retentate flow rate and/or the permeate flow rate of the corresponding stage.
6. The membrane separation and recombination method of core nutritional ingredients of infant milk products according to claim 5, wherein the ultrafiltration membrane has a membrane pore size of: 1000D-50000D;
the water adding amount during washing and filtering of the 2 nd-stage micro-ultrafiltration membrane is 60-80% of the retentate flow and/or the permeate flow of the 2 nd-stage ultrafiltration; the water adding amount during washing and filtering of the 3 rd-stage ultrafiltration membrane is 60-80% of the trapped fluid flow and/or the permeate fluid flow of the 3 rd-stage ultrafiltration.
7. Membrane separation and recombination method of core nutritional components of infant milk products according to claim 1 or 2, characterized by comprising: the fat content of the skim milk is less than or equal to 0.08%;
the degreasing temperature in degreasing is 45-55 ℃.
8. Membrane separation and recombination method of core nutritional components of infant milk products according to claim 1 or 2, characterized by comprising: desalting the whey protein concentrate by an ion exchange or electrodialysis technology to prepare the desalted whey protein concentrate; judging the desalination end point according to the conductivity change of the whey protein concentrate;
and/or desalting the lactose concentrated solution by an ion exchange or electrodialysis technology to prepare the desalted lactose concentrated solution; the endpoint of desalination was determined from the conductivity change of the lactose concentrate.
9. The infant milk product comprises infant formula liquid milk, infant formula powder, infant formula fresh milk or infant protein pudding, and is characterized in that more than 95% of core nutritional ingredients in the infant milk product are from more than one of cream, casein trapped fluid, whey protein concentrated solution and lactose concentrated solution by mass percent;
the cream, the casein retentate, the whey protein concentrate and the lactose concentrate are prepared by the method of any one of claims 1-8.
10. An electronic device comprising a memory, a processor and a computer program stored on the memory and executable on the processor, wherein the processor, when executing the program, implements a method for membrane separation and reconstitution of core nutritional ingredients of infant milk products according to any one of claims 1 to 8.
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