CN110623243B - High calcium salt compound and preparation method thereof - Google Patents

High calcium salt compound and preparation method thereof Download PDF

Info

Publication number
CN110623243B
CN110623243B CN201910860364.XA CN201910860364A CN110623243B CN 110623243 B CN110623243 B CN 110623243B CN 201910860364 A CN201910860364 A CN 201910860364A CN 110623243 B CN110623243 B CN 110623243B
Authority
CN
China
Prior art keywords
calcium salt
whey
content
high calcium
mass
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910860364.XA
Other languages
Chinese (zh)
Other versions
CN110623243A (en
Inventor
刘豪
宗学醒
闫清泉
李志国
李玲玉
边燕飞
王彩霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Inner Mongolia Mengniu Dairy Group Co Ltd
Original Assignee
Inner Mongolia Mengniu Dairy Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Inner Mongolia Mengniu Dairy Group Co Ltd filed Critical Inner Mongolia Mengniu Dairy Group Co Ltd
Priority to CN201910860364.XA priority Critical patent/CN110623243B/en
Publication of CN110623243A publication Critical patent/CN110623243A/en
Application granted granted Critical
Publication of CN110623243B publication Critical patent/CN110623243B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/40Table salts; Dietetic salt substitutes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • A23L33/10Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
    • A23L33/16Inorganic salts, minerals or trace elements
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/04Sulfur, selenium or tellurium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/06Aluminium, calcium or magnesium; Compounds thereof, e.g. clay
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K33/00Medicinal preparations containing inorganic active ingredients
    • A61K33/42Phosphorus; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K35/00Medicinal preparations containing materials or reaction products thereof with undetermined constitution
    • A61K35/12Materials from mammals; Compositions comprising non-specified tissues or cells; Compositions comprising non-embryonic stem cells; Genetically modified cells
    • A61K35/20Milk; Whey; Colostrum
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P3/00Drugs for disorders of the metabolism
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/80Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
    • Y02P60/87Re-use of by-products of food processing for fodder production

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Epidemiology (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Nutrition Science (AREA)
  • Diabetes (AREA)
  • Biotechnology (AREA)
  • Hematology (AREA)
  • Obesity (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Cell Biology (AREA)
  • Developmental Biology & Embryology (AREA)
  • Immunology (AREA)
  • Virology (AREA)
  • Zoology (AREA)
  • Mycology (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention provides a high calcium salt compound, a preparation method thereof and a food or a medicine containing the high calcium salt compound, wherein the high calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate radical, chloride ion, sulfate radical and carbonate radical, and the total content of the calcium, potassium, sodium, magnesium, phosphate radical, chloride ion, sulfate radical and carbonate radical is 90-95 mass% based on the total mass of the high calcium salt compound. The high calcium salt compound of the invention is rich in various nutrient substances, has high nutritive value, good purity and strong safety, can be used for food or medicine, and has wide application prospect.

Description

High calcium salt compound and preparation method thereof
Technical Field
The invention relates to the field of food. In particular, the invention relates to a high calcium salt compound and a preparation method thereof.
Background
99% of calcium is found in bones of the human body, and since the human body cannot produce calcium by itself, it must be ingested from food. However, many people have unbalanced dietary habits and like to eat instant food, so that not only can enough calcium be absorbed, but also calcium in the body is easily lost; in addition, the bone loss speed is increased with age, and the bone crisis can be caused after a long time. Therefore, it has become a popular trend to meet the demand of calcium in human body by eating food with high calcium added. The studies published in the international journal "lancets" show that: after the milk calcium is eaten, the increase of the bone density still exists after the milk calcium is stopped for several years, and the absorption effect is good. About 25% of calcium ions in fresh raw milk (pH of about 6.78) are on casein micelles, and how to increase calcium from insoluble to soluble calcium, i.e., a method for preparing calcium-rich salts from cow milk, is still under study.
Disclosure of Invention
The present invention aims to solve at least to some extent at least one of the technical problems of the prior art.
In one aspect of the invention, the invention provides a high calcium salt-based compound. According to the embodiment of the invention, the high calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate, wherein the total content of the calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate is 90-95 mass%, the content of the calcium is 36-38 mass%, the content of the potassium is 22-24 mass%, the content of the magnesium is 1-2 mass%, and the content of the sodium is 7-8 mass%, based on the total mass of the high calcium salt compound. According to the embodiment of the invention, the high-calcium salt compound mainly comprises calcium, potassium, sodium, magnesium, phosphate, chloride ions, sulfate radicals and carbonate, the purity (content) of the compound is as high as 90-95 mass%, and the high-calcium salt compound has high nutritional value. In addition, the safety is high, and the method can be used for food or medicines and has wide application prospect.
According to an embodiment of the present invention, the high calcium salt compound may further have the following additional technical features:
according to the embodiment of the invention, the raw material for preparing the high calcium salt compound comprises raw milk, and the ratio of the calcium content in the high calcium salt compound to the calcium content in the raw milk is 80-85 mass%; the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%; the ratio of the phosphate content in the high calcium salt compound to the phosphate content in raw milk is 55-60 mass%; the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65-70 mass%.
In another aspect of the invention, the invention provides a method for preparing high calcium salt complexes. According to an embodiment of the invention, the method comprises: (1) Curdling acidified raw milk by using rennin so as to obtain a clot, cutting, standing and stirring the clot; (2) Collecting the whey when the pH of the coagulum obtained after the stirring reaches a first predetermined pH, in order to remove casein; (3) Fermenting the whey, during which beta-lactoglobulin is removed; simultaneously, piling the curd after discharging the whey liquid, collecting the whey liquid with the pH value of whey discharged from the curd reaching a second preset pH value from the beginning of piling, and mixing the whey liquid with the whey liquid after removing the beta-lactoglobulin; (4) Fermenting the mixed whey liquid obtained in the step (3), and sequentially removing bovine serum albumin and alpha-lactalbumin to obtain a protein removing liquid; (5) And (3) filtering, sterilizing and drying the protein removing liquid by using a nanofiltration membrane so as to obtain the high calcium salt compound. Therefore, the high-calcium salt compound obtained by the method disclosed by the embodiment of the invention is high in purity, rich in calcium, magnesium, potassium, sodium, phosphate, chloride ions, sulfate and carbonate, simple and convenient to operate, high in safety and suitable for large-scale production.
According to an embodiment of the invention, said first predetermined pH value is between 6.1 and 6.2 and said second predetermined pH value is between 5.10 and 5.15.
According to an embodiment of the present invention, in the step (3), when the whey is fermented to a pH of 5.3 to 5.4, the whey is filtered, and the filtrate is collected so as to remove β -lactoglobulin.
According to an embodiment of the invention, the filtration is performed with a 1-2 micron filter membrane.
According to an embodiment of the present invention, the step (3) further comprises: when the pH of the curd-draining whey reaches a second predetermined pH, the curd is washed with water and the washed wash liquor, the collected whey and the beta-lactoglobulin-depleted whey are subjected to said mixing.
According to the embodiment of the invention, the mixing temperature of the whey liquid and the water is 25-30 ℃, and the mass ratio of the whey liquid to the water is 1: (1.8-2.3).
According to the embodiment of the invention, in the step (4), when the whey is fermented to 5.1, the whey is filtered, the filtrate is collected so as to remove bovine serum albumin, and then when the filtrate is fermented to 4.4, the filtrate is filtered, and the filtrate is collected so as to obtain the protein removing liquid.
According to an embodiment of the invention, the filtration is performed with a 1-2 micron filter membrane.
According to the embodiment of the invention, the addition amount of the rennin is 30-35g/1000kg based on the mass of the acidified raw milk.
According to an embodiment of the invention, the temperature of the curd treatment is 37-39 ℃ and the time is 35-40 minutes.
According to an embodiment of the invention, the cut of the clot is of a size of 2-3cm 2
According to the embodiment of the invention, in the step (5), the filtration is performed by adopting a nanofiltration mode, the aperture of the adopted nanofiltration membrane is 1-1.5nm, the permeation quantity is 4-5L/min, and the temperature is 30-40 ℃.
According to an embodiment of the present invention, the sterilization is performed at 75 to 85 ℃ for 24 to 30 seconds.
According to the embodiment of the invention, the drying treatment is carried out by adopting a spray drying mode, wherein the exhaust air temperature is 75-90 ℃, and the temperature of the sterilized filtrate is 40-60 ℃.
In another aspect of the present invention, the present invention provides a high calcium salt compound. According to the embodiment of the present invention, the high calcium salt-based compound is obtained by the method for preparing the high calcium salt-based compound described above. Therefore, the high-calcium salt compound provided by the embodiment of the invention has high nutritive value and high safety, can be used for food or medicines, and has a wide application prospect.
According to the embodiment of the invention, the high calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate, wherein the total content of the calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate is 90-95 mass%, the content of the calcium is 36-38 mass%, the content of the potassium is 22-24 mass%, the content of the magnesium is 1-2 mass%, and the content of the sodium is 7-8 mass%, based on the total mass of the high calcium salt compound.
According to the embodiment of the invention, the ratio of the calcium content in the high calcium salt compound to the calcium content in the raw milk is 80-85 mass% based on the mass of calcium in the raw milk; the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%; the ratio of the phosphate radical content in the high calcium salt compound to the phosphate radical content in raw cow milk is 55-60 mass%; the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65-70 mass%.
In yet another aspect of the present invention, the present invention provides a food or pharmaceutical product. According to an embodiment of the present invention, the food or pharmaceutical product contains the above-mentioned high calcium salt-based compound or the high calcium salt-based compound obtained by the above-mentioned method. As described above, the high calcium salt compound has high purity, is rich in calcium, magnesium, potassium, sodium, phosphate, chloride, sulfate and carbonate, has high nutritive value and high safety, and can be used as food or medicine.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The following describes in detail embodiments of the present invention. The following examples are illustrative only and are not to be construed as limiting the invention.
The present invention provides a high calcium salt-based compound, a method for producing the same, food and pharmaceutical products, which will be described in detail below.
High calcium salt compound
In one aspect of the invention, the invention provides a high calcium salt-based compound. According to the embodiment of the invention, the high calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate, wherein the total content of the calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate is 90-95 mass%, the content of the calcium is 36-38 mass%, the content of the potassium is 22-24 mass%, the content of the magnesium is 1-2 mass%, and the content of the sodium is 7-8 mass%, based on the total mass of the high calcium salt compound.
The high calcium salt compound mainly comprises calcium, potassium, sodium, magnesium, phosphate radical, chloride ion, sulfate radical and carbonate radical, and the purity (content) of the high calcium salt compound is as high as 90-95 mass%. In addition, the composition also contains small amount of other components such as zinc and selenium. Therefore, the high calcium salt compound provided by the embodiment of the invention has high nutritional value. And the safety is high, the product can be used for food or medicine, and the application prospect is wide.
According to the embodiment of the invention, the raw materials for preparing the high-calcium salt compound comprise raw milk, and the ratio of the calcium content in the high-calcium salt compound to the calcium content in the raw milk is 80-85 mass%; the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%; the ratio of the phosphate content in the high calcium salt compound to the phosphate content in the raw milk is 55 to 60 percent by mass; the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65 to 70 percent by mass. Therefore, the extraction rate of calcium, potassium, phosphate radical and chloride ions in the high calcium salt compound is higher.
Method for preparing high calcium salt compound
In another aspect of the invention, the invention provides a method for preparing high calcium salt complexes.
At present, in order to enrich calcium in cow milk, a membrane filtration technology is mainly adopted. However, it has certain limitations, and the complex suspension system for processing milk has the following defects: A. the purity/content of the final concentrate is low; B. different substances need different membrane treatments, and the screening combination of a plurality of membranes is complex to use, so that the loss of nutrient substances is easily caused; C. high cost and difficult maintenance.
For this purpose, the inventor creatively adopts the natural cheese technology, under the action of pre-acidification and rennet, the casein is denatured and precipitated to form coagulum, thereby removing the casein. Then, the components in the discharged whey can be extracted by physical sieve pores and chemical actions such as anion-cation exchange adsorption, macroporous adsorption resin, ammonium salt precipitation, dialysis and the like. However, the treatment of whey in the above manner results in loss of nutrients on the one hand and some adsorbent filling materials on the other hand do not guarantee food safety. Further, the inventor utilizes the characteristic of whey protein isoelectric point aggregation and sedimentation, and precipitates and removes whey protein when the pH value is continuously reduced and the whey protein isoelectric point is reached in the process of stacking and brewing the clot. Lactose is changed into lactic acid in the fermentation process, and is filtered by a nanofiltration membrane (NF membrane for short) to finally obtain natural salt substances with high purity/content, wherein the natural salt substances are rich in calcium, potassium, sodium, magnesium, phosphate radical, chloride ion, sulfate radical and carbonate radical.
According to an embodiment of the present invention, a method of preparing a high calcium salt-based compound includes:
s100, curding the acidified raw milk by using rennin to obtain a curd, and cutting, standing and stirring the curd. Thus, the casein is removed by the natural cheese process to denature the casein for precipitation, forming a clot.
According to the embodiment of the invention, the addition amount of the rennin is 30 to 35g/1000kg based on the mass of the acidified raw milk. Thereby, the casein is sufficiently denatured and precipitated to form a clot. In the traditional process, the addition of the chymosin is about 20g/1000kg probably, the chymosin addition of the application is higher, and most of casein enters the clot, so that the casein content in whey liquid is lower, and the subsequent protein removal process and difficulty are reduced. The action protein of chymosin is kappa-casein, if the addition amount is too high, non-specific enzyme digestion of the chymosin can be caused, some alpha-casein or beta-casein enters the whey liquid, the subsequent protein removal process and difficulty are increased, and the extraction rate of each ion and the purity of the product are low.
The source of chymosin in the present application is not limited, and it can be obtained by a method such as self-preparation, donation, or marketing, and can be selected flexibly according to actual conditions. According to a particular embodiment of the invention, the chymosin is selected from the group consisting of CHY-MAX from the company Kehansen TM Power NB。
According to an embodiment of the invention, the temperature of the curd treatment is 37-39 ℃ and the time is 35-40 minutes. Thereby sufficiently denaturing and precipitating the casein to form a clot.
According to an embodiment of the invention, the size of the cut is 2-3cm 2 . Thereby facilitating the discharge of whey.
S200 when the pH of the coagulum obtained after agitation reaches a first predetermined pH, collecting the whey in order to remove the casein.
According to an embodiment of the invention, the first predetermined pH value is between 6.1 and 6.2. Insoluble calcium on casein micelles at this pH value can free from the micelles into the whey, forming soluble calcium.
S300, fermenting the whey liquid, and removing beta-lactoglobulin in the process; simultaneously, the curd after discharging the whey liquid is piled, the whey liquid with the pH value of whey discharged from the curd reaching a second preset pH value from the beginning of piling is collected, and the whey liquid is mixed with the whey liquid after removing the beta-lactoglobulin.
According to an embodiment of the invention, the second predetermined pH value is between 5.10 and 5.15. When the pH of the whey is discharged to 5.10-5.15, the bound calcium is almost completely converted into free calcium, which is discharged from the whey.
According to an embodiment of the present invention, when the whey is fermented to a pH of 5.3 to 5.4, the whey is filtered and the filtrate is collected to remove β -lactoglobulin in step S300. When the pH value of the whey liquid is 5.3-5.4, the isoelectric point of beta-lactoglobulin (the protein with the highest content in whey protein, the content is 50.77%) is reached, aggregation and sedimentation occur, and the whey liquid is removed by filtration.
According to an embodiment of the invention, the filtration is performed with a 1-2 micron filter membrane. Thereby, the beta-lactoglobulin is separated and removed.
According to an embodiment of the present invention, step S300 further includes: when the pH of the curd-draining whey reaches a second predetermined pH, the curd is washed with water and the washed wash liquor, the collected whey and the beta-lactoglobulin-depleted whey are mixed. As the pH is lowered, the calcium ions bound to the casein gradually dissociate into free calcium, which is excreted as the whey is depleted. When the pH of the whey is discharged to 5.10-5.15, the bound calcium is almost completely converted to free calcium, most of which is discharged with the whey, and a small amount of which remains adhered to the surface of the curd, and the remaining calcium is washed away by mixing water with the curd, thereby increasing the calcium yield.
According to the embodiment of the invention, the mixing temperature of the whey liquid and the water is 25-30 ℃, and the mass ratio of the whey liquid to the water is 1: (1.8-2.3). Thus, the salt-based complex remaining on the surface of the clot can be sufficiently washed, and the yield of calcium can be improved.
S400, fermenting the mixed whey liquid obtained in the step S300, and sequentially removing bovine serum albumin and alpha-lactalbumin to obtain a protein-removed liquid.
According to the embodiment of the present invention, in step S400, when the whey is fermented to 5.1, the whey is filtered, the filtrate is collected so as to remove bovine serum albumin, and then when the filtrate is fermented to 4.4, the filtrate is filtered, and the filtrate is collected so as to obtain the deproteinized liquid. The pH value is lowered with the fermentation of the whey liquid, and when the pH value reaches 5.1, the isoelectric point of BSA (whey protein content of about 6.21%) is reached, and the BSA is removed by using a 1-2 μm filter. Then, the pH value of the whey liquid is continuously reduced, and when the pH value reaches 4.4, the isoelectric point of the alpha-lactalbumin is reached, and a filter membrane of 1-2 microns can be adopted for removing.
S500, filtering, sterilizing and drying the protein removing liquid by using a nanofiltration membrane so as to obtain the high calcium salt compound.
According to the embodiment of the invention, in the step S500, the filtration is performed by adopting a nanofiltration mode, the aperture of the adopted nanofiltration membrane is 1-1.5nm, the permeation quantity is 4-5L/min, and the temperature is 30-40 ℃. Therefore, the lactic acid can be effectively removed, and the loss of other nutrient substances is also avoided. If the temperature is too low, salts are likely to be precipitated. If the amount of the permeation is too large, the product is likely to contain an excessive amount of the undesired substances.
According to an embodiment of the present invention, the sterilization is performed at 75 to 85 ℃ for 24 to 30 seconds. According to another embodiment of the invention, the drying treatment is carried out by a spray drying method, wherein the exhaust air temperature is 75-90 ℃, and the temperature of the sterilized filtrate is 40-60 ℃. Therefore, the aims of sterilization and drying are fulfilled, and the loss of other nutrient substances is avoided.
In another aspect of the present invention, the present invention provides a calcium salt-based compound obtained by the above-described method for preparing a high calcium salt-based compound. The high-calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate radical, chloride ion, sulfate radical and carbonate radical, wherein the total content of the calcium, the potassium, the sodium, the magnesium, the phosphate radical, the chloride ion, the sulfate radical and the carbonate radical is 90-95 mass percent, the content of the calcium is 36-38 mass percent, the content of the potassium is 22-24 mass percent, the content of the magnesium is 1-2 mass percent, and the content of the sodium is 7-8 mass percent. Therefore, the high calcium salt compound provided by the embodiment of the invention has high nutritional value. And the safety is high, the product can be used for food or medicine, and the application prospect is wide.
According to the embodiment of the invention, the raw material for preparing the high calcium salt compound comprises raw milk, and the ratio of the calcium content in the high calcium salt compound to the calcium content in the raw milk is 80-85 mass%; the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%; the ratio of the phosphate radical content in the high calcium salt compound to the phosphate radical content in the raw milk is 55-60 mass%; the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65 to 70 percent by mass. Therefore, the extraction rate of calcium, potassium, phosphate radical and chloride ions in the high calcium salt compound is higher.
Food or medicine
In yet another aspect of the present invention, the present invention provides a food or pharmaceutical product. According to an embodiment of the present invention, the food or pharmaceutical product contains the above-mentioned high calcium salt-based compound. As described above, the high calcium salt-based compound has high nutritional value and high safety, and can be widely used in foods or medicines.
The scheme of the invention will be explained with reference to the following examples. It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to techniques or conditions described in literature in the art or according to the product specification. The reagents or instruments used are conventional products which are commercially available, and are not indicated by manufacturers.
Examples
(1) Extraction of salt and calcium
The casein and fat are separated by using a natural cheese technology. The specific process and parameters are as follows:
(1) filtering raw milk, and centrifugally degreasing:
the raw milk (pH =6.78 + -0.05) which is qualified is taken to be degreased, and the fat is basically separated.
TABLE 1 average content of related minerals in milk
Figure BDA0002199551910000071
(2) Pasteurization and cooling:
the barnacle temperature and time combination was: the temperature of the mixture is controlled at 72 ℃ for 15s,
cooling temperature: 37 ℃ is carried out.
(3) Inoculation and pre-acidification:
pouring raw milk into a cheese tank, adding 10U/ton (Kehansen) of leavening agent at 37 deg.C, and continuously and slowly stirring for 40min by a stirrer with rotation speed of 5 rpm.
(4) Adding rennet curd (casein isolation), and cutting and standing the clot:
adding 30-35g/1000Kg rennin into raw milk, stirring for 1min, standing at 37-39 deg.C for 35-40min, and testing the curd hardness to determine whether to cut. If the coagulum meets the requirement, cutting into 2-3cm pieces 3 And standing for 5min.
(5) Stirring without heating:
the stirrer was started (stirrer speed was set to 10 rpm) and the temperature was maintained at 37 ℃.
(6) When whey pH =6.10-6.20, whey is drained and this serum will be collected and labeled as a-serum (whey tank a-serum):
the drained cheese whey was centrifuged (4000 r/min,5 min) to remove the small amount of casein remaining.
(7) The clot is piled and the rest of the whey drained from the clot is continuously collected into whey tank a-serum:
when pH of whey a-serum =5.40, β -lactoglobulin aggregates settled. Followed by filtration through a sieve (type: mesh number 10000, pore size 1.3 μm).
(8) The clumps are continued to be piled and further the calcium ion containing whey drained from the clumps is collected in whey tank a-serum:
A. when the pH of the clot is =5.10-5.15, calcium ions discharged from the clot are washed by ultrapure water at 25-30 ℃, and the washed water is discharged into a whey tank A-serum, wherein the mass of the clot is as follows: and the mass of the ultrapure water = 1.
B. The small amount of casein remaining in the A-serum was removed by centrifugation (4000 r/min,5 min).
(9) When the pH =5.10 in the serum tank a-serum, a 1.3 micron filtration was performed to remove bovine serum albumin.
(2) Further separation of the salt and calcium components (to isoelectric point of alpha-lactalbumin):
the whey A-serum is continuously fermented until the pH is =4.4, and the aggregation and sedimentation are carried out until the isoelectric point of the alpha-lactalbumin is reached. Filtering with a screen (type: 10000 mesh, 1.3 μm pore diameter), and naming the filtrate as Natural-serum.
(3) Purification of salts and calcium components (NF membrane filtration):
the filtrate Natural-serum is further purified and filtered by an NF membrane, and the parameters are as follows: 4-5L/min, aperture of 1-1.5nm, and temperature of 30-40 deg.C.
(4) The sterilization process comprises the following steps:
sterilization parameters: 75-85 ℃/24-30s.
(5) Powdery preparation of salt and calcium components and packaging and preservation (spray drying)
A. And (3) carrying out spray drying on the Natural-serum treated by the NF membrane to obtain powder.
The spraying parameters are as follows: the exhaust temperature is controlled at 75-90 deg.C, and the concentrated feed liquid temperature is 40-60 deg.C.
B. And discharging the powder, packaging and storing.
TABLE 2 Process parameters
Figure BDA0002199551910000091
Comparative example 1
A high calcium salt-based complex was prepared by the method of example 1, except that the cow milk obtained in step (2) was passed through UF membranes (pore size 0.01 to 0.02 μm) and NF membranes (pore size 1.5 to 2 nm) in the order of permeation amount: 4-5L/min, and the temperature is 30-40 ℃. Then, the operations of steps (4) and (5) are performed.
Comparative example 2
A high calcium salt-based compound was prepared according to the method of example 1, except that in step (6), the pH of the whey-out was 6.30.
Comparative example 3
A high calcium salt-based complex was prepared by the method of example 1 except that the amount of chymosin added was 38g/1000kg.
Example 4
The compositions of the high calcium salt compounds obtained in examples 1 to 3 and comparative examples 1 to 3 were determined by the following specific steps:
1. determination of salt substances: the measurement was carried out according to the method of ash content. The total ash content refers to the weight of the total ash content obtained by burning and oxidizing organic matters in a sample at a certain temperature by mineral matters and inorganic salts or other impurities in food and then weighing the residual white matters.
GB 5009.4-2016 determination of ash content in food safety national standard food, first law determination of total ash content in food.
Wherein: the method comprises the following steps of (1) measuring salt substances in milk, and pretreating a sample: defatting raw milk, and vacuum freeze drying to obtain lyophilized powder.
2. The method for measuring the calcium content comprises the following steps: GB 5009.92-2016 determination of calcium in food safety national standard food, first method flame atomic absorption spectrometry.
3. The method for measuring the potassium content comprises the following steps: GB 5009.91-2017 determination of potassium and sodium in national standard food for food safety, first method flame atomic absorption spectrometry.
4. The method for measuring the content of phosphate radical comprises the following steps: GB 5009.256-2016 determination of various phosphates in food safety national standard food.
5. The determination method of the chloride content comprises the following steps: GB 5009.44-2016 determination of chloride in food safety national standard food.
As shown in table 3, it can be seen that the high calcium salt-based compound obtained by the method of the present invention has high purity and is rich in calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate, and carbonate.
In the comparative example 1, the membrane filtration mode is adopted to remove the protein in the raw milk, the removal effect is poor, the impurity protein in the product is more, the product purity is lower, the extraction efficiency of calcium, potassium, phosphate radical and chloride ion is influenced, and the ion loss is serious.
In comparative example 2, whey drainage had started too early, resulting in incomplete casein precipitation, higher impurity content in the product, lower purity, and lower extraction of calcium, potassium, phosphate and chloride ions.
In comparative example 3, the addition of rennin was too high, which easily caused non-specific enzyme digestion of rennin, resulting in some α -casein or β -casein entering the whey, increasing the subsequent protein removal process and difficulty, and reduced extraction rate of each ion and purity of the product.
TABLE 3 high calcium salt-based Compound composition
Figure BDA0002199551910000101
Figure BDA0002199551910000111
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.

Claims (9)

1. A method for preparing a high calcium salt-based compound, comprising:
(1) Curdling acidified raw milk by using rennin so as to obtain a clot, cutting, standing and stirring the clot;
(2) Collecting the whey when the pH of the coagulum obtained after the stirring reaches a first predetermined pH, in order to remove casein;
(3) Fermenting the whey, during which beta-lactoglobulin is removed;
simultaneously, piling the curd after discharging the whey liquid, collecting the whey liquid with the pH value of whey discharged from the curd reaching a second preset pH value from the beginning of piling, and mixing the whey liquid with the whey liquid after removing the beta-lactoglobulin;
(4) Fermenting the mixed whey liquid obtained in the step (3), and sequentially removing bovine serum albumin and alpha-lactalbumin to obtain a protein removing liquid;
(5) Filtering, sterilizing and drying the protein removing liquid by using a nanofiltration membrane so as to obtain the high calcium salt compound,
wherein the first predetermined pH value is 6.1-6.2, and the second predetermined pH value is 5.10-5.15.
2. The method of claim 1, wherein the raw material for preparing the high calcium salt-based compound comprises raw milk,
the ratio of the calcium content in the high calcium salt compound to the calcium content in the raw milk is 80-85 mass%;
the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%;
the ratio of the phosphate radical content in the high calcium salt compound to the phosphate radical content in raw cow milk is 55-60 mass%;
the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65-70% by mass.
3. The method according to claim 1, wherein in the step (3), when the whey is fermented to a pH of 5.3 to 5.4, the whey is filtered, and the filtrate is collected to remove β -lactoglobulin;
optionally, the filtration is performed using a 1-2 micron filter membrane.
4. The method of claim 1, wherein step (3) further comprises:
washing the curd with water when the pH of the curd-draining whey reaches a second predetermined pH and said mixing of the washed wash liquor, the collected whey and said beta-lactoglobulin-depleted whey;
optionally, the mixing temperature of the whey liquid and water is 25-30 ℃, and the mass ratio of the whey liquid to the water is 1: (1.8-2.3).
5. The method according to claim 1, wherein in the step (4), when the whey is fermented to 5.1, the whey is filtered, the filtrate is collected to remove bovine serum albumin, and then when the filtrate is fermented to 4.4, the filtrate is filtered, the filtrate is collected to obtain the protein-removed liquid;
optionally, the filtration is performed using a 1-2 micron filter membrane.
6. The method according to claim 1, wherein the amount of rennet added is 30-35g/1000kg, based on the mass of the acidified raw milk;
optionally, the temperature of the curd treatment is 37-39 ℃, and the time is 35-40 minutes;
optionally, the size of the cut of the clot is 2-3cm 2
7. The method according to claim 1, wherein in the step (5), the filtration is performed by nanofiltration, and the nanofiltration membrane has a pore diameter of 1 to 1.5nm, a permeation amount of 4 to 5L/min, and a temperature of 30 to 40 ℃;
optionally, the sterilization is carried out at 75-85 ℃ for 24-30 seconds;
optionally, the drying treatment is carried out by adopting a spray drying mode, wherein the air exhaust temperature is 75-90 ℃, and the temperature of the sterilized filtrate is 40-60 ℃.
8. A high calcium salt-based compound obtained by the method for producing a high calcium salt-based compound according to any one of claims 1 to 7;
optionally, the high calcium salt compound contains calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate,
wherein the total content of calcium, potassium, sodium, magnesium, phosphate, chloride, sulfate and carbonate is 90-95 mass% based on the total mass of the high calcium salt-based compound;
optionally, the ratio of the calcium content in the high calcium salt compound to the calcium content in raw milk is 80-85 mass%;
the ratio of the potassium content in the high calcium salt compound to the potassium content in the raw milk is 55-60 mass%;
the ratio of the phosphate radical content in the high calcium salt compound to the phosphate radical content in raw cow milk is 55-60 mass%;
the ratio of the content of chloride ions in the high calcium salt compound to the content of chloride ions in raw milk is 65-70 mass%.
9. A food or pharmaceutical product comprising the high calcium salt-based compound according to claim 8.
CN201910860364.XA 2019-09-11 2019-09-11 High calcium salt compound and preparation method thereof Active CN110623243B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910860364.XA CN110623243B (en) 2019-09-11 2019-09-11 High calcium salt compound and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910860364.XA CN110623243B (en) 2019-09-11 2019-09-11 High calcium salt compound and preparation method thereof

Publications (2)

Publication Number Publication Date
CN110623243A CN110623243A (en) 2019-12-31
CN110623243B true CN110623243B (en) 2023-03-31

Family

ID=68972138

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910860364.XA Active CN110623243B (en) 2019-09-11 2019-09-11 High calcium salt compound and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110623243B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115644451A (en) * 2022-09-30 2023-01-31 内蒙古伊利实业集团股份有限公司 Mineral composition and product and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1243887A (en) * 1984-07-03 1988-11-01 Shuryo Nakai REDUCING .beta.-LACTOGLOBULIN CONTENT IN WHEY PROTEIN CONCENTRATES FOR INFANT FORMULA USE
CN103910779A (en) * 2006-05-31 2014-07-09 Lfb生物科技公司 Method for the extraction of one or several proteins in milk
CN106417888A (en) * 2016-09-27 2017-02-22 江南大学 Method for separating cow milk beta-casein and whey protein at low temperature through microfiltration to simulate composition of human lactoprotein
EP3375788A1 (en) * 2017-03-13 2018-09-19 ETH Zurich Composite materials comprising amyloid fibrils and nanoparticulate nutritional minerals
CN109561724A (en) * 2016-06-21 2019-04-02 阿拉食品公司 The product for producing the method for the improvement nutrition product containing lactoprotein and lactose class and being obtained by this method

Family Cites Families (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FI96266C (en) * 1994-02-23 1996-06-10 Jouko Savolainen Method for isolating whey proteins
US5986063A (en) * 1998-07-31 1999-11-16 Wisconsin Alumni Research Foundation Isolating β-lactoglobulin and α-lactalbumin by eluting from a cation exchanger without sodium chloride
EP1234507A1 (en) * 2001-02-26 2002-08-28 Wageningen Centre for Food Sciences Process for isolating beta-lactoglobulin from milk or milk fractions
US20060062873A1 (en) * 2004-09-13 2006-03-23 Jeng-Jung Yee Curds for processed and imitation cheese, cheese products produced therefrom, novel intermediate products and methods of making same
BR112012029291A2 (en) * 2010-06-16 2015-09-08 Tropicana Prod Inc encapsulated salts and use in high acid beverages
CN102302116B (en) * 2011-06-10 2013-11-27 营养屋(成都)生物医药有限公司 Calcium supplementing and calcium locking health care food and preparation method thereof
CN104777257B (en) * 2015-04-30 2017-01-18 澳优乳业(中国)有限公司 Fast separation and detection method for whey protein components in dairy product
CN106417613A (en) * 2015-08-07 2017-02-22 内蒙古伊利实业集团股份有限公司 Alpha-lactalbumin-rich whey powder and preparation method thereof
US20170306504A1 (en) * 2016-04-26 2017-10-26 Ecolab Usa Inc. Corrosion inhibitor compositions and methods of using same
CN106418072B (en) * 2016-08-25 2020-09-15 方雅悯 Production process of bioactive water
CN107801785B (en) * 2017-10-26 2021-01-15 光明乳业股份有限公司 Red line semi-hard cheese and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CA1243887A (en) * 1984-07-03 1988-11-01 Shuryo Nakai REDUCING .beta.-LACTOGLOBULIN CONTENT IN WHEY PROTEIN CONCENTRATES FOR INFANT FORMULA USE
CN103910779A (en) * 2006-05-31 2014-07-09 Lfb生物科技公司 Method for the extraction of one or several proteins in milk
CN109561724A (en) * 2016-06-21 2019-04-02 阿拉食品公司 The product for producing the method for the improvement nutrition product containing lactoprotein and lactose class and being obtained by this method
CN106417888A (en) * 2016-09-27 2017-02-22 江南大学 Method for separating cow milk beta-casein and whey protein at low temperature through microfiltration to simulate composition of human lactoprotein
EP3375788A1 (en) * 2017-03-13 2018-09-19 ETH Zurich Composite materials comprising amyloid fibrils and nanoparticulate nutritional minerals

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
Emma L.Synergistic stabilization of heat-treated emulsions containing mixtures of milk proteins.《International Dairy Journal》.2007,第第17卷卷第95-103页. *
王银娟 ; 王晓君 ; 田芬 ; 孙勇 ; 欧凯 ; 吴伟都 ; 高兴华 ; .乳清浓缩蛋白改善脱脂发酵乳饮料的稳定性.乳业科学与技术.2014,(06),第13-17页. *

Also Published As

Publication number Publication date
CN110623243A (en) 2019-12-31

Similar Documents

Publication Publication Date Title
CN1899054A (en) Method for making sugar-removing milk
EP1133238A1 (en) Method for preparing a protein composition and an infant formula containing same
CN110367339B (en) Kappa-casein-rich whey powder and preparation method and application thereof
CN103501621A (en) Cheese and preparing the same
JPH02503425A (en) whey protein fraction
WO2013131494A1 (en) Method for producing low-ash poultry plasma protein powder by utilizing poultry blood
AU631035B2 (en) Low fat cheese by evaporation of retentate
CN108606063A (en) A kind of Greece's flavored fermented milk and preparation method thereof made using MPC liquid
CN109788771A (en) The method for producing infant formula product and dairy products
CN110623243B (en) High calcium salt compound and preparation method thereof
CN100423646C (en) Process for reclaiming lactoalbumin from waste liquid of casein industrial production
WO2002034062A1 (en) Method for obtaining products enriched in phospho- and sphingolipids
AU653666B2 (en) Method for manufacture of pre-cheese and natural cheese
JP4876137B2 (en) Method for producing calcium-containing milk composition
EP0326617A1 (en) Process for the production of low-phosphorus milk
CN1312295A (en) Flocculation charification-ultrafiltration concentration process of producing composite immunoreactive protein
US20030078392A1 (en) Milk and cheese modification process, including methods of extracting beta-lactoglobulin and caseins from milk and milk products, and novel products thereby produced
CN105519666B (en) Liquid diary product and preparation method thereof
CN209825088U (en) Utilize dairy products deep-processing to prepare casein's device
JPS60232052A (en) Method of making milk mineral concentrate
Varnam et al. Dairy protein products
CN112913962A (en) Preparation method of protein powder
CN110547467A (en) casein-based probiotic delivery gel and preparation method and application thereof
CN116636562A (en) Separation preparation method of milk fat globule membrane
RU2298940C2 (en) Method for production of protein hydrolyzate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant