CN112655768A - Preparation method of milk powder containing lactoferrin - Google Patents
Preparation method of milk powder containing lactoferrin Download PDFInfo
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Abstract
The invention provides a preparation method of milk powder containing lactoferrin. The preparation method comprises the following steps: step S1, performing cream separation treatment on the liquid milk to obtain skim milk A and cream; step S2, carrying out chromatography treatment on the skim milk A to obtain skim milk B and crude lactoferrin; step S3, preparing milk powder by using the skim milk B; step S4, purifying the crude lactoferrin to obtain lactoferrin; and step S5, mixing the lactoferrin with the milk powder according to a set proportion to obtain the milk powder containing the lactoferrin. This application carries out cream separation processing and carries out chromatography with skim milk A through directly carrying out liquid milk, obtains skim milk B and crude lactoferrin to carry out solitary lactoferrin purification to the crude lactoferrin that obtains, and utilize the separation to obtain skim milk B simultaneously and carry out the preparation of milk powder. The preparation method does not need to buy expensive commercial lactoferrin separately, and reduces the production cost of the milk powder containing lactoferrin.
Description
Technical Field
The invention relates to the technical field of milk powder preparation, and particularly relates to a preparation method of milk powder containing lactoferrin.
Background
Lactoferrin is widely present in mammalian milk and is a multifunctional iron-binding glycoprotein having antibacterial, antiviral, immunomodulating, iron absorption promoting, osteocyte proliferation promoting, etc. properties. Meanwhile, lactoferrin is a heat-sensitive protein, and is easy to denature due to too high temperature, and researches show that in a lower pasteurization temperature range, the heating has little influence on the antibacterial activity of bovine lactoferrin, and the overhigh temperature (90-120 ℃) can denature the bovine lactoferrin, so that the antibacterial activity of the bovine lactoferrin is greatly reduced. The milk powder is prepared by taking raw milk and milk products thereof as raw materials in the production process, adding or not adding other raw materials, food additives and nutrition enhancers, homogenizing, sterilizing (85-95 ℃ for 10-40 s), concentrating and spray drying (the air inlet temperature is 170-185 ℃), so that the lactoferrin denaturation rate is very high, and the active lactoferrin content in the milk powder is very low.
Although the extraction and purification of lactoferrin have already been realized in industrial production, raw milk or cheese whey is used as a raw material and extracted by a chromatographic method; lactoferrin is widely applied to various foods, particularly infant formula milk powder, and is unavailable through a whey way due to laggard cheese industry and lack of whey resources in China; in addition, due to regulation, the milk after extracting the lactoferrin from the milk cannot be sold in the form of liquid milk and milk powder, so that the lactoferrin in China completely depends on import. In recent years, the national standard of lactoferrin improves the proportion of lactoferrin in protein to 90% to 95%, which leads to shortage of lactoferrin raw materials meeting the national standard, so that the price of lactoferrin is increased from 0.7 ten-thousand yuan/kg to 2 ten-thousand yuan/kg, the cost of formula powder products is greatly increased, and the formula powder industry in China is further faced with the situation of 'neck clamping', therefore, the problem of lactoferrin variability in raw milk for producing milk powder is solved, and the method is one of the problems to be solved at present in producing milk powder containing lactoferrin.
Disclosure of Invention
The invention mainly aims to provide a preparation method of milk powder containing lactoferrin, and aims to solve the problem that the production cost of milk powder containing lactoferrin is high in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a method for preparing a milk powder containing lactoferrin, the method comprising: step S1, performing cream separation treatment on the liquid milk to obtain skim milk A and cream; step S2, carrying out chromatography treatment on the skim milk A to obtain skim milk B and crude lactoferrin; step S3, preparing milk powder by using the skim milk B; step S4, purifying the crude lactoferrin to obtain lactoferrin; and step S5, mixing the lactoferrin with the milk powder according to a set proportion to obtain the milk powder containing the lactoferrin.
Further, the preparation method further comprises the following steps: and (3) checking and accepting the raw milk, and purifying the raw milk to obtain liquid milk, wherein the raw milk is preferably raw cow milk or raw goat milk, and the temperature of the checked and accepted raw milk is preferably controlled to be 0-50 ℃.
Further, the step S1 includes: preheating the liquid milk to 35-55 ℃ to obtain preheated milk; and (3) performing cream separation treatment on the preheated milk to obtain skim milk A and cream, wherein the cream separation treatment is preferably centrifugal separation, the rotation speed of the centrifugal separation is 7000-15000 r/min, and the fat content of the skim milk A is 0.001-0.1%.
Further, the chromatographic column of the above chromatographic treatment is packed with an ion exchange resin, and the crude lactoferrin is adsorbed to the chromatographic column, and preferably the ion exchange resin is selected from any one or a combination of plural kinds of agarose type ion exchange resins, acrylic acid type ion exchange resins, and polystyrene type ion exchange resins.
Further, the step S4 includes: performing first elution on the chromatographic column by using a first washing solution to obtain a first elution chromatographic column and a first eluent; performing second elution on the first elution chromatographic column by using a second washing solution to obtain a second eluent; ultrafiltering the second eluent to obtain ultrafiltrate; and carrying out second drying on the ultrafiltrate to obtain lactoferrin, wherein the first washing liquid and the second washing liquid are respectively a sodium salt solution or a potassium salt solution, the pore diameter of an ultrafiltration membrane used for ultrafiltration is preferably 10-75 kD, the second drying is preferably spray drying, the second drying is preferably freeze drying, the analysis temperature of freeze drying is preferably-10-20 ℃, and the freeze drying time is preferably 6-24 hours.
Further, the concentration of the second washing reagent is higher than that of the first washing reagent, and it is more preferable that the concentration of the first washing reagent is 0.1 to 0.8mol/L and the concentration of the second washing reagent is 0.4 to 1.5 mol/L.
Further, the step S3 includes performing a first sterilization on the skim milk B to obtain sterilized skim milk B; standardizing the sterilized skim milk B and cream to obtain standardized skim milk; adopting an additive to prepare the standardized skim milk to obtain a prepared emulsion; homogenizing the ingredient emulsion to obtain homogenized emulsion; performing second sterilization on the homogenized emulsion to obtain sterilized emulsion; concentrating the sterilized emulsion to obtain a concentrated emulsion; carrying out primary drying on the concentrated emulsion to obtain milk powder, preferably carrying out primary sterilization at the temperature of 80-116 ℃, and preferably carrying out primary sterilization for 3-30 s; preferably, the temperature of the second sterilization is 92-102 ℃, and the time of the second sterilization is 0.1-1 s; the preferable additive is one or more of protein, fat and nutrient raw and auxiliary materials, the preferable homogenizing temperature is 40-60 ℃, and the preferable homogenizing pressure is 15-25 MPa.
Further, the solid content of the concentrated emulsion is 48-52%, the first drying is preferably spray drying, and the temperature of the spray drying is preferably 170-195 ℃.
Further, the cream is subjected to a third sterilization treatment before standardization, preferably the temperature of the third sterilization is 80-116 ℃, preferably the time of the third sterilization is 3-30 s, and preferably the content of the milk fat in the cream after the third sterilization treatment is 30-45%.
Further, the set ratio is that the mass ratio of the lactoferrin to the milk powder is 1: 100-10000, preferably 1: 500-5000, and the mixing time is preferably 3-15 min, preferably 5-12 min.
The inventor researches and discovers that heat denaturation loss of the lactoferrin is serious in the milk powder production process, the raw milk loses about half of the heat denaturation loss after pasteurization, the lactoferrin is uniformly and completely denatured after the sterilization and concentration processes, and the non-deformed lactoferrin is detected by adopting a heparin column method and is not detected. This application carries out milk fat separation processing and carries out chromatography with skim milk A through directly carrying out liquid milk, obtains skim milk B and crude lactoferrin to carry out solitary lactoferrin purification to the crude lactoferrin that obtains, above-mentioned in-process does not have pasteurization, has consequently avoided the lactoferrin variability that high temperature leads to. And simultaneously, the skim milk B obtained by separation is used for preparing the milk powder. Finally, the milk powder and the lactoferrin are mixed to obtain the milk powder containing the lactoferrin, so that the preparation method does not need to buy expensive commercial lactoferrin independently, the lactoferrin is extracted simultaneously in the process of preparing the milk powder, and the obtained lactoferrin is directly used for the purpose of producing the milk powder containing the lactoferrin, so that the production cost of the milk powder containing the lactoferrin is greatly reduced, the preparation method is simple, and the raw materials are easy to obtain.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a flow chart of a preparation process of a milk powder containing lactoferrin according to example 1 of the present invention;
fig. 2 shows a picture of the dissolution of milk powder corresponding to the reconstitution score of milk powder provided by the present invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged under appropriate circumstances in order to facilitate the description of the embodiments of the invention herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As analyzed by the background art, the prior art has the problem of high production cost of the milk powder containing the lactoferrin, and the invention provides a preparation method of the milk powder containing the lactoferrin for solving the problem.
In an exemplary embodiment of the present application, there is provided a method for preparing a milk powder containing lactoferrin, the method comprising: step S1, performing cream separation treatment on the liquid milk to obtain skim milk A and cream; step S2, carrying out chromatography treatment on the skim milk A to obtain skim milk B and crude lactoferrin; step S3, preparing milk powder by using the skim milk B; step S4, purifying the crude lactoferrin to obtain lactoferrin; and step S5, mixing the lactoferrin with the milk powder according to a set proportion to obtain the milk powder containing the lactoferrin.
The inventor researches and discovers that heat denaturation loss of the lactoferrin is serious in the milk powder production process, the raw milk loses about half of the heat denaturation loss after pasteurization, the lactoferrin is uniformly and completely denatured after the sterilization and concentration processes, and the non-deformed lactoferrin is detected by adopting a heparin column method and is not detected. This application carries out milk fat separation processing and carries out chromatography with skim milk A through directly carrying out liquid milk, obtains skim milk B and crude lactoferrin to carry out solitary lactoferrin purification to the crude lactoferrin that obtains, above-mentioned in-process does not have pasteurization, has consequently avoided the lactoferrin variability that high temperature leads to. And simultaneously, the skim milk B obtained by separation is used for preparing the milk powder. Finally, the milk powder and the lactoferrin are mixed to obtain the milk powder containing the lactoferrin, so that the preparation method does not need to buy expensive commercial lactoferrin independently, the lactoferrin is extracted simultaneously in the process of preparing the milk powder, and the obtained lactoferrin is directly used for the purpose of producing the milk powder containing the lactoferrin, so that the production cost of the milk powder containing the lactoferrin is greatly reduced, the preparation method is simple, and the raw materials are easy to obtain.
In order to improve the cleanliness indexes of lactoferrin and powdered milk, in an embodiment of the present application, the preparation method further includes: and (3) checking and accepting the raw milk, and purifying the raw milk to obtain liquid milk, wherein the raw milk is preferably raw cow milk or raw goat milk, and the temperature of the checked and accepted raw milk is preferably controlled to be 0-50 ℃.
The microbial indexes of the raw milk are as follows: the total number of bacterial colonies is 0-30 ten thousand CFU/mL, the total number of aerobic spores is 0-50 CFU/mL, the number of thermophilic aerobic spores is 0-50 CFU/mL, the number of psychrophilic bacteria is 0-10000 CFU/mL, raw milk is inspected and cleaned at the temperature of 0-50 ℃, and the loss of lactoferrin in the raw milk can be reduced as much as possible through controlling the temperature, so that processed milk with high lactoferrin content is obtained, and the subsequent efficient extraction of lactoferrin is facilitated.
In an embodiment of the present application, the step S1 includes: preheating the liquid milk to 35-55 ℃ to obtain preheated milk; and (3) performing cream separation treatment on the preheated milk to obtain skim milk A and cream, wherein the cream separation treatment is preferably centrifugal separation, the rotation speed of the centrifugal separation is 7000-15000 r/min, and the fat content of the skim milk A is 0.001-0.1%.
After the liquid milk is preheated to 35-55 ℃, on one hand, heat loss to the lactoferrin is avoided, on the other hand, the separation effect of the skim milk A and the cream is better improved, and the centrifugal separation at the rotating speed is more favorable for separating the skim milk A and the cream as much as possible, so that the skim milk A with the fat content is obtained, and the interference effect of the fat on the purified lactoferrin is reduced. Of course, the milk after the preheating is subjected to the cream separation process by a person skilled in the art with reference to conventional separation methods known in the art.
In one embodiment of the present application, lactoferrin is adsorbed to a chromatography column using an ion exchange resin to separate skim milk B from crude lactoferrin, and in order to improve the adsorption effect, the chromatography column is preferably packed with an ion exchange resin, and the crude lactoferrin is adsorbed to the chromatography column, and preferably the ion exchange resin is selected from any one or a combination of plural kinds of ion exchange resins of an agarose type, an acrylic acid type, and a polystyrene type.
In an embodiment of the present application, the step S4 includes: performing first elution on the chromatographic column by using a first washing solution to obtain a first elution chromatographic column and a first eluent; performing second elution on the first elution chromatographic column by using a second washing solution to obtain a second eluent; ultrafiltering the second eluent to obtain ultrafiltrate; and carrying out second drying on the ultrafiltrate to obtain lactoferrin, wherein the first washing liquid and the second washing liquid are respectively a sodium salt solution or a potassium salt solution, the pore diameter of an ultrafiltration membrane used for ultrafiltration is preferably 10-75 kD, the second drying is preferably spray drying, the second drying is preferably freeze drying, the analysis temperature of freeze drying is preferably-10-20 ℃, and the freeze drying time is preferably 6-24 hours.
Most of impurities in the crude lactoferritin are removed through the first elution of the chromatographic column by the first washing liquid, so that the crude lactoferritin is primarily purified. And carrying out second elution on the first elution chromatographic column after impurity removal so as to wash the lactoferrin adsorbed in the chromatographic column into second eluent, and carrying out ultrafiltration on the second eluent so as to further remove impurities in the lactoferrin, so that the crude lactoferrin is purified again, and the lactoferrin with higher relative purity is obtained. Wherein the freeze-drying is beneficial to avoid denaturation of the lactoferrin, thereby reducing the lactoferrin loss in the second drying of the ultrafiltrate.
In order to improve the efficiency and elution effect of the two elutions, the concentration of the second washing reagent is preferably higher than the concentration of the first washing reagent, and more preferably the concentration of the first washing reagent is 0.1 to 0.8mol/L and the concentration of the second washing reagent is 0.4 to 1.5 mol/L.
In an embodiment of the present application, the step S3 includes performing a first sterilization on the skim milk B to obtain sterilized skim milk B; standardizing the sterilized skim milk B and cream to obtain standardized skim milk; adopting an additive to prepare the standardized skim milk to obtain a prepared emulsion; homogenizing the ingredient emulsion to obtain homogenized emulsion; performing second sterilization on the homogenized emulsion to obtain sterilized emulsion; concentrating the sterilized emulsion to obtain a concentrated emulsion; carrying out primary drying on the concentrated emulsion to obtain milk powder, preferably carrying out primary sterilization at the temperature of 80-116 ℃, and preferably carrying out primary sterilization for 3-30 s; preferably, the temperature of the second sterilization is 92-102 ℃, and the time of the second sterilization is 0.1-1 s; the preferable additive is one or more of protein, fat and nutrient raw and auxiliary materials, the preferable homogenizing temperature is 40-60 ℃, and the preferable homogenizing pressure is 15-25 MPa.
The preparation process of the milk powder can refer to the prior art, and the preparation process is preferably carried out under the conditions in order to improve the preparation efficiency of the milk powder. Wherein the control of the temperature and time of the first sterilization and the second sterilization is helpful for removing bacteria, and the milk powder with the least bacteria is obtained; the category of the additive is beneficial to balancing the nutrition of the milk powder; the homogenization condition is favorable for enabling the powder of the milk powder to be easier to redissolve as much as possible, thereby obtaining the milk powder with higher quality on the whole.
In order to reduce the working difficulty of the first drying and shorten the period of the first drying, the solid content of the concentrated emulsion is preferably 48-52%, the first drying is preferably spray drying, and the temperature of the spray drying is preferably 170-195 ℃.
In one embodiment of the present application, the cream is subjected to a third sterilization treatment before standardization, preferably the third sterilization temperature is 80 to 116 ℃, preferably the third sterilization time is 3 to 30 seconds, and preferably the cream after the third sterilization treatment has a milk fat content of 30 to 45%.
The third sterilization on the cream is beneficial to reducing the interference effect of bacteria on standardization and avoiding the influence of the bacteria in the cream on the quality of the final milk powder.
In one embodiment of the present application, the set ratio is that the mass ratio of lactoferrin to milk powder is 1:100 to 10000, preferably 1:500 to 5000, and the mixing time is preferably 3 to 15min, preferably 5 to 12 min.
The lactoferrin and the milk powder are simultaneously obtained by the preparation method, the lactoferrin and the milk powder do not need to be purchased separately, and the milk powder containing the lactoferrin can be obtained only by mixing the lactoferrin and the milk powder according to the proportion, so that the production cost is greatly reduced, wherein the mixing can be carried out by adopting a pneumatic mixing or machine stirring mixing method.
The advantageous effects of the present application will be described below with reference to specific examples and comparative examples.
Example 1
This example provides a lactoferrin enriched baby formula milk powder, prepared per 1000 parts of milk powder, without considering lactoferrin, from the following components:
3200 parts of raw milk, 375 parts of desalted whey powder, 40 parts of lactose, 85 parts of galacto-oligosaccharide, 80 parts of vegetable oil, 10 parts of ARA powder, 10 parts of DHA powder, 45 parts of whey protein powder, 5 parts of calcium citrate, 3 parts of compound vitamin and 1 part of compound mineral substance.
(1) And (4) acceptance: the microorganism indexes in the raw milk are as follows: the total number of colonies is 2.44 ten thousand CFU/mL, the total number of aerobic spores is 10CFU/mL, the number of thermophilic aerobic spores is 5CFU/mL, the number of psychrophiles is 780CFU/mL, and other indexes meet GB 19301.
(2) Cleaning milk: 3200 parts of raw milk is filtered, degassed, purified and cooled to 8 ℃ to obtain liquid milk, and the heat treatment temperature of the liquid milk in the processes of milk collection and acceptance inspection is 20 ℃.
(3) Cream treatment: preheating the liquid milk at 45 deg.C, performing cream separation with butterfly centrifuge at a separation speed of 8000r/min to obtain skim milk A with fat content of 0.05%.
Skim milk A: cooling to 6 deg.C, and storing in skimmed milk A tank.
② dilute cream: pasteurizing at 85 deg.C for 30s, cooling to 6 deg.C, and storing in cream jar.
(3) Chromatography treatment
Firstly, extraction: and allowing the skim milk A to pass through a chromatographic column filled with agarose ion exchange resin, adsorbing lactoferrin by ion resin, pasteurizing the flowing skim milk B at 85 ℃ for 30s, cooling to 6 ℃, and temporarily storing in a skim milk B tank.
Elution: after the agarose ionic resin adsorbs lactoferrin and reaches full load, firstly, 0.1mol/L sodium chloride solution is adopted for first elution to obtain a first elution chromatographic column and first eluent, and then 0.4mol/L sodium chloride solution is adopted for second elution to the first elution chromatographic column to obtain second eluent.
③ desalting: and (4) carrying out ultrafiltration on the second eluent by adopting a flat membrane ultrafiltration membrane with the pore diameter of 60kD to obtain ultrafiltrate.
Fourthly, second drying: and (3) carrying out low-temperature freeze drying on the ultrafiltrate, wherein the resolution temperature of the freeze drying is 0 ℃, and the freeze drying time is 20h, so that 0.361 part of lactoferrin is obtained, and the purity (of the lactoferrin accounts for 97.1 percent of the protein).
(4) And (3) standardization: and standardizing the skim milk B and the cream to obtain standardized skim milk.
(5) Preparing materials: adding the standardized skim milk into a blending tank, sequentially adding 375 parts of desalted whey powder, 40 parts of lactose, 85 parts of galacto-oligosaccharide, 80 parts of vegetable oil, 10 parts of ARA powder, 10 parts of DHA powder, 45 parts of whey protein powder, 5 parts of calcium citrate, 3 parts of compound vitamin and 1 part of compound mineral substance, and mixing to obtain a blended emulsion.
(6) Homogenizing: homogenizing the mixture emulsion to obtain homogenized emulsion at 45 deg.C and 20MPa, and cooling to 6 deg.C.
(7) And (5) second sterilization: and heating the homogenized emulsion to 43-47 ℃, then carrying out flash evaporation, and carrying out instant sterilization (0.1s) on the flash-evaporated material at 98 ℃ to obtain the sterilized emulsion.
(8) Concentration: and concentrating the sterilized emulsion to obtain a concentrated emulsion, wherein the solid content of the concentrated emulsion is 50%.
(9) First drying: and (3) carrying out spray drying on the concentrated emulsion under the conditions that the temperature of a main fan is 180 ℃ and the exhaust temperature is 95 ℃, cooling to obtain milk powder, and carrying out detection on various indexes.
(10) Mixing: the lactoferrin and the milk powder are mixed according to the ratio of 1:5000, the mixing time of a machine stirring type dry mixer is 5min, the infant formula milk powder rich in lactoferrin is obtained, the lactoferrin content in the milk powder is 35mg/100g, the infant formula milk powder is detected and packaged, and the process flow can refer to fig. 1.
Example 2
Example 2 differs from example 1 in that the heat treatment temperature of the liquid milk in the processes of receiving and accepting milk is 0 ℃, the total number of bacterial colonies is 2.43 ten thousand CFU/mL, the total number of aerobic spores is 8CFU/mL, the number of thermophilic aerobic spores is 4CFU/mL, the number of psychrophilic bacteria is 650CFU/mL, 0.363 parts of lactoferrin is obtained, the purity of lactoferrin (accounting for protein) is 96.8%, and finally the infant formula milk powder rich in lactoferrin is obtained, and the lactoferrin content in the milk powder is 35.1mg/100 g.
Example 3
Example 3 differs from example 1 in that the heat treatment temperature of the liquid milk during the milk receiving and acceptance treatment is 50 ℃, and the microbial indicators in the obtained liquid milk are as follows: the total number of colonies is 3.36 ten thousand CFU/mL, the total number of aerobic spores is 11CFU/mL, the number of thermophilic aerobic spores is 8CFU/mL, the number of psychrophiles is 830CFU/mL, 0.347 parts of lactoferrin is obtained, the purity (accounting for protein) of lactoferrin is 95.7%, and the infant formula milk powder rich in lactoferrin is finally obtained, wherein the lactoferrin content in the milk powder is 33.2mg/100 g.
Example 4
Example 4 differs from example 1 in that the heat treatment temperature of the liquid milk during the milk receiving and acceptance treatment is 70 ℃, and the microorganism indexes of the obtained liquid milk are as follows: the total number of bacterial colonies is 0.068 ten thousand CFU/mL, the total number of aerobic spores is 8CFU/mL, the number of thermophilic aerobic spores is 3CFU/mL, the number of psychrophilic bacteria is 420CFU/mL, 0.216 parts of lactoferrin is obtained, the purity (accounting for protein) of lactoferrin is 88.1%, and finally the lactoferrin-enriched infant formula milk powder is obtained, wherein the lactoferrin content in the milk powder is 19mg/100 g.
Example 5
Example 5 differs from example 1 in that the ion exchange resin was an acrylic type ion exchange resin, yielding 0.356 parts of lactoferrin, with a lactoferrin purity (protein) of 95.8%, and finally yielding a lactoferrin enriched baby formula with a lactoferrin content of 34.1mg/100 g.
Example 6
Example 6 differs from example 1 in that after preheating the liquid milk to 35 ℃, preheated milk is obtained, the rotation speed of centrifugal separation is 7000r/min, the fat content of skim milk a is 0.1%, 0.366 parts of lactoferrin is obtained, the purity of lactoferrin (protein) is 96.3%, and finally the infant formula milk powder rich in lactoferrin is obtained, wherein the lactoferrin content in the milk powder is 35.2mg/100 g.
Example 7
Example 7 differs from example 1 in that after preheating the liquid milk to 55 ℃, preheated milk is obtained, the rotation speed of centrifugal separation is 15000r/min, the fat content of skim milk a is 0.001%, 0.370g of lactoferrin is obtained, the purity (protein content) of lactoferrin is 95.1%, and finally the infant formula milk powder rich in lactoferrin is obtained, and the lactoferrin content in the milk powder is 35.2mg/100 g.
Example 8
Example 8 differs from example 1 in that the pore size of the flat membrane ultrafiltration membrane is 10kD, 0.371 parts of lactoferrin is obtained, the purity of lactoferrin (protein) is 96.2%, and finally the lactoferrin-rich infant formula milk powder is obtained, wherein the lactoferrin content in the milk powder is 35.6mg/100 g.
Example 9
Example 9 differs from example 1 in that the pore size of the flat membrane ultrafiltration membrane is 75kD, 0.367 parts of lactoferrin is obtained, the purity (protein) of the lactoferrin is 96.9%, and finally the lactoferrin-rich infant formula milk powder with the lactoferrin content of 35.6mg/100g is obtained.
Example 10
Example 10 differs from example 1 in that the resolution temperature of the freeze-drying was 10 ℃ and the freeze-drying time was 24 hours, yielding 0.368 parts of lactoferrin, with a lactoferrin purity (protein content) of 96.8%, and finally yielding a lactoferrin-enriched baby formula, with a lactoferrin content of 35.6mg/100 g.
Example 11
Example 11 differs from example 1 in that the desorption temperature of the freeze-drying is 20 ℃ and the freeze-drying time is 12 hours, thus obtaining 0.368 parts of lactoferrin, the purity (protein) of the lactoferrin is 95.6%, and finally obtaining the infant formula milk powder rich in the lactoferrin, wherein the lactoferrin content in the milk powder is 35.2mg/100 g.
Example 12
Example 12 differs from example 1 in that the resolving temperature of freeze-drying was 30 ℃ and the freeze-drying time was 6 hours, yielding 0.365 parts of lactoferrin, with a lactoferrin purity (protein) of 91.6%, and finally yielding a lactoferrin-enriched baby formula, with a lactoferrin content of 33.4mg/100 g.
Example 13
Example 13 differs from example 1 in that first elution is performed with 0.5mol/L sodium chloride solution to obtain a first elution chromatographic column and a first eluent, and then second elution is performed with 1.2mol/L sodium chloride solution to obtain 0.362 parts of lactoferrin, wherein the purity of lactoferrin (protein) is 95.6%, and finally lactoferrin-enriched formula milk powder for infants is obtained, wherein the lactoferrin content in the milk powder is 34.6mg/100 g.
Example 14
Example 14 differs from example 1 in that first elution is performed with 0.8mol/L sodium chloride solution to obtain a first elution chromatographic column and a first eluent, and then second elution is performed with 1.5mol/L sodium chloride solution to obtain 0.369 parts of lactoferrin, the purity of lactoferrin (protein) is 95.8%, finally lactoferrin enriched formula milk powder for young children is obtained, and the lactoferrin content in the milk powder is 35.3mg/100 g.
Example 15
Example 15 differs from example 1 in that first elution is performed with 0.6mol/L sodium chloride solution to obtain a first elution chromatographic column and a first eluent, and then second elution is performed with 0.4mol/L sodium chloride solution to obtain 0.372 parts of lactoferrin, wherein the purity of lactoferrin (protein) is 96.7%, and finally lactoferrin-enriched infant formula milk powder is obtained, wherein the lactoferrin content in the milk powder is 33.2mg/100 g.
Example 16
Example 16 differs from example 15 in that the sodium chloride solution was replaced by the corresponding potassium chloride solution, yielding 0.367 parts of lactoferrin, with a lactoferrin purity (protein) of 96.3%, and finally yielding a lactoferrin enriched baby formula, with a lactoferrin content of 35.3mg/100g in the milk.
Example 17
Example 17 differs from example 1 in that cream is pasteurized at 80 ℃ for 20s, skim milk B is pasteurized at 80 ℃ for 20s, the batch emulsion is homogenized at 40 ℃ under a homogenization pressure of 15Mpa, the homogenized emulsion is pasteurized at 92 ℃ for 0.1s, the solid content of the concentrated emulsion is 48%, and the first drying temperature is 170 ℃ to finally obtain the lactoferrin-rich infant formula milk powder.
Example 18
Example 18 differs from example 1 in that cream was pasteurized at 116 ℃ for 3s, skim milk B was pasteurized at 116 ℃ for 3s, the batch emulsion was homogenized at 60 ℃ under 25Mpa, the homogenized emulsion was pasteurized at 102 ℃ for 1s, the solids content of the concentrated emulsion was 52%, the first drying temperature was 195 ℃, and finally a lactoferrin enriched baby formula was obtained.
Example 19
Example 19 differs from example 1 in that the lactoferrin is mixed with the powdered milk in a ratio of 1:500 for a period of 12min, resulting in a lactoferrin enriched infant formula.
Example 20
Example 20 differs from example 1 in that the lactoferrin was mixed with the powdered milk in a ratio of 1:100 for a period of 3min to finally obtain a lactoferrin enriched infant formula.
Example 21
Example 21 differs from example 1 in that the lactoferrin is mixed with the milk powder in a ratio of 1:10000 for 15min, resulting in a lactoferrin enriched infant formula.
Example 22
Example 22 differs from example 1 in that 5000 parts of raw milk, the raw milk microbiological indicators are: the total number of colonies was 1.13 ten thousand CFU/mL, the total number of aerobic spores was 8CFU/mL, the number of thermophilic aerobic spores was 9CFU/mL, and the number of psychrophiles was 960 CFU/mL. The additive is 215 parts of solid corn syrup, 170 parts of desalted whey powder, 215 parts of solid corn syrup and 20 parts of fructo-oligosaccharide to obtain 0.536 part of lactoferrin, the purity (of lactoferrin accounts for protein) of the lactoferrin is 97.9 percent, and the modified milk powder rich in lactoferrin is finally obtained, wherein the lactoferrin content in the milk powder is 52.5mg/100 g.
Example 23
Example 23 differs from example 1 in 7600 parts of raw milk, and the microbial indicators of raw milk are: the total number of colonies was 3.23 ten thousand CFU/mL, the total number of aerobic spores was 15CFU/mL, the number of thermophilic aerobic spores was 20CFU/mL, and the number of psychrophiles was 1250 CFU/mL. The additive is 20 parts of fructo-oligosaccharide and 1 part of compound nutrient, and 0.921 part of lactoferrin is obtained, the purity (accounting for protein) of the lactoferrin is 97.7 percent, and the modified milk powder rich in lactoferrin is finally obtained, wherein the content of the lactoferrin in the milk powder is 90mg/100 g.
Example 24
Example 24 differs from example 1 in that the heat treatment temperature of the liquid milk during the milk receiving and acceptance treatment is 10 ℃, and the microbial indicator in the liquid milk is: the total number of colonies is 155 ten thousand CFU/mL, the total number of aerobic spores is 90CFU/mL, the number of thermophilic aerobic spores is 120CFU/mL, the number of psychrophilic bacteria is 22500CFU/mL, 0.359 parts of lactoferrin is obtained, the purity (accounting for protein) of the lactoferrin is 95.3%, and the lactoferrin-enriched infant formula milk powder is finally obtained, wherein the lactoferrin content in the milk powder is 34.2mg/100 g.
Comparative example 1
The difference between the comparative example 1 and the example 23 is that the additional addition of the lactoferrin is purchased commercially, the purchase price of the lactoferrin market is 1.8 ten thousand yuan/kg, the undenatured lactoferrin in the product reaches 81.3mg/100g, and the formula cost of the product is 48620 yuan/ton; by the preparation method of the embodiment 1, the extraction and protection of the lactoferrin are realized, and the lactoferrin is backfilled, so that the unmodified lactoferrin of the product reaches 82.1mg/100g, the formula cost of the product is 35520 yuan/ton, and the cost is 13100 yuan/ton, which is specifically shown in table 1.
Comparative example 2
The difference between the comparative example 2 and the example 1 is that the liquid milk is pasteurized at 100 ℃ and then is subjected to milk fat separation treatment to finally obtain the modified milk powder, and lactoferrin is not detected.
TABLE 1
| Item | Example 23 | Comparative example 1 |
| Milk ironProtein content | 82.1 | 81.3 |
| Cost per ton of flour (Yuan) | 35520 | 48620 |
The extraction rate of lactoferrin in the above examples 1, 22 and 23 was more than 75%, and the extraction rate of undenatured lactoferrin in the examples 1, 22 and 23 was 32.3mg/100g, 52.5mg/100g and 90mg/100g, respectively, while the extraction rate of undenatured lactoferrin in the comparative example 2 was not detected, which is shown in table 2.
TABLE 2
The method for judging the dissolving property of milk powder comprises the following steps: respectively taking 200mL of warm water with the temperature of 50 ℃, respectively adding 25g of any one of the milk powders obtained in the examples 1 to 24, the comparative example 1 and the comparative example 2, stirring for 10 circles by a small spoon, observing the dissolution state, namely the brewing score, specifically judging the standard as shown in the following table 3, and listing the final test result as shown in the table 4, wherein the dissolution condition of the milk powder corresponding to each brewing score is shown in the figure 2.
TABLE 3
TABLE 4
In the above example 24, since the microbial indicators in the liquid milk are relatively high, the total number of bacterial colonies is difficult to control in the production process, and the acidity of the product is high, so that the reconstitution property is poor, as can be seen from the comparison between the comparative example 1 and the example 23, the method of the present application can greatly reduce the production cost, and the liquid milk in the comparative example 2 has the lactoferrin basically destroyed in the sterilization process before the cream separation treatment, so that the preparation method of the present application can obtain the milk-containing ferritin milk powder with low cost and guaranteed quality.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
the inventor researches and discovers that heat denaturation loss of the lactoferrin is serious in the milk powder production process, the raw milk loses about half of the heat denaturation loss after pasteurization, the lactoferrin is uniformly and completely denatured after the sterilization and concentration processes, and the non-deformed lactoferrin is detected by adopting a heparin column method and is not detected. This application carries out milk fat separation processing and carries out chromatography with skim milk A through directly carrying out liquid milk, obtains skim milk B and crude lactoferrin to carry out solitary lactoferrin purification to the crude lactoferrin that obtains, above-mentioned in-process does not have pasteurization, has consequently avoided the lactoferrin variability that high temperature leads to. And simultaneously, the skim milk B obtained by separation is used for preparing the milk powder. Finally, the milk powder and the lactoferrin are mixed to obtain the milk powder containing the lactoferrin, so that the preparation method does not need to buy expensive commercial lactoferrin independently, the lactoferrin is extracted simultaneously in the process of preparing the milk powder, and the obtained lactoferrin is directly used for the purpose of producing the milk powder containing the lactoferrin, so that the production cost of the milk powder containing the lactoferrin is greatly reduced, the preparation method is simple, and the raw materials are easy to obtain.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The preparation method of the milk powder containing the lactoferrin is characterized by comprising the following steps:
step S1, performing cream separation treatment on the liquid milk to obtain skim milk A and cream;
step S2, carrying out chromatography treatment on the skim milk A to obtain skim milk B and crude lactoferrin;
step S3, preparing milk powder by using the skim milk B;
step S4, purifying the crude lactoferrin to obtain lactoferrin;
and step S5, mixing the lactoferrin with the milk powder in a set ratio to obtain the milk powder containing lactoferrin.
2. The method of manufacturing according to claim 1, further comprising: and (2) checking and accepting the raw milk, and purifying the raw milk to obtain the liquid milk, preferably selecting the raw milk as raw cow milk or raw goat milk, and preferably controlling the temperature of the checked and accepted raw milk and the temperature of the purified milk to be 0-50 ℃.
3. The production method according to claim 1 or 2, wherein the step S1 includes:
preheating the liquid milk to 35-55 ℃ to obtain preheated milk;
and (2) carrying out the cream separation treatment on the preheated milk to obtain the skim milk A and the cream, preferably, the cream separation treatment is centrifugal separation, preferably, the rotating speed of the centrifugal separation is 7000-15000 r/min, and preferably, the fat content of the skim milk A is 0.001-0.1%.
4. The preparation method according to any one of claims 1 to 3, wherein the chromatography column is packed with an ion exchange resin, and the crude lactoferrin is adsorbed to the chromatography column, and preferably the ion exchange resin is selected from any one or a combination of more of an agarose type ion exchange resin, an acrylic acid type ion exchange resin, and a polystyrene type ion exchange resin.
5. The method for preparing a composite material according to claim 4, wherein the step S4 includes:
performing first elution on the chromatographic column by using a first washing solution to obtain a first elution chromatographic column and a first eluent;
performing second elution on the first elution chromatographic column by using a second washing solution to obtain a second eluent;
carrying out ultrafiltration on the second eluent to obtain ultrafiltrate;
carrying out second drying on the ultrafiltrate to obtain the lactoferrin,
the first washing liquid and the second washing liquid are respectively and independently sodium salt solution or potassium salt solution, the aperture of an ultrafiltration membrane used for ultrafiltration is preferably 10-75 kD, the second drying is preferably spray drying, the second drying is preferably freeze drying, the resolution temperature of the freeze drying is preferably-10-20 ℃, and the freeze drying time is preferably 6-24 h.
6. The process according to claim 5, wherein the concentration of the second washing reagent is higher than that of the first washing reagent, and more preferably the concentration of the first washing reagent is 0.1 to 0.8mol/L and the concentration of the second washing reagent is 0.4 to 1.5 mol/L.
7. The production method according to any one of claims 1 to 3, wherein the step S3 includes,
performing first sterilization on the skim milk B to obtain sterilized skim milk B;
standardizing the sterilized skim milk B and the cream to obtain standardized skim milk;
adopting an additive to prepare the standardized skim milk to obtain a prepared emulsion;
homogenizing the ingredient emulsion to obtain homogenized emulsion;
performing second sterilization on the homogenized emulsion to obtain sterilized emulsion;
concentrating the sterilized emulsion to obtain a concentrated emulsion;
carrying out first drying on the concentrated emulsion to obtain the milk powder,
preferably, the temperature of the first sterilization is 80-116 ℃, and the time of the first sterilization is 3-30 s; preferably, the temperature of the second sterilization is 92-102 ℃, and the time of the second sterilization is 0.1-1 s; preferably, the additive is selected from one or more of protein, fat and nutrient raw and auxiliary materials, the homogenizing temperature is preferably 40-60 ℃, and the homogenizing pressure is preferably 15-25 MPa.
8. The preparation method according to claim 7, wherein the solid content of the concentrated emulsion is 48-52%, preferably the first drying is spray drying, and preferably the temperature of the spray drying is 170-195 ℃.
9. The method according to claim 7, wherein the cream is subjected to a third sterilization treatment before being standardized, preferably the temperature of the third sterilization is 80-116 ℃, preferably the time of the third sterilization is 3-30 s, and preferably the cream after the third sterilization treatment has a milk fat content of 30-45%.
10. The preparation method according to any one of claims 1 to 3, wherein the set ratio is such that the mass ratio of the lactoferrin to the milk powder is 1:100 to 10000, preferably 1:500 to 5000, and preferably the mixing time is 3 to 15min, preferably 5 to 12 min.
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