CN108567045A - A kind of method and system being classified production casein using Qula as raw material gradient pH value - Google Patents
A kind of method and system being classified production casein using Qula as raw material gradient pH value Download PDFInfo
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- CN108567045A CN108567045A CN201710155093.9A CN201710155093A CN108567045A CN 108567045 A CN108567045 A CN 108567045A CN 201710155093 A CN201710155093 A CN 201710155093A CN 108567045 A CN108567045 A CN 108567045A
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- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 title claims abstract description 189
- 235000021240 caseins Nutrition 0.000 title claims abstract description 188
- 239000005018 casein Substances 0.000 title claims abstract description 187
- 238000000034 method Methods 0.000 title claims abstract description 50
- 239000002994 raw material Substances 0.000 title claims description 16
- 238000004519 manufacturing process Methods 0.000 title description 8
- 239000006228 supernatant Substances 0.000 claims abstract description 52
- 238000001556 precipitation Methods 0.000 claims abstract description 40
- 238000011282 treatment Methods 0.000 claims abstract description 32
- 239000007790 solid phase Substances 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims description 88
- 230000001105 regulatory effect Effects 0.000 claims description 54
- 239000002253 acid Substances 0.000 claims description 26
- 238000000926 separation method Methods 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 19
- 239000013049 sediment Substances 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 235000013351 cheese Nutrition 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 8
- 238000012806 monitoring device Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 11
- 102000011632 Caseins Human genes 0.000 description 170
- 108010076119 Caseins Proteins 0.000 description 170
- 230000001804 emulsifying effect Effects 0.000 description 10
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 7
- 239000000839 emulsion Substances 0.000 description 7
- 239000008101 lactose Substances 0.000 description 7
- 239000002932 luster Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 102000004316 Oxidoreductases Human genes 0.000 description 4
- 108090000854 Oxidoreductases Proteins 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 235000018102 proteins Nutrition 0.000 description 4
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
- 238000004945 emulsification Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 235000020255 yak milk Nutrition 0.000 description 3
- 241000219307 Atriplex rosea Species 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 108060008539 Transglutaminase Proteins 0.000 description 1
- 235000020244 animal milk Nutrition 0.000 description 1
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229940021722 caseins Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 235000020247 cow milk Nutrition 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 235000013365 dairy product Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229960002442 glucosamine Drugs 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000006166 lysate Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 102000003601 transglutaminase Human genes 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/20—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from milk, e.g. casein; from whey
- A23J1/202—Casein or caseinates
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Peptides Or Proteins (AREA)
- Dairy Products (AREA)
Abstract
The present invention proposes a kind of method and system preparing casein.The method includes：(1) pH value of Qula solution is adjusted to the first predetermined pH value；(2) obtained mixture in step (1) is subjected to the first solid phase separating treatment, to obtain the first supernatant and the first precipitation；(3) pH value of first supernatant is adjusted to 4.4~4.6；And obtained mixture in step (3) is carried out second solid phase separating treatment by (4), to obtain the second precipitation, second precipitation constitutes first object casein.Different stage (dissolving pH value) and the higher casein of purity can be respectively obtained using the method and system for preparing casein of the present invention.In addition, the method and system of the present invention is easy to operate, it is suitable for large-scale production.
Description
Technical field
The present invention relates to field of food.In particular it relates to prepare the method and system of casein.
Background technology
Yak is the peculiar domestic animal on Qinghai-Tibet Platean, and China is the main production country of yak, accounts for the world total (14,000,000)
92%, it is distributed in the provinces and regions such as Xinjiang, Tibet, Yunnan, Sichuan, Qinghai, Gansu.Yak to High aititude, low pressure, very cold with
And the ecological environment of alpine steppe etc. has indomitable resistivity, is the main economic source of the pastoral area people.Yak milk nutrition at
Divide and be higher than common cow's milk, there is higher nutritive value, be that other ox kinds are incomparable " pure natural concentrated milk ".But due to it
Special existence geographical environment, local herdsman by most yak milk degreasing, boil, spontaneous fermentation air-dry coarse cheese-is made
Qula so that yak milk is able to long-term storage, and deep processing and utilization is carried out convenient for collecting.
Casein, also known as casein are the phosphor proteins in animal milk.Qula is rich in casein, is that China's production is dry
The primary raw material of casein.
However, the mode for obtaining casein at present still has much room for improvement.
Invention content
The present invention is directed to solve at least one the technical problems existing in the prior art at least to a certain extent.For this purpose,
The present invention proposes a kind of method and system preparing casein.It can using the method and system for preparing casein of the present invention
Respectively obtain different stage (dissolving pH value) and the higher casein of purity.In addition, the method and system of the present invention is easy to operate,
Suitable for large-scale production.
It should be noted that the present invention is the following discovery based on inventor and completes：
Currently, main be adjusted to target ph using aqueous slkali by Qula solution, it is the target ph to dissolve pH value
Target casein can dissolve, and remaining dissolving pH value casein cannot dissolve, through be separated by solid-liquid separation can obtain containing mesh
Mark the dissolving feed liquid of casein；Then dissolving feed liquid is carried out pH value to adjust until reach casein isoelectric point, precipitation and separation, with
Just target casein is obtained.But generally use disposably adjusts pH value in the prior art, i.e., a target ph is only arranged.
Inventor has found that pH is the key factor for influencing casein structure and function property, and pH value, lysate are adjusted according to disposable
The substances such as middle lactose, protein are more, the reactions such as Yi Fashengmei ladds, amino-acid oxidase under the conditions of higher pH, make gained
Casein color and luster, emulsibility are poor, seriously affect its utility value.
In view of this, inventor has found by many experiments, Qula material is subjected to gradient pH value adjusting using aqueous slkali,
It is first adjusted to low ph value, and obtained feed liquid is separated by solid-liquid separation, supernatant and precipitation is obtained, adjusts the pH of supernatant
Value obtains the casein of low dissolving pH value to isoelectric point；Then precipitation is adjusted to the pH value higher than aforementioned low ph value, repeated
Aforesaid operations so recycle successively, and the pH value that each round is adjusted is above preceding primary at least 1, to obtain different stage in batches
Casein.In addition, the water-soluble substances such as lactose, protein in Qula can with being separated by solid-liquid separation into supernatant, i.e., with
A part of water-soluble substances can be discharged in re-adjustments pH value every time so that water-soluble substances content reduces in precipitation, avoids
The reactions such as Mei Lade, amino-acid oxidase occur.The method and system according to the ... of the embodiment of the present invention for preparing casein can as a result,
Respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality.In addition, the method and system of the present invention
It is easy to operate, it is suitable for large-scale production.
For this purpose, in one aspect of the invention, the present invention proposes a kind of method preparing casein.It is according to the present invention
Embodiment, the method includes：(1) pH value of Qula solution is adjusted to the first predetermined pH value；(2) by gained in step (1)
The mixture arrived carries out the first solid phase separating treatment, to obtain the first supernatant and the first precipitation；(3) by first supernatant
The pH value of liquid is adjusted to 4.4~4.6；And obtained mixture in step (3) is carried out second solid phase separating treatment by (4),
To obtain the second precipitation, second precipitation constitutes first object casein.According to the ... of the embodiment of the present invention prepare is done as a result,
The method of casein can obtain the casein of isolated different stage, and easy to operate, be suitable for large-scale production.
According to an embodiment of the invention, the above-mentioned method for preparing casein can also further have following supplementary technology special
Sign：
According to an embodiment of the invention, the described first predetermined pH value is more than 6.0, and the Qula solution is by repeating
What at least one wheel the following steps obtained：(i) pH value of the first raw material containing casein is adjusted to the second predetermined pH value, institute
It states the second predetermined pH value and is less than the described first predetermined pH value, the start numbers of the second predetermined pH value are consolidating no more than 6.0
Fixed number value；(ii) obtained mixture in step (i) is subjected to third solid phase separating treatment, so as to obtain third supernatant and
Third precipitates, wherein when the difference of the described second predetermined pH value and the described first predetermined pH value is no more than 1, the third precipitation
The Qula solution is constituted, when the difference of the described second predetermined pH value and the described first predetermined pH value is more than 1, the third is sunk
Shallow lake is back to step (i) and repeats step (i) and the wheels of (ii) at least one, wherein second predetermined pH of each round increases
1, until the difference of the described second predetermined pH value and the described first predetermined pH value is no more than 1.
Inventor has found, by using gradient pH value from low to high to obtain the casein of different stage, and each rank
Casein purity it is higher, less adulterate the casein of other ranks.In addition, the lactose in Qula can be with separation of solid and liquid
Into supernatant, i.e., with re-adjustments pH value, a part of lactose can be discharged every time so that lactose content drops in precipitation
It is low, it avoids that the reactions such as Mei Lade, amino-acid oxidase occur.The method energy according to the ... of the embodiment of the present invention for preparing casein as a result,
Enough respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality.Moreover, it is easy to operate, it is suitable for rule
Modelling produces.
According to an embodiment of the invention, step (ii) further comprises：The pH value of the third supernatant is adjusted to 4.4
~4.6, and detached by solid phase to obtain the second target casein.Inventor has found, by by the pH value of third supernatant
It is adjusted to the isoelectric point of casein so that casein precipitate, to obtain target product.It is according to the ... of the embodiment of the present invention as a result,
The method for preparing casein can respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality.And
And it is easy to operate, it is suitable for large-scale production.
According to an embodiment of the invention, step (1) and (i) in, using aqueous slkali carry out pH value adjusting.It is according to the present invention
Preferred embodiment, a concentration of 4mol/L of the aqueous slkali.It is predetermined to obtain having thereby, it is possible to effectively adjust pH value
Dissolve the target casein of pH value.
According to an embodiment of the invention, in step (3) and (ii), pH value adjusting is carried out using acid solution.According to the present invention
Preferred embodiment, a concentration of 1.0mol/L of the acid solution.Thereby, it is possible to effectively adjust pH value to electricity such as caseins
Point.
According to an embodiment of the invention, the first solid phase separating treatment, second solid phase separating treatment and third solid phase point
It is to centrifuge 20min under the rotating speed of 4500g from processing.Thereby, it is possible to effectively detach supernatant and precipitation.
In another aspect of this invention, the present invention proposes another method for preparing casein.Reality according to the present invention
Example is applied, the method includes：(a) Qula raw material, solid-liquid ratio 1 are added in the dissolving cylinder equipped with distilled water:20 (V/V), room temperature
Lower immersion 10min, obtains the first feed liquid；(b) when the sodium hydroxide solution of 4mol/L being used to adjust first material liquid pH value to 6.0
Stop plus alkali, stir 1h, the pH value of the first feed liquid described in constantly regulate is to 6.0 in course of dissolution；It (c) will be obtained by step (b)
Mixed liquor centrifuge 20min under the rotating speed of 4500g, with filtered through gauze remove fat, obtain supernatant and sediment；(d) it uses
Supernatant pH value is adjusted to 4.4~4.6 by 1.0mol/L HCl solutions, and by obtained mixed liquor under the rotating speed of 4500g
Centrifuge 5min；(e) distilled water and the obtained precipitation of acetone washing step (d) are used respectively twice, to obtain pH6.0 cheese
Element；(f) sediment is back to step (a) and repeats the wheels of step (a)~(e) six, wherein the first material in step (b)
The pH value of liquid is followed successively by 7.0,8.0,9.0,10.0,11.0 and 12.0, to respectively obtain pH7.0 casein, pH8.0 cheese
Element, pH9.0 casein, pH10.0 casein, pH11.0 casein, pH12.0 casein；And (g) by the cheese of acquisition
Element carries out vacuum freeze drying, and temperature is -50 DEG C, and pressure is 10~50Pa, time 48h.As a result, according to embodiments of the present invention
The method for preparing casein can respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality,
And it is easy to operate, it is suitable for large-scale production.
In still another aspect of the invention, the present invention propose it is a kind of implement it is described above prepare casein method be
System.According to an embodiment of the invention, the system comprises：First pH value regulating device, the first pH value regulating device are suitable for
Adjust the pH value of Qula solution；Equipment for separating liquid from solid, the equipment for separating liquid from solid are connected with the first pH value regulating device, fit
In carrying out solid-liquid separation treatment to obtained feed liquid after adjusting pH value, to obtain the first supernatant and the first sediment；The
Two pH value regulating devices, the second pH value regulating device are connected with the equipment for separating liquid from solid, are suitable for adjusting the supernatant
PH value, to obtain the second sediment；First circulation pipeline, the first circulation pipeline are adjusted with first pH value respectively
Device is connected with equipment for separating liquid from solid, suitable for making first sediment be back to the first pH value regulating device；Second follows
Endless tube road, the second circulation pipeline are connected with the equipment for separating liquid from solid and the second pH value regulating device respectively, are suitable for separation
Second sediment, to obtain casein.It as a result, can using the system according to the ... of the embodiment of the present invention for preparing casein
Respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality.In addition, the method and system of the present invention
It is easy to operate, it is suitable for large-scale production.
According to an embodiment of the invention, the system further comprises：Aqueous slkali storage device, the aqueous slkali deposit dress
It sets and is connected with the first pH value regulating device, aqueous slkali is housed in the aqueous slkali storage device, be suitable for adjusting described first
The pH value of feed liquid in pH value regulating device；And acid solution storage device, the acid solution storage device and second pH value
Regulating device is connected, and acid solution is housed in the acid solution storage device, is suitable for adjusting the pH value of first supernatant.By
This, different stage (dissolving pH value), purity can be respectively obtained using the system according to the ... of the embodiment of the present invention for preparing casein
The preferable casein of higher and quality, and it is easy to operate, it is suitable for large-scale production.
According to an embodiment of the invention, the system further comprises：PH value control device, the aqueous slkali storage device
It is connected with the first pH value regulating device by the pH value control device, the pH value control device is suitable for controlling described the
The pH value of feed liquid in one pH value regulating device, it is preferable that in control the first pH value regulating device the pH value of feed liquid be 6.0,
7.0,8.0,9.0,10.0,11.0 or 12.0；PH value monitoring device, the pH value detection device control with the pH value fill respectively
It sets and is connected with the first pH value regulating device, the pH value monitoring device is suitable for monitoring feed liquid in the first pH value regulating device
PH value.As a result, different stage (dissolving pH can be respectively obtained using the system according to the ... of the embodiment of the present invention for preparing casein
Value), purity is higher and the preferable casein of quality, and easy to operate, be suitable for large-scale production.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obviously, or practice through the invention is recognized.
Description of the drawings
The above-mentioned and/or additional aspect and advantage of the present invention will become in the description from combination following accompanying drawings to embodiment
Obviously and it is readily appreciated that, wherein：
Fig. 1 shows the flow diagram according to an embodiment of the invention for preparing casein method；
Fig. 2 shows the flow diagram in accordance with another embodiment of the present invention for preparing casein method；
Fig. 3 shows the structural schematic diagram according to an embodiment of the invention for preparing casein system；
Fig. 4 shows the structural schematic diagram in accordance with another embodiment of the present invention for preparing casein system；
Fig. 5 shows the structural schematic diagram for preparing casein system according to another embodiment of the invention；
Fig. 6 shows emulsifying activity analysis chart according to an embodiment of the invention；And
Fig. 7 shows emulsion stability analysis chart according to an embodiment of the invention.
Specific implementation mode
The embodiment of the present invention is described below in detail.The embodiments described below is exemplary, and is only used for explaining this hair
It is bright, and be not considered as limiting the invention.
It should be noted that term " first ", " second " are used for description purposes only, it is not understood to indicate or imply phase
To importance or implicitly indicate the quantity of indicated technical characteristic.Define " first " as a result, the feature of " second " can be with
Express or implicitly include one or more this feature.Further, in the description of the present invention, unless otherwise saying
Bright, the meaning of " plurality " is two or more.
The present invention proposes the method and system for preparing casein, will be described in greater detail respectively below.
The method for preparing casein
In one aspect of the invention, the present invention proposes a kind of method preparing casein.Implementation according to the present invention
Example, referring to Fig. 1, this method includes：
S100 adjusts pH value to the first predetermined pH value
In this step, the pH value of Qula solution is adjusted to the first predetermined pH value.Thereby, it is possible to dissolve pH value not
Casein more than the first predetermined pH value dissolves, and the casein of remaining dissolving pH value (being more than the first predetermined pH value) is not molten
Solution.As a result, so that later separation goes out to dissolve the casein that pH value is no more than the first predetermined pH value.
According to an embodiment of the invention, pH value adjusting is carried out using aqueous slkali.According to a preferred embodiment of the invention, alkali soluble
A concentration of 4mol/L of liquid.Inventor obtains above-mentioned more excellent aqueous slkali pH value by many experiments.If concentration is too low, aqueous slkali
Dosage is excessive, and increases workload for subsequent solid-liquid separation treatment.
It should be noted that it can be pre-processed using conventional method according to the property or state of Qula solution,
To carry out subsequent operation.According to a particular embodiment of the invention, solid-state Qula solution is added to the water immersion 10 minutes, feed liquid
Than being 1:20 (V/V) so that it is swollen, and can fully be dissolved convenient for adjusting target casein after pH value.
S200 the first solid phase separating treatments
In this step, obtained mixture in step S100 is subjected to the first solid phase separating treatment, to obtain the
One supernatant and the first precipitation.As a result, containing the casein that dissolving pH value is the first predetermined pH value in the first supernatant, first is heavy
It is more than the casein of the first predetermined pH value in shallow lake containing dissolving pH value, realizes the purpose of separation.
According to an embodiment of the invention, the first solid phase separating treatment is to centrifuge 20min under the rotating speed of 4500g.As a result, can
It enough effectively will precipitation and separation of the supernatant.
S300 adjusts pH value to 4.4~4.6
In this step, the pH value of first supernatant is adjusted to 4.4~4.6.Inventor has found, by the first supernatant
The pH value of liquid is adjusted to 4.4~4.6, to reach the isoelectric point of casein, makes its precipitation, to further isolated purer
Casein.
According to an embodiment of the invention, in step S300, pH value adjusting is carried out using acid solution.It is according to the present invention preferred
Embodiment, a concentration of 1.0mol/L of acid solution.Inventor obtains above-mentioned more excellent acid solution pH value by many experiments.If concentration
Too low, the dosage of acid solution is excessive, and increases workload for subsequent solid-liquid separation treatment.
S400 second solid phase separating treatments
In this step, obtained mixture in step S300 is subjected to second solid phase separating treatment, to obtain the
Two precipitations, the second precipitation constitute first object casein.It is the first predetermined pH value thereby, it is possible to obtain purer dissolving pH value
Casein.
According to an embodiment of the invention, the first solid phase separating treatment is to centrifuge 20min under the rotating speed of 4500g.As a result, can
It enough effectively will precipitation and separation of the supernatant.The casein for being 6.0 thereby, it is possible to obtain purer dissolving pH value.
It should be noted that according to an embodiment of the invention, acid solution can be added while stirring in the process by adjusting pH value
Or aqueous slkali fully reacts so that acid solution or aqueous slkali are uniformly mixed with feed liquid.
In addition it is also necessary to explanation, the first object casein of acquisition can also be post-processed, pure to obtain
Casein.Considered critical is not made for the mode of post-processing, can be selected according to actual needs.Tool according to the present invention
Obtained first object casein is washed twice with distilled water and acetone, then is dried by body embodiment respectively.
Furthermore, it should be noted that those skilled in the art can select the first predetermined pH value according to actual needs.Specifically
Ground, if it is 6.0 to select the first predetermined pH value, then passing through step S100 to S400, it is 6.0 that can directly obtain dissolving pH value
Casein can further use following operation if the first predetermined pH value of selection is more than 6.0, not at the same level to respectively obtain
Other casein：
According to an embodiment of the invention, referring to Fig. 2, the first predetermined pH value is more than 6.0, and Qula solution is by repeating
What at least one wheel the following steps obtained：
S110 adjusts pH value to the second predetermined pH value
In this step, the pH value of the first raw material containing casein is adjusted to the second predetermined pH value, second is predetermined
PH value is less than the first predetermined pH value, and the start numbers of the second predetermined pH value are the fixed numbers no more than 6.0.PH is dissolved as a result,
Value, which is the casein of the second predetermined pH value, to be dissolved, and the casein of remaining dissolving pH value (being more than the second predetermined pH value) is not
Dissolving.As a result, so that later separation goes out to dissolve the casein that pH value is the second predetermined pH value.
According to an embodiment of the invention, pH value adjusting is carried out using aqueous slkali.According to a preferred embodiment of the invention, alkali soluble
A concentration of 4mol/L of liquid.Inventor obtains above-mentioned more excellent aqueous slkali pH value by many experiments.If concentration is too low, aqueous slkali
Dosage is excessive, and increases workload for subsequent solid-liquid separation treatment.
It should be noted that can be according to the property or state of the first raw material containing casein, using conventional method
It is pre-processed, to carry out subsequent operation.According to a particular embodiment of the invention, solid-state is contained the first of casein
Raw material are added to the water immersion 10 minutes, solid-liquid ratio 1:20 (V/V) so that it is swollen, convenient for adjusting target after pH value
Casein can fully dissolve.
S120 third solid phase separating treatments
In this step, obtained mixture in step S110 is subjected to third solid phase separating treatment, to obtain the
Three supernatants and third precipitation.
According to an embodiment of the invention, third solid phase separating treatment is to centrifuge 20min under the rotating speed of 4500g.As a result, can
It enough effectively will precipitation and separation of the supernatant.
According to an embodiment of the invention, according to the difference of the second predetermined pH value and the first predetermined pH value, using two kinds of differences
Mode handles third precipitation, specifically, 1) when the difference of the second predetermined pH value and the first predetermined pH value is no more than 1, third precipitation
Qula solution is constituted, the operation of step S100 to S400 is carried out；2) when the difference of the second predetermined pH value and the first predetermined pH value is more than 1
When, carry out following operation：
S130 return to step S110 repeats the wheels of step S110 and S120 at least one
In this step, third precipitation is shown as the first raw material containing casein, be back to step S110 repeat into
Row step S110 and S120 at least one takes turns, wherein the second predetermined pH of each round increases by 1, until the second predetermined pH value and first
The difference of predetermined pH value is no more than 1.As a result, by improving pH value step by step, to obtain the casein of different stage respectively.
It should be noted that those skilled in the art can choose whether to need to obtain third supernatant by actual conditions
In casein.If desired obtain the casein in third supernatant, then the pH value of third supernatant can be adjusted to 4.4~
4.6, and detached by solid phase to obtain the second target casein.Inventor has found, the pH value of third supernatant is adjusted to
4.4~4.6, to reach the isoelectric point of casein, make its precipitation, to further isolated purer casein.
According to a particular embodiment of the invention, in step S120, pH value adjusting is carried out using acid solution.It is according to the present invention
Preferred embodiment, a concentration of 1.0mol/L of acid solution.Inventor obtains above-mentioned more excellent acid solution pH value by many experiments.If
Concentration is too low, and the dosage of acid solution is excessive, and increases workload for subsequent solid-liquid separation treatment.
In addition, the present invention proposes another method for preparing casein.According to an embodiment of the invention, this method packet
It includes：(a) Qula raw material, solid-liquid ratio 1 are added in the dissolving cylinder equipped with distilled water:20 (V/V), impregnate 10min, obtain at room temperature
First feed liquid；(b) it uses the sodium hydroxide solution of 4mol/L to adjust first material liquid pH value to stopping plus alkali when 6.0, stirs 1h,
The pH value of the first feed liquid described in constantly regulate is to 6.0 in course of dissolution；(c) by the obtained mixed liquor of step (b) 4500g's
20min is centrifuged under rotating speed, fat is removed with filtered through gauze, obtains supernatant and sediment；(d) use 1.0mol/L HCl solutions will
Supernatant pH value is adjusted to 4.4~4.6, and obtained mixed liquor is centrifuged 5min under the rotating speed of 4500g；(e) it uses respectively
Distilled water and acetone washing step (d) it is obtained precipitation twice, to obtain pH6.0 casein；(f) sediment is shown
Make Qula raw material, is back to step (a) and repeats the wheels of step (a)~(e) six, wherein the pH value of the first feed liquid in step (b)
7.0,8.0,9.0,10.0,11.0 and 12.0 are followed successively by, it is dry to respectively obtain pH7.0 casein, pH8.0 casein, pH9.0
Casein, pH10.0 casein, pH11.0 casein, pH12.0 casein；And the casein of acquisition (g) is subjected to vacuum
Freeze-drying, temperature are -50 DEG C, and pressure is 10~50Pa, time 48h.It is according to the ... of the embodiment of the present invention as a result, to prepare cheese
The method of element can respectively obtain that different stage (dissolving pH value), purity is higher and the preferable casein of quality.Moreover, operation letter
Just, it is suitable for large-scale production.
It should be noted that for the convenience of description, by dissolve pH value be 7.0 casein be referred to as " pH7.0 casein ",
Similarly, " pH8.0 casein, pH9.0 casein, pH10.0 casein, pH11.0 casein, pH12.0 casein " respectively refers to
Dissolving pH value is respectively 8.0,9.0,10.0,11.0 and 12.0 casein.
The system for preparing casein
In another aspect of this invention, the present invention propose it is a kind of implement it is described above prepare casein method be
System.According to an embodiment of the invention, referring to Fig. 3, which includes：First pH value regulating device 100, equipment for separating liquid from solid 200,
Second pH value regulating device 300, first circulation pipeline 400 and second circulation pipeline 500.It is according to the ... of the embodiment of the present invention as a result,
The system for preparing casein can respectively obtain that different stage (dissolving pH value), purity are higher and the preferable casein element of quality.
Moreover, it is easy to operate, it is suitable for large-scale production.The system will be described in detail below.
According to an embodiment of the invention, referring to Fig. 3, which includes：
First pH value regulating device 100
According to an embodiment of the invention, the first pH value regulating device is suitable for adjusting the pH value of Qula solution.
According to a particular embodiment of the invention, in the apparatus, the pH value of Qula solution is adjusted to the first predetermined pH value.
The casein dissolving that thereby, it is possible to dissolve pH value no more than the first predetermined pH value, and remaining dissolving pH value (it is pre- to be more than first
Determine pH value) casein it is undissolved.As a result, so that later separation goes out to dissolve the cheese that pH value is no more than the first predetermined pH value
Element.
It should be noted that according to an embodiment of the invention, it, can be according to Qula solution in the first pH value regulating device
Property or state, it is pre-processed using conventional method, to carry out subsequent operation.Specific implementation according to the present invention
Solid-state Qula solution is added to the water immersion 10 minutes, solid-liquid ratio 1 by example:20 (V/V) so that it is swollen, convenient for adjusting
Target casein can fully dissolve after pH value.
Equipment for separating liquid from solid 200
According to an embodiment of the invention, equipment for separating liquid from solid is connected with the first pH value regulating device, is suitable for adjusting pH value
Obtained feed liquid carries out solid-liquid separation treatment afterwards, to obtain the first supernatant and the first sediment.First supernatant as a result,
In containing the casein that dissolving pH value is the first predetermined pH value, be more than the first predetermined pH value containing dissolving pH value in the first precipitation
Casein realizes the purpose of separation.
Second pH value regulating device 300
According to an embodiment of the invention, the second pH value regulating device is connected with equipment for separating liquid from solid, is suitable for adjusting on first
The pH value of clear liquid.
According to a particular embodiment of the invention, the pH value of the first supernatant is adjusted to 4.4~4.6.Inventor's discovery, will
The pH value of first supernatant is adjusted to 4.4~4.6, to reach the isoelectric point of casein, makes its precipitation, to further detach
Obtain purer casein.
First circulation pipeline 400
According to an embodiment of the invention, first circulation pipeline respectively with the first pH value regulating device and equipment for separating liquid from solid phase
Even, suitable for making the first sediment be back to the first pH value regulating device.
Second circulation pipeline 500
According to an embodiment of the invention, second circulation pipeline respectively with equipment for separating liquid from solid and the second pH value regulating device phase
Even, it is suitable for carrying out solid-liquid separation treatment to the obtained feed liquid of the pH value for adjusting the first supernatant, to obtain casein.By
This, can obtain the casein that purer dissolving pH value is the first predetermined pH value.
Specifically, if the first predetermined pH value is 6.0, then Qula solution passes through the first pH value regulating device 100, consolidates successively
Liquid separating apparatus 200, the second pH value regulating device 300, second circulation pipeline 500 and equipment for separating liquid from solid 200, can directly obtain
The casein that pH value is 6.0 must be dissolved.
If the first predetermined pH value is more than 6.0, then Qula solution is obtained by repeating at least one wheel the following steps
's：
S110 adjusts pH value to the second predetermined pH value
The step carries out in the first pH value regulating device, and being will be containing the pH value tune of the first raw material of casein
For section to the second predetermined pH value, the second predetermined pH value is less than the first predetermined pH value, the start numbers of the second predetermined pH value be no more than
6.0 fixed numbers.Dissolving pH value, which is the casein of the second predetermined pH value, as a result, to dissolve, and remaining dissolving pH value (is more than
Second predetermined pH value) casein it is undissolved.As a result, so that later separation goes out to dissolve the cheese that pH value is the second predetermined pH value
Element.
S120 third solid phase separating treatments
The step is carried out in equipment for separating liquid from solid 200, is that obtained mixture in step S110 is carried out third
Solid phase separating treatment, to obtain third supernatant and third precipitation.
According to an embodiment of the invention, according to the difference of the second predetermined pH value and the first predetermined pH value, using two kinds of differences
Mode handles third precipitation, specifically, 1) when the difference of the second predetermined pH value and the first predetermined pH value is no more than 1, third precipitation
Constitute Qula solution, successively pass through the first pH value regulating device 100, equipment for separating liquid from solid 200, the second pH value regulating device 300,
Second circulation pipeline 500 and equipment for separating liquid from solid 200 can directly obtain the casein that dissolving pH value is the first predetermined pH value；
2) when the difference of the second predetermined pH value and the first predetermined pH value is more than 1, following operation is carried out：
S130 return to step S110 repeats the wheels of step S110 and S120 at least one
In the step, third is precipitated and is back to the first pH value regulating device by first circulation pipeline 400, is repeated
Step S110 and S120 at least one takes turns, wherein the second predetermined pH of each round increases by 1, until the second predetermined pH value is pre- with first
The difference for determining pH value is no more than 1.As a result, by improving pH value step by step, to obtain the casein of different stage respectively.
According to an embodiment of the invention, referring to Fig. 4, which further comprises：Aqueous slkali storage device 600 and acid are molten
Liquid storage device 700.
According to a particular embodiment of the invention, aqueous slkali storage device 600 is connected with the first pH value regulating device 100, alkali
Aqueous slkali is housed in solution storage device 600, is suitable for adjusting the pH value of feed liquid in the first pH value regulating device.
According to a particular embodiment of the invention, acid solution storage device 700 is connected with the second pH value regulating device 300, acid
Acid solution is housed in solution storage device 700, is suitable for adjusting the pH value of the first supernatant.
According to an embodiment of the invention, referring to Fig. 5, which further comprises：PH value control device 800 and pH value prison
Survey device 900.
According to a particular embodiment of the invention, aqueous slkali storage device is adjusted by pH value control device and the first pH value and is filled
Set connected, pH value of the pH value control device suitable for controlling feed liquid in the first pH value regulating device.Preferred implementation according to the present invention
Example, the pH value for controlling feed liquid in the first pH value regulating device are 6.0,7.0,8.0,9.0,10.0,11.0 or 12.0.
According to a particular embodiment of the invention, pH value detection device adjusts with pH value control device and the first pH value fill respectively
Set connected, pH value of the pH value monitoring device suitable for monitoring feed liquid in the first pH value regulating device.
It should be noted that it will be appreciated by those skilled in the art that herein used in term " control device ",
" monitoring device " is interpreted broadly, either automatically controlling, such as can also be by manually being controlled by computer
System, wherein preferably use automatic control mode, thus, it is possible to realize the automation of production, reduce labour cost, improve gained
To casein quality batch between consistency.
It will be appreciated to those of skill in the art that above for feature described in the method for casein and excellent is prepared
Point is equally applicable to the system, and details are not described herein.
The solution of the present invention is explained below in conjunction with embodiment.It will be understood to those of skill in the art that following
Embodiment is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Particular technique or item are not specified in embodiment
Part, it is carried out according to technology or condition described in document in the art or according to product description.Agents useful for same or instrument
Production firm person is not specified in device, and being can be with conventional products that are commercially available.
Embodiment 1
In this embodiment, the casein of different stage is prepared in following manner：
(1) Qula raw material, solid-liquid ratio 1 are added in the dissolving cylinder equipped with distilled water:20 (V/V), impregnate at room temperature
10min obtains the first feed liquid；
(2) it uses the sodium hydroxide solution of 4mol/L to adjust the first material liquid pH value to stopping plus alkali when 6.0, stirs 1h, dissolving
The pH value of the first feed liquid of constantly regulate is to 6.0 in the process；
(3) step (2) obtained mixed liquor is centrifuged into 20min under the rotating speed of 4500g, degreasing is removed with filtered through gauze
Fat obtains supernatant and sediment；
(4) supernatant pH value is adjusted to 4.4~4.6 with 1.0mol/L HCl solutions, and obtained mixed liquor is existed
5min is centrifuged under the rotating speed of 4500g；
(5) distilled water and the obtained precipitation of acetone washing step (4) are used respectively twice, to obtain pH6.0 casein；
(6) sediment is back to step (1) and repeats the wheel of step (1)~(5) six, wherein the first material in step (2)
The pH value of liquid is followed successively by 7.0,8.0,9.0,10.0,11.0 and 12.0, to respectively obtain pH7.0 casein, pH8.0 cheese
Element, pH9.0 casein, pH10.0 casein, pH11.0 casein, pH12.0 casein；And
(7) casein of acquisition is subjected to vacuum freeze drying, temperature is -50 DEG C, and pressure is 10~50Pa, and the time is
48h。
2 color and luster of embodiment detects
It is dry that 1 obtained pH6.0 casein of embodiment, pH7.0 casein, pH8.0 are measured respectively using light splitting colour difference meter
The color and luster of casein, pH9.0 casein, pH10.0 casein, pH11.0 casein, pH12.0 casein, the results are shown in Table 1.
As can be seen that Qula casein color and luster is influenced notable (p ＜ 0.05) by dissolving pH.With the increase of dissolving pH, brightness value (L*
Value) it is substantially reduced, red scale value (a* values) and yellow value degree (b* values) significantly increase (p ＜ 0.05), are computed Qula casein whiteness
Value W is gradually reduced with the increase of dissolving pH, and color and luster is deteriorated.Brown angle value C values, in the trend risen, show with the increase of dissolving pH
With the increase of dissolving pH, the generation of sample Huang-brown does not reach saturation, illustrates casein in the stronger item of alkaline condition
The Maillard reaction occurred under part makes the color of sample more complicated.
1 color and luster of table is analyzed
| Sample | L* | a* | b* | W | C |
| pH6 | 86.97±0.21c | -0.19±0.03d | 9.30±0.13c | 83.99±0.23b | 9.31±0.12c |
| pH7 | 87.38±0.17bc | -0.26±0.03c | 9.57±0.15c | 84.16±0.18b | 9.57±0.15c |
| pH8 | 85.81±0.13d | 0.00±0.01e | 11.02±0.07d | 82.03±0.14c | 11.02±0.07d |
| pH9 | 84.59±0.32e | 0.22±0.04f | 12.28±0.24e | 80.30±0.38d | 12.28±0.24e |
| pH10 | 83.21±0.16f | 0.59±0.05h | 13.08±0.21f | 78.71±0.25e | 13.09±0.21f |
| pH11 | 83.12±1.04f | 0.37±0.08g | 12.92±0.14f | 78.74±0.85e | 12.92±0.14f |
| pH12 | 82.50±0.18f | 1.48±0.03i | 14.67±0.20g | 77.12±0.26f | 14.75±0.20g |
Note：L*- brightness values (value), a*- red scale values (value), b*- yellow value degrees (value), W- whiteness values, the brown angle value of C-
3 emulsifying activity of embodiment (EAI) and emulsion stability (ESI) detection
1 obtained pH6.0 casein of embodiment, pH7.0 casein, pH8.0 casein, pH9.0 cheese are measured respectively
The emulsifying activity of element, pH10.0 casein, pH11.0 casein, pH12.0 casein, the specific method is as follows：
With reference to Jiang and Zhao, 2011 (Jiang S J, Zhao X H.Transglutaminase-induced
cross-linking and glucosamine conjugation of casein and some functional
properties of the modified product[J].International Dairy Journal,2011,21(4):
Method analysis 198-205.) measures the emulsifying activity and emulsion stability of casein sample.A certain amount of casein sample is weighed,
It is made into the casein solution of 2mg/mL.Above-mentioned casein solution 6.00mL and 2.00mL is taken to be mixed in 50mL centrifuge tubes, in
20000rpm emulsifyings 1min；Respectively 50 are taken at distance centrifugation bottom of the tube 0.5cm in 0min, standing 10min and 30min
μ L lotions, and be the SDS solution mixings of 1g/L with 5mL mass concentrations, reference is done with a concentration of 1g/L SDS solution, is recorded
Absorbance value at 500nm.
Emulsifying activity (EAI, m2/ g) and the calculation formula of emulsion stability (ESI, %) it is as follows：
ESI (%)=100 × Ai/A0
In formula, C is the concentration of casein solution before emulsification, g/L；D is extension rate, is 100；For cuvette thickness,
0.01mm；θ is the volume fraction of oil phase in lotion, is 0.25；A0For the absorbance of 0min after emulsification；AiTo stand the suction of i min
Shading value.
The results are shown in Figure 6 for emulsifying activity, with gradually rising for dissolving pH value, the emulsifying activity of corresponding casein
The trend of reduction is substantially presented.Thus, it is possible to select the casein of different stage according to actual production demand.
The results are shown in Figure 7 for emulsion stability, and with gradually rising for dissolving pH value, the emulsification of corresponding casein is steady
The qualitative trend that reduction is substantially presented.Thus, it is possible to select the casein of different stage according to actual production demand.
Comparative example 1
In the comparative example, casein is prepared in following manner：
(1) Qula raw material, solid-liquid ratio 1 are added in the dissolving cylinder equipped with distilled water:20 (V/V), impregnate at room temperature
10min obtains the first feed liquid；
(2) it uses the sodium hydroxide solution of 4mol/L to adjust the first material liquid pH value to stopping plus alkali when 10.0, stirs 1h, dissolving
The pH value of the first feed liquid of constantly regulate makes it remain unchanged in the process；
(3) step (2) obtained mixed liquor is centrifuged into 20min under the rotating speed of 4500g, degreasing is removed with filtered through gauze
Fat obtains supernatant and sediment；
(4) supernatant pH value is adjusted to 4.4~4.6 with 1.0mol/L HCl solutions, and obtained mixed liquor is existed
5min is centrifuged under the rotating speed of 4500g；
(5) distilled water and the obtained precipitation of acetone washing step (4) are used respectively twice, to obtain casein.
Measure the emulsifying activity and emulsion stability of the casein respectively according to the method for embodiment 3 and 4, respectively
16.09±0.41m2/ g and 19.85 ± 0.81% (30min), the emulsifying activity and emulsion stability of casein are relatively low, main former
Because the substances such as lactose, protein may be contained in Qula, pH value is adjusted using disposable, excessively high pH value makes lactose, albumen
The reactions such as undesirable change, such as Mei Lade, amino-acid oxidase occur for the substances such as matter, to influence the quality of casein.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiments or example.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changes, replacing and modification.
Claims (10)
1. a kind of method preparing casein, which is characterized in that including：
(1) pH value of Qula solution is adjusted to the first predetermined pH value；
(2) obtained mixture in step (1) is subjected to the first solid phase separating treatment, to obtain the first supernatant and first
Precipitation；
(3) pH value of first supernatant is adjusted to 4.4~4.6；And
(4) obtained mixture in step (3) is subjected to second solid phase separating treatment, to obtain the second precipitation, described the
Two precipitations constitute first object casein.
2. according to the method described in claim 1, it is characterized in that, the first predetermined pH value be more than 6.0, the Qula solution
It is to be obtained by repeating at least one wheel the following steps：
(i) pH value of the first raw material containing casein is adjusted to the second predetermined pH value, the second predetermined pH value is less than
The first predetermined pH value, the start numbers of the second predetermined pH value are the fixed numbers no more than 6.0；
(ii) obtained mixture in step (i) is subjected to third solid phase separating treatment, to obtain third supernatant and the
Three precipitations,
Wherein, when the difference of the described second predetermined pH value and the described first predetermined pH value is no more than 1, the third precipitation constitutes institute
Qula solution is stated, when the difference of the described second predetermined pH value and the described first predetermined pH value is more than 1, the third is precipitated and is returned
Repeating step (i) to step (i) and (ii) at least one takes turns, wherein second predetermined pH of each round increases by 1, until
The difference of the second predetermined pH value and the described first predetermined pH value is no more than 1.
3. according to the method described in claim 2, it is characterized in that, step (ii) further comprises：
The pH value of the third supernatant is adjusted to 4.4~4.6, and is detached by solid phase to obtain the second target cheese
Element.
4. according to the method described in claim 2, it is characterized in that, step (1) and (i) in, using aqueous slkali carry out pH value tune
Section,
Preferably, a concentration of 4mol/L of the aqueous slkali.
5. according to the method described in claim 3, it is characterized in that, in step (3) and (ii), pH value tune is carried out using acid solution
Section,
Preferably, a concentration of 1.0mol/L of the acid solution.
6. according to the method described in claim 2, it is characterized in that, at the first solid phase separating treatment, second solid phase separation
Reason and third solid phase separating treatment are to centrifuge 20min under the rotating speed of 4500g.
7. a kind of method preparing casein, which is characterized in that including：
(a) Qula raw material, solid-liquid ratio 1 are added in the dissolving cylinder equipped with distilled water:20 (V/V), impregnate 10min, obtain at room temperature
To the first feed liquid；
(b) it uses the sodium hydroxide solution of 4mol/L to adjust first material liquid pH value to stopping plus alkali when 6.0, stirs 1h, dissolving
The pH value of the first feed liquid described in constantly regulate is to 6.0 in the process；
(c) the obtained mixed liquor of step (b) is centrifuged into 20min under the rotating speed of 4500g, removes fat with filtered through gauze, obtains
To supernatant and sediment；
(d) the supernatant pH value is adjusted to 4.4~4.6 with 1.0mol/L HCl solutions, and obtained mixed liquor is existed
5min is centrifuged under the rotating speed of 4500g；
(e) distilled water and the obtained precipitation of acetone washing step (d) are used respectively twice, to obtain pH6.0 casein；
(f) sediment is back to step (a) and repeats the wheels of step (a)~(e) six, wherein the first material in step (b)
The pH value of liquid is followed successively by 7.0,8.0,9.0,10.0,11.0 and 12.0, to respectively obtain pH7.0 casein, pH8.0 cheese
Element, pH9.0 casein, pH10.0 casein, pH11.0 casein, pH12.0 casein；And
(g) casein of acquisition is subjected to vacuum freeze drying, temperature is -50 DEG C, and pressure is 10~50Pa, and the time is
48h。
8. a kind of any one of implementation claim 1~7 system for preparing casein method, which is characterized in that including：
First pH value regulating device, the first pH value regulating device are suitable for adjusting the pH value of the Qula solution；
Equipment for separating liquid from solid, the equipment for separating liquid from solid are connected with the first pH value regulating device, after being suitable for adjusting pH value
Obtained feed liquid carries out solid-liquid separation treatment, to obtain the first supernatant and the first sediment；
Second pH value regulating device, the second pH value regulating device are connected with the equipment for separating liquid from solid, are suitable for described in adjusting
The pH value of first supernatant；
First circulation pipeline, the first circulation pipeline respectively with the first pH value regulating device and equipment for separating liquid from solid phase
Even, suitable for making first sediment be back to the first pH value regulating device；And
Second circulation pipeline, the second circulation pipeline respectively with the equipment for separating liquid from solid and the second pH value regulating device phase
Even, it is suitable for carrying out solid-liquid separation treatment to the obtained feed liquid of the pH value for adjusting first supernatant, to obtain casein.
9. system according to claim 8, which is characterized in that further comprise：
Aqueous slkali storage device, the aqueous slkali storage device are connected with the first pH value regulating device, the aqueous slkali storage
Aqueous slkali is housed in standby device, is suitable for adjusting the pH value of feed liquid in the first pH value regulating device；And
Acid solution storage device, the acid solution storage device are connected with the second pH value regulating device, the acid solution storage
Acid solution is housed in standby device, is suitable for adjusting the pH value of first supernatant.
10. system according to claim 9, which is characterized in that further comprise：
PH value control device, the aqueous slkali storage device pass through the pH value control device and the first pH value regulating device
It is connected, the pH value control device is suitable for controlling the pH value of feed liquid in the first pH value regulating device, it is preferable that described in control
The pH value of feed liquid is 6.0,7.0,8.0,9.0,10.0,11.0 or 12.0 in first pH value regulating device；
PH value monitoring device, the pH value detection device respectively with the pH value control device and the first pH value regulating device phase
Even, the pH value monitoring device is suitable for monitoring the pH value of feed liquid in the first pH value regulating device.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113248589A (en) * | 2021-06-30 | 2021-08-13 | 中国海洋大学 | Preparation method of Qula casein |
| CN115989846A (en) * | 2023-03-21 | 2023-04-21 | 中国农业大学 | Graded preparation method of trovain |
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| CN113248589A (en) * | 2021-06-30 | 2021-08-13 | 中国海洋大学 | Preparation method of Qula casein |
| CN115989846A (en) * | 2023-03-21 | 2023-04-21 | 中国农业大学 | Graded preparation method of trovain |
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| CN108567045B (en) | 2021-03-26 |
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