CN104904989A - Lactoprotein concentrate with high thermal stability and preparation method thereof - Google Patents

Lactoprotein concentrate with high thermal stability and preparation method thereof Download PDF

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CN104904989A
CN104904989A CN201510388532.1A CN201510388532A CN104904989A CN 104904989 A CN104904989 A CN 104904989A CN 201510388532 A CN201510388532 A CN 201510388532A CN 104904989 A CN104904989 A CN 104904989A
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content
ultrafiltration
concentration
trapped fluid
temperature
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CN104904989B (en
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孙颜君
郭本恒
莫蓓红
刘振民
石春权
朱培
郑远荣
焦晶凯
凌勇飚
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Shanghai Bright Dairy and Food Co Ltd
Bright Dairy and Food Co Ltd
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Abstract

The invention discloses a lactoprotein concentrate with high thermal stability and a preparation method thereof The method comprises the following steps of: 1, degreasing raw milk, adding emulsified salt, wherein the mass volume percentage of the emulsified salt is 0.1-0.5%, the emulsified salt is selected from two or three of sodium citrate, sodium pyrophosphate and trisodium phosphate, and the mass ratio of the sodium citrate to the sodium pyrophosphate is 2:3-3:2, the mass ratio of the sodium citrate to the trisodium phosphate is 3:7-7:3, and the mass ratio of the sodium pyrophosphate to the trisodium phosphate is 3:2-4:1, stirring for 5-10min at the speed of 50-100r/m and the temperature of 50-55 DEG C, regulating the pH value to be 5.0-6.5, and sterilizing; evaporating to concentrate or filter washing to concentrate after ultra-filtering at the temperature of 10-40 DEG C, and spray drying. According to the preparation method of the lactoprotein concentrate, the albuminous degeneration is well prevented, and the production efficiency is improved. The prepared lactoprotein concentrate has good thermal stability at high temperatures.

Description

Lactoprotein concentrate of high thermal stability and preparation method thereof
Technical field
The present invention relates to dairy products field, lactoprotein concentrate product being specifically related to a kind of high thermal stability and preparation method thereof.
Background technology
Lactoprotein concentrate (Milk protein concentrates, MPC) refers to that the milk protein content utilizing membrane separating method to produce is at 40-85% or the product more than 85%.We can be called (embrane method) lactoprotein concentrate, or claim (embrane method) newborn protein concentrate.
Business-like MPC protein quality mark is not at 42-85% etc., in MPC, protein content is higher, and lactose content is lower, and casein is similar to raw milk with the ratio of lactalbumin, the best original character maintaining albumen, these characteristics make it to be able to extensive use in food processing.Due to this series products high protein Low lactose milk, be commonly used to increase percent protein in dairy products processing, but can albuminous degeneration be there is in higher protein content in high-temperature sterilization process, thus affect the nutritive peculiarity of albumen, and be unfavorable for the processing of product.Existing quite a lot of research at present improves MPC product dissolubility about raising, as adopted the methods such as ion-exchange, ultrasonic wave and super-pressure, but less about the research improving product heat endurance.
In membrane separating process, improve temperature and can improve membrane flux, thus improve separative efficiency, but too high temperature can increase albuminous degeneration.Therefore, seldom can take into account separative efficiency and albuminous degeneration in current technique simultaneously.
Summary of the invention
Technical problem to be solved by this invention existingly prepare temperature too high in the technique of lactoprotein concentrate in order to overcome and can increase albuminous degeneration and seldom can take into account separative efficiency and protein-denatured technical problem simultaneously, provides a kind of preparation method of lactoprotein concentrate of high thermal stability.The present invention not only well prevents albuminous degeneration in MPC, and is beneficial to the carrying out of ultrafiltration technology, improves production efficiency.Obtained MPC powder drying, with dense milk fragrance, in vivid milky, has good powder property, at high temperature.The MPC that this method is obtained has good heat endurance, can be widely used in food processing.
One of technical solution of the present invention: a kind of method preparing the lactoprotein concentrate of high thermal stability, it comprises the following steps: (1) gets raw milk degreasing, emulsification salt is added in skimmed milk, the quality percent by volume that described emulsification salt quality accounts for described degreasing raw milk volume is 0.1-0.5%, described emulsification salt is be selected from any two or three in natrium citricum, sodium pyrophosphate and tertiary sodium phosphate, and the mass ratio of described natrium citricum and sodium pyrophosphate is 2: 3-3: 2; The mass ratio of described natrium citricum and tertiary sodium phosphate is 3: 7-7: 3; The mass ratio of described sodium pyrophosphate and tertiary sodium phosphate is 3: 2-4: 1,50-55 DEG C 50-100 rev/min and stirs 5-10 minute, and regulate pH to 5.0-6.5, sterilization, obtains sterilization skimmed milk; (2) evaporation and concentration after the 10-40 DEG C of ultrafiltration of described for step (1) sterilization skimmed milk or filter wash are concentrated, spraying dry.
In the present invention, described raw milk can be the raw milk of this area, this area routine, as fresh milk or reconstituted milk, is preferably fresh milk.
In the present invention, described raw milk can be the raw milk of this area routine, as raw milk or raw sheep breast, is preferably raw milk.
In the present invention, in described raw milk, the content of protein can be the customary amount of this area, be preferably 3.0-3.5%, be more preferably 3.2-3.5%, be 3.2% best, the content of fat can be the customary amount of this area, be preferably 3.6-4.2%, be more preferably 3.6-3.8%, be 3.8% best, the content of lactose can be the content of this area routine, be preferably 4.0-4.95%, be more preferably 4.0-4.5%, be 4.5% best, the content of ash content can be the content of this area routine, be preferably 0.6-0.8%, be more preferably 0.6-0.7%, be 0.6% best, described percentage is the mass percent accounting for raw milk gross mass.
In the present invention, step (1) is: (1) gets raw milk degreasing, emulsification salt is added in skimmed milk, the quality percent by volume that described emulsification salt quality accounts for described degreasing raw milk volume is 0.1-0.5%, described emulsification salt is be selected from any two or three in natrium citricum, sodium pyrophosphate and tertiary sodium phosphate, and the mass ratio of described natrium citricum and sodium pyrophosphate is 2: 3-3: 2; The mass ratio of described natrium citricum and tertiary sodium phosphate is 3: 7-7: 3; The mass ratio of described sodium pyrophosphate and tertiary sodium phosphate is 3: 2-4: 1,50-55 DEG C 50-100 rev/min and stirs 5-10 minute, and regulate pH to 5.0-6.5, sterilization, obtains sterilization skimmed milk.
In step (1), described degreasing can, for producing operation conventional in MPC, be preferably centrifugal degreasing.The temperature of described degreasing can for producing temperature conventional in MPC, and being preferably 40-60 DEG C, is more preferably 50-55 DEG C, is 53 DEG C best.The centrifugal rotating speed of described degreasing can be the rotating speed of this area routine, and be preferably 7000-12000r/min, that better is 8000-10000r/min, is 9000r/min best.The centrifugal feed rate of described degreasing is 90-120L/h, and being preferably 95-100L/h, is more preferably 98L/h.The temperature of described stirring is 50-55 DEG C, is preferably 50-53 DEG C, is more preferably 53 DEG C, the rotating speed of described stirring is 50-100rpm, is preferably 50-80rpm, is more preferably 80rpm, the time of described stirring is 5-10min, is preferably 5-8min, is more preferably 8min.
Described emulsification salt is any two kinds of being selected from natrium citricum, sodium pyrophosphate and tertiary sodium phosphate, is preferably natrium citricum and sodium pyrophosphate.The quality percent by volume that described emulsification salt quality accounts for described degreasing raw milk cumulative volume is 0.1-0.5%, is preferably 0.1-0.3%, is more preferably 0.3%.When described emulsification salt comprises natrium citricum and sodium pyrophosphate, the mass ratio of described natrium citricum and sodium pyrophosphate is 2: 3-3: 2, is preferably 1: 1-3: 2, and better is 1: 1.When described emulsification salt comprises natrium citricum and tertiary sodium phosphate, the mass ratio of described natrium citricum and tertiary sodium phosphate is 3: 7-7: 3, is preferably 3: 7-1: 1, is more preferably 3: 7.When described emulsification salt comprises sodium pyrophosphate and tertiary sodium phosphate, the mass ratio of described sodium pyrophosphate and tertiary sodium phosphate is 3: 2-4: 1, is preferably 4: 1.Described adjust pH can be the operation of this area routine, as by acid or alkali adjust ph, preferably uses 1mol/L NaOH or HCl standard liquid adjust ph.Described pH value is 5.0-6.5, is preferably 5.5-6.0, is more preferably 5.8-6.0, is 6.0 best.Described sterilization can for producing operation conventional in MPC, and the temperature of described sterilization can for producing temperature conventional in MPC, and being preferably 130-140 DEG C, is more preferably 135-140 DEG C, is 135 DEG C best.The time of described sterilization can be conventional duration, and being preferably 3-5s, is more preferably 4-5s, is 5s best.
In the present invention, step (2) is: evaporation and concentration after the 10-40 DEG C of ultrafiltration of described for step (1) sterilization skimmed milk or filter wash are concentrated, spraying dry.
In step (2), the molecular cut off of the filter membrane of described ultrafiltration can for producing size conventional in MPC, and being preferably 5-30kDa, is more preferably 10kDa.The filter membrane of described ultrafiltration can for producing filter membrane conventional in MPC, and such as cellulose ester membrane, regenerated cellulose film, ceramic membrane, poly (ether sulfone) film or polyvinylidene fluoride film are preferably regenerated cellulose film.The temperature of described ultrafiltration is 10-40 DEG C, is more preferably 10-15 DEG C, is 10 DEG C best.The pressure of described ultrafiltration can, for producing the pressure of conventional size in MPC, be preferably 1.5 × 10 5-3 × 10 5pa is more preferably 2 × 10 5-3 × 10 5pa is 3 × 10 best 5pa.The cycles of concentration of described ultrafiltration can, for producing multiple conventional in MPC, be preferably concentrate 3-7 doubly.When obtained MPC is MPC40, the cycles of concentration of described ultrafiltration is 3-5 times, is preferably 3-4 times, is more preferably 4 times.When obtained MPC is MPC70, the cycles of concentration of described ultrafiltration is 4-6 times, is preferably 5-6 times, is more preferably 6 times.When obtained MPC is MPC85, the cycles of concentration of described ultrafiltration is 5-7 times, is preferably 6-7 times, is more preferably 7 times.
Described filter wash for producing operation conventional in MPC, preferably can comprise: fill in the trapped fluid of described ultrafiltration with the isopyknic deionized water of permeate after ultrafiltration concentration further, repeats 2-4 time, more preferably repetition 2-3 time, best repetition 3 times.When obtained MPC is MPC70, the cycles of concentration of described further ultrafiltration is 4-6 times, is preferably 5-6 times, is more preferably 6 times.When obtained MPC is MPC85, the cycles of concentration of described further ultrafiltration is 5-7 times, is preferably 6-7 times, is more preferably 7 times.
Described evaporation and concentration can, for producing evaporation and concentration operation conventional in MPC, be preferably film vacuum evaporation and concentration.The temperature of described film vacuum evaporation and concentration is 60-70 DEG C, is preferably 60-65 DEG C, is more preferably 65 DEG C.The solid content of described for step (1) sterilization skimmed milk is preferably concentrated into 20-25% by described concentrating, protein content is concentrated into 11-25%, fat content is concentrated into 0.4-0.9%, content of ashes is concentrated into 1.5-3.5%, lactose content is concentrated into 0.05-8%, and described percentage is the mass percent of the sterilization skimmed milk gross mass after accounting for described concentrating.
Described spraying dry can, for producing operation conventional in MPC, preferably adopt vertical spray drying tower to carry out.Described spray-dired EAT can be the temperature of this area routine, is preferably 110-140 DEG C, is more preferably 110-130 DEG C, is 130 DEG C best.Described spray-dired temperature of outgoing air can be the temperature of this area routine, is preferably 60-90 DEG C, is more preferably 60-70 DEG C, is 70 DEG C best.Described spray-dired pressure can be the pressure of the conventional size in this area, and being preferably 0.8-1.2bar, is more preferably 1-1.2bar, is 1.2bar best.Described spray-dired feed rate can be the pressure of this area routine, is preferably 0.6-1.4kg/h, is more preferably 1-1.4kg/h, is 1.4kg/h best.
By ultrafiltration different multiples in step (2), the number of times that optionally filter wash is different can obtain the lactoprotein concentrated product of different protein content, is specially:
A, after described for step (1) sterilization skim milk ultra being concentrated 3-5 times, trapped fluid being carried out evaporation and concentration to solid content is 20%-25%, protein content is 11-14%, fat content is 0.50-0.60%, lactose content is 6.5-8%, content of ashes is 3-3.5%, carry out spraying dry and namely obtain MPC40, solid content is 95%-97%, protein content is 40.15-43.86%, fat content is 0.95-1.05%, lactose content is 45-47%, content of ashes is 6.5-8.0%, described percentage is the mass percent of the sterilization skimmed milk gross mass after accounting for described concentrating.。
B, ultrafiltration is stopped after described for step (1) sterilization skim milk ultra being concentrated 4-6 times, ultrafiltration concentration is continued to 4-6 times add deionized water to original volume in trapped fluid after, repetition like this 2-4 time, finally obtaining solid content in trapped fluid is 20-23%, protein content is 15-18%, fat content is 0.70-0.90%, lactose content is 2.0-3.5%, content of ashes is 1.50-2.0%, carry out spraying dry and namely obtain MPC70, solid content is 95%-97%, protein content is 68.50-71.65%, fat content is 0.95-1.50%, lactose content is 15-17%, content of ashes is 7.5-8.5%, described percentage is the mass percent of the sterilization skimmed milk gross mass after accounting for described concentrating.。
C, ultrafiltration is stopped after described for step (1) sterilization skim milk ultra being concentrated 5-7 times, ultrafiltration concentration is continued to 5-7 times add deionized water to original volume in trapped fluid after, repetition like this 2-4 time, finally obtaining solid content in trapped fluid is 20-23%, protein content is 16-20%, fat content is 0.40-0.60%, lactose content is 0.05-0.10%, content of ashes is 1.50-2.0%, carry out spraying dry and namely obtain MPC85, solid content is 95%-97%, protein content is 84.50-86.50%, fat content is 1.50-1.70%, lactose content is 0.70-0.80%, content of ashes is 6.5-7.5%, described percentage is the mass percent of the sterilization skimmed milk gross mass after accounting for described concentrating.。
Technical solution of the present invention two: a kind of lactoprotein concentrate of high stability, it is obtained by preceding method.
Without prejudice to the field on the basis of common sense, above-mentioned each optimum condition, can be combined, obtain the preferred embodiments of the invention.
Agents useful for same of the present invention and raw material are all commercially.
Positive progressive effect of the present invention is: the present invention well prevent the albuminous degeneration in MPC, and is beneficial to the carrying out of ultrafiltration technology, improves production efficiency.Obtained MPC powder drying, with strong milk fragrance, in vivid milky, has good powder property, and at high temperature obtained according to the inventive method MPC has good heat endurance, can be widely used in food processing.
Detailed description of the invention
Mode below by embodiment further illustrates the present invention, but does not therefore limit the present invention among described scope of embodiments.The experimental technique of unreceipted actual conditions in the following example, conventionally and condition, or selects according to catalogue.
Material and reagent
Raw milk: Shanghai Bright Dairy & Food Co., Ltd.; Natrium citricum/potassium, sodium pyrophosphate/potassium, tertiary sodium phosphate/potassium, calgon/potassium, sodium dihydrogen phosphate/potassium, sodium hydrogen phosphate/potassium, tertiary sodium phosphate and sodium phosphate trimer: Beijing chemical reagent Co., Ltd
Film device: 10kDaPES film is Synder filtration Co., Ltd; Thin film evaporation inspissator: Shanghai moral large sky one Chemical Equipment Co., Ltd.; Spray drying device is purchased from Co., Ltd in GEA engineering.
The yield of mistake film pressure (TMP) used in embodiment below adopts following formulae discovery:
Wherein, P chargingand P backflowrepresent the pressure of feed end and backflow end respectively;
The experimental technique used in following embodiment if no special instructions, is conventional method.
Material used in following embodiment, reagent etc., if no special instructions, all can obtain from commercial channels.
Embodiment 1
1) fresh raw milk is got, its protein content is 3.2% (w/w), fat content is 3.8% (w/w), lactose content is 4.5% (w/w), content of ashes is 0.7%, be heated to 53 DEG C and carry out centrifugal degreasing, centrifugation rate is 9000r/min, feed rate is 98L/h, natrium citricum and sodium pyrophosphate is added in above-mentioned skimmed milk, both proportionings are 1: 1, total addition level is 0.3% (w/w), 8min is stirred at 53 DEG C, stir speed (S.S.) is 80rpm, use 1mol/L HCl standard liquid adjust ph to 5.8 while stirring, 130 DEG C of sterilization 5s,
2) with the regenerated cellulose film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 15 DEG C, pressure 2 × 10 5pa, in ultra-filtration process, membrane flux is 25Lm -2h -1, after adding deionized water, membrane flux is 30Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 4 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 23% (w/w) to solid content, protein content is 13% (w/w), fat content is 0.55% (w/w), and lactose content is 7% (w/w), and ash content is 3.2% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22% (w/w), and protein content is 17% (w/w), and fat content is 0.8% (w/w), lactose content is 3% (w/w), and ash content is 1.8% (w/w);
C, MPC85: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22% (w/w), and protein content is 18% (w/w), and fat content is 0.5% (w/w), lactose content is 0.08% (w/w), and ash content is 1.75% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 125 DEG C, outlet temperature 68 DEG C, pressure 1bar, and charging flow velocity 1kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 2
1) fresh raw milk is got, its protein content is 3.0% (w/w), fat content is 3.85% (w/w), lactose content is 4.0% (w/w), content of ashes is 0.6%, be heated to 50 DEG C and carry out centrifugal degreasing, centrifugation rate is 8000r/min, feed rate is 95L/h, natrium citricum and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 3: 7, total addition level is 0.1% (w/w), 5min is stirred at 53 DEG C, stir speed (S.S.) is 50rpm, use 1mol/L HCl standard liquid adjust ph to 5.5 while stirring, 140 DEG C of sterilization 3s,
2) with the regenerated cellulose film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 10 DEG C, pressure 1.5 × 10 5pa, in ultra-filtration process, membrane flux is 20Lm -2h -1, after adding deionized water, membrane flux is 25Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 3 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 20% (w/w) to solid content, protein content is 11% (w/w), fat content is 0.50% (w/w), and lactose content is 6.5% (w/w), and ash content is 3.0% (w/w);
B, MPC70: after ultrafiltration concentration 4 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 2 times, collect final trapped fluid, trapped fluid solid content is 20% (w/w), and protein content is 15% (w/w), and fat content is 0.7% (w/w), lactose content is 2.0% (w/w), and ash content is 1.5% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 2 times, collect final trapped fluid, trapped fluid solid content is 20% (w/w), and protein content is 16% (w/w), and fat content is 0.4% (w/w), lactose content is 0.05% (w/w), and ash content is 1.50% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 110 DEG C, outlet temperature 60 DEG C, pressure 1bar, charging flow velocity 0.6kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 3
1) fresh raw milk is got, its protein content is 3.5% (w/w), fat content is 4.2% (w/w), lactose content is 4.95% (w/w), content of ashes is 0.80%, be heated to 55 DEG C and carry out centrifugal degreasing, centrifugation rate is 10000r/min, feed rate is 100L/h, sodium pyrophosphate and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 4: 1, total addition level is 0.5% (w/w), 10min is stirred at 55 DEG C, stir speed (S.S.) is 100rpm, use 1mol/L HCl standard liquid adjust ph to 6.0 while stirring, 135 DEG C of sterilization 4s,
2) with the regenerated cellulose film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 40 DEG C, pressure 3 × 10 5pa, in ultra-filtration process, membrane flux is 30Lm -2h -1, after adding deionized water, membrane flux is 35Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 5 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 70 DEG C, be 25% (w/w) to solid content, protein content is 14% (w/w), fat content is 0.60% (w/w), and lactose content is 8% (w/w), and ash content is 3.5% (w/w);
B, MPC70: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 4 times, collect final trapped fluid, trapped fluid solid content is 23% (w/w), and protein content is 18% (w/w), and fat content is 0.9% (w/w), lactose content is 3.5% (w/w), and ash content is 2.0% (w/w);
C, MPC85: after ultrafiltration concentration 7 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 4 times, collect final trapped fluid, trapped fluid solid content is 23% (w/w), and protein content is 20% (w/w), and fat content is 0.6% (w/w), lactose content is 0.10% (w/w), and ash content is 2.0% (w/w);
3) carry out spraying dry by the trapped fluid after evaporation and concentration with through the trapped fluid of filter wash, condition is: inlet temperature 130 DEG C, outlet temperature 70 DEG C, pressure 1.2bar, charging flow velocity 1.4kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 4
1) fresh raw milk is got, its protein content is 3.4% (w/w), fat content is 3.6% (w/w), lactose content is 4.2% (w/w), content of ashes is 0.7%, be heated to 60 DEG C and carry out centrifugal degreasing, centrifugation rate is 7000r/min, feed rate is 90L/h, natrium citricum and sodium pyrophosphate is added in above-mentioned skimmed milk, both proportionings are 3: 2, total addition level is 0.3% (w/w), 8min is stirred at 53 DEG C, stir speed (S.S.) is 80rpm, use 1mol/L HCl standard liquid adjust ph to 6.5 while stirring, 130 DEG C of sterilization 5s sterilization,
2) with the cellulose ester membrane of 5kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 20 DEG C, pressure 2 × 10 5pa, in ultra-filtration process, membrane flux is 25Lm -2h -1, after adding deionized water, membrane flux is 35Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 4 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 24% (w/w) to solid content, protein content is 12% (w/w), fat content is 0.55% (w/w), and lactose content is 6.6% (w/w), and ash content is 3.4% (w/w);
B, MPC70: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22% (w/w), and protein content is 16% (w/w), and fat content is 0.8% (w/w), lactose content is 2.9% (w/w), and ash content is 1.9% (w/w);
C, MPC85: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 4 times, collect final trapped fluid, trapped fluid solid content is 22% (w/w), and protein content is 17% (w/w), and fat content is 0.55% (w/w), lactose content is 0.08% (w/w), and ash content is 1.75% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 140 DEG C, outlet temperature 90 DEG C, pressure 1bar, and charging flow velocity 1kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 5
1) fresh raw milk is got, its protein content is 3.5% (w/w), fat content is 4.2% (w/w), lactose content is 4.95% (w/w), content of ashes is 0.80%, be heated to 40 DEG C and carry out centrifugal degreasing, centrifugation rate is 12000r/min, feed rate is 120L/h, natrium citricum and sodium pyrophosphate is added in above-mentioned skimmed milk, both proportionings are 2:3, total addition level is 0.3% (w/w), 8min is stirred at 53 DEG C, stir speed (S.S.) is 80rpm, use 1mol/L HCl standard liquid adjust ph to 6.5 while stirring, 130 DEG C of sterilization 5s sterilization,
2) with the ceramic membrane of 30kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 25 DEG C, pressure 2 × 10 5pa, in ultra-filtration process, membrane flux is 29Lm -2h -1, after adding deionized water, membrane flux is 35Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 5 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 23% (w/w) to solid content, protein content is 13% (w/w), fat content is 0.53% (w/w), and lactose content is 6.7% (w/w), and ash content is 3.4% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22% (w/w), and protein content is 17% (w/w), and fat content is 0.85% (w/w), lactose content is 2.7% (w/w), and ash content is 1.7% (w/w);
C, MPC85: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 21% (w/w), and protein content is 17% (w/w), and fat content is 0.4% (w/w), lactose content is 0.05% (w/w), and ash content is 1.79% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 140 DEG C, outlet temperature 90 DEG C, pressure 1bar, and charging flow velocity 1kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 6
1) fresh raw milk is got, its protein content is 3.0% (w/w), fat content is 3.85% (w/w), lactose content is 4.0% (w/w), content of ashes is 0.6%, be heated to 50 DEG C and carry out centrifugal degreasing, centrifugation rate is 8000r/min, feed rate is 95L/h, natrium citricum and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 1: 4, total addition level is 0.1% (w/w), 5min is stirred at 50 DEG C, stir speed (S.S.) is 50rpm, use 1mol/L HCl standard liquid adjust ph to 5.5 while stirring, 140 DEG C of sterilization 3s,
2) with the poly (ether sulfone) film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 10 DEG C, pressure 1.7 × 10 5pa, in ultra-filtration process, membrane flux is 25Lm -2h -1, after adding deionized water, membrane flux is 35Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 3 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 23.80% (w/w) to solid content, protein content is 11.84% (w/w), fat content is 0.55% (w/w), and lactose content is 6.58% (w/w), and ash content is 3.3% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 21.56% (w/w), and protein content is 16.49% (w/w), and fat content is 0.83% (w/w), lactose content is 2.79% (w/w), and ash content is 1.64% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 2 times, collect final trapped fluid, trapped fluid solid content is 22.65% (w/w), and protein content is 17.46% (w/w), and fat content is 0.49% (w/w), lactose content is 0.07% (w/w), and ash content is 1.50% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 125 DEG C, outlet temperature 75 DEG C, pressure 1bar, charging flow velocity 0.8kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 7
1) fresh raw milk is got, its protein content is 3.0% (w/w), fat content is 3.85% (w/w), lactose content is 4.0% (w/w), content of ashes is 0.6%, be heated to 50 DEG C and carry out centrifugal degreasing, centrifugation rate is 8000r/min, feed rate is 95L/h, natrium citricum and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 7: 3, total addition level is 0.2% (w/w), 5min is stirred at 50 DEG C, stir speed (S.S.) is 50rpm, use 1mol/L HCl standard liquid adjust ph to 5.0 while stirring, 135 DEG C of sterilization 4s,
2) with the polyvinylidene fluoride film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 10 DEG C, pressure 2.7 × 10 5pa, in ultra-filtration process, membrane flux is 20.89Lm -2h -1, after adding deionized water, membrane flux is 32.65Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 4 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 24.30% (w/w) to solid content, protein content is 12.89% (w/w), fat content is 0.57% (w/w), and lactose content is 6.70% (w/w), and ash content is 3.45% (w/w);
B, MPC70: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22.46% (w/w), and protein content is 16.60% (w/w), and fat content is 0.85% (w/w), lactose content is 3.25% (w/w), and ash content is 1.65% (w/w);
C, MPC85: after ultrafiltration concentration 6 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 23.65% (w/w), and protein content is 17.84% (w/w), and fat content is 0.52% (w/w), lactose content is 0.08% (w/w), and ash content is 1.55% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 135 DEG C, outlet temperature 80 DEG C, pressure 1bar, charging flow velocity 1.35kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 8
1) fresh raw milk is got, its protein content is 3.2% (w/w), fat content is 3.8% (w/w), lactose content is 4.5% (w/w), content of ashes is 0.7%, be heated to 53 DEG C and carry out centrifugal degreasing, centrifugation rate is 9000r/min, feed rate is 98L/h, natrium citricum and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 1: 1, total addition level is 0.4% (w/w), 8min is stirred at 53 DEG C, stir speed (S.S.) is 80rpm, use 1mol/L HCl standard liquid adjust ph to 5.8 while stirring, 130 DEG C of sterilization 4s sterilization,
2) with the regenerated cellulose film of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 25 DEG C, pressure 2 × 10 5pa, in ultra-filtration process, membrane flux is 22.76Lm -2h -1, after adding deionized water, membrane flux is 30.49Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 4 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 65 DEG C, be 24.75% (w/w) to solid content, protein content is 13.46% (w/w), fat content is 0.57% (w/w), and lactose content is 7.5% (w/w), and ash content is 3.4% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 2 times, collect final trapped fluid, trapped fluid solid content is 22.84% (w/w), and protein content is 17.63% (w/w), and fat content is 0.78% (w/w), lactose content is 2.85% (w/w), and ash content is 1.85% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22.46% (w/w), and protein content is 18.16% (w/w), and fat content is 0.55% (w/w), lactose content is 0.09% (w/w), and ash content is 1.75% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash (would you please confirm after amendment) are carried out spraying dry here, condition is: inlet temperature 125 DEG C, outlet temperature 68 DEG C, pressure 1bar, charging flow velocity 1kg/h, namely the MPC40 of high thermal stability is obtained, MPC70 and MPC85 after drying.
Embodiment 9
1) fresh raw milk is got, its protein content is 3.0% (w/w), fat content is 3.85% (w/w), lactose content is 4.0% (w/w), content of ashes is 0.6%, be heated to 50 DEG C and carry out centrifugal degreasing, centrifugation rate is 8000r/min, feed rate is 95L/h, sodium pyrophosphate and tertiary sodium phosphate is added in above-mentioned skimmed milk, both proportionings are 3: 2, total addition level is 0.25% (w/w), 5min is stirred at 50 DEG C, stir speed (S.S.) is 50rpm, use 1mol/L HCl standard liquid adjust ph to 5.5 while stirring, 140 DEG C of sterilization 3s,
2) with the cellulose ester membrane of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 20 DEG C, pressure 2.7 × 10 5pa, in ultra-filtration process, membrane flux is 24.90Lm -2h -1, after adding deionized water, membrane flux is 33.46Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 3 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 70 DEG C, be 24.80% (w/w) to solid content, protein content is 11.72% (w/w), fat content is 0.58% (w/w), and lactose content is 6.70% (w/w), and ash content is 3.25% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22.46% (w/w), and protein content is 16.90% (w/w), and fat content is 0.9% (w/w), lactose content is 3.25% (w/w), and ash content is 1.75% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 4 times, collect final trapped fluid, trapped fluid solid content is 22.95% (w/w), and protein content is 19.95% (w/w), and fat content is 0.55% (w/w), lactose content is 0.085% (w/w), and ash content is 1.80% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 135 DEG C, outlet temperature 85 DEG C, pressure 0.95bar, charging flow velocity 0.95kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Embodiment 10
1) fresh raw milk is got, its protein content is 3.0% (w/w), fat content is 3.85% (w/w), lactose content is 4.0% (w/w), content of ashes is 0.6%, be heated to 50 DEG C and carry out centrifugal degreasing, centrifugation rate is 8000r/min, feed rate is 95L/h, natrium citricum is added in above-mentioned skimmed milk, sodium pyrophosphate and tertiary sodium phosphate, the proportioning of three is 2: 3: 2, total addition level is 0.25% (w/w), 5min is stirred at 50 DEG C, stir speed (S.S.) is 50rpm, use 1mol/L HCl standard liquid adjust ph to 5.5 while stirring, 140 DEG C of sterilization 3s,
2) with the cellulose ester membrane of 10kDa by step 1) skimmed milk after sterilization carries out ultrafiltration, ultrafiltrate temperature 20 DEG C, pressure 2.7 × 10 5pa, in ultra-filtration process, membrane flux is 24.90Lm -2h -1, after adding deionized water, membrane flux is 33.46Lm -2h -1, particularly:
A, MPC40: after ultrafiltration concentration 3 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 70 DEG C, be 24.80% (w/w) to solid content, protein content is 11.72% (w/w), fat content is 0.58% (w/w), and lactose content is 6.70% (w/w), and ash content is 3.25% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 3 times, collect final trapped fluid, trapped fluid solid content is 22.46% (w/w), and protein content is 16.90% (w/w), and fat content is 0.9% (w/w), lactose content is 3.25% (w/w), and ash content is 1.75% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after filter wash like this repeats 4 times, collect final trapped fluid, trapped fluid solid content is 22.95% (w/w), and protein content is 19.95% (w/w), and fat content is 0.55% (w/w), lactose content is 0.085% (w/w), and ash content is 1.80% (w/w);
3) trapped fluid through evaporation and concentration and the trapped fluid through filter wash are carried out spraying dry, condition is: inlet temperature 135 DEG C, outlet temperature 85 DEG C, pressure 0.95bar, charging flow velocity 0.95kg/h, namely obtains the MPC40 of high thermal stability, MPC70 and MPC85 after drying.
Comparative example 1
1): do not add emulsification salt, other are with embodiment 1 step 1);
2): divided by lower outside, all the other are with embodiment 1 step 2), in ultra-filtration process, membrane flux is 13Lm -2h -1, after adding deionized water, membrane flux is 18Lm -2h -1, be specially:
A, MPC40: after ultrafiltration 5 times, collect trapped fluid, directly carry out evaporation and concentration, evaporation and concentration temperature is 70 DEG C, be 23.15% (w/w) to solid content, protein content is 13.21% (w/w), fat content is 0.56% (w/w), and lactose content is 7.5% (w/w), and ash content is 3.25% (w/w);
B, MPC70: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after repetition like this 3 times, collect final trapped fluid, trapped fluid solid content is 22.04% (w/w), and protein content is 16.11% (w/w), and fat content is 0.89% (w/w), lactose content is 3.15% (w/w), and ash content is 1.85% (w/w);
C, MPC85: after ultrafiltration concentration 5 times, stop ultrafiltration, deionized water isopyknic with permeate is filled into identical with first volume in trapped fluid, after repetition like this 4 times, collect final trapped fluid, trapped fluid solid content is 20.11% (w/w), and protein content is 16.40% (w/w), and fat content is 0.41% (w/w), lactose content is 0.10% (w/w), and ash content is 1.98% (w/w);
3) carry out spraying dry by the trapped fluid after evaporation and concentration with through the trapped fluid of filter wash, condition is: inlet temperature 130 DEG C, outlet temperature 70 DEG C, pressure 1.2bar, charging flow velocity 1.4kg/h, after drying the MPC40 of high thermal stability, MPC70 and MPC85 product.
Comparative example 2
All operations step, with embodiment 2, is only step 1) in emulsification salt add total amount be 0.05% (w/w), wherein the ratio of natrium citricum and tertiary sodium phosphate is 1:9.
Comparative example 3
All operations step is with embodiment 3, only step 1) in pH be adjusted to 7.0.
Effect example 1
Thermal stability determination method
HCT is with reference to the method for Davies and White (1959): from the product of embodiment 1-10 and comparative example 1-3, get the MPC solution that 3ml is mixed with 5% be respectively placed in heat-resisting test tube, then 120 DEG C of oil baths are placed in, observe the state of solution in test tube, and record from time required for oil bath to the visible flocculent deposit of naked eyes, this time namely can the heat endurance of reaction solution, and the time, longer explanation heat endurance was better.The composition of embodiment 1-10MPC product and thermostable effect in the composition of Table 1-10, comparative example 1-3MPC product and thermal stability result in Table 11-13.
The composition of table 1 embodiment 1 product and heat endurance
The composition of table 2 embodiment 2 product and heat endurance
The composition of table 3 embodiment 3 product and heat endurance
The composition of table 4 embodiment 4 product and heat endurance
The composition of table 5 embodiment 5 product and heat endurance
The composition of table 6 embodiment 6 product and heat endurance
The composition of table 7 embodiment 7 product and heat endurance
The composition of table 8 embodiment 8 product and heat endurance
The composition of table 9 embodiment 9 product and heat endurance
The composition of table 10 embodiment 10 product and heat endurance
The composition of table 11 comparative example 1 product and heat endurance
The composition of table 12 comparative example 2 product and heat endurance
The composition of table 13 comparative example 3 product and heat endurance
From comparative example 1, at low temperatures ultrafiltration, if do not add emulsification salt in skimmed milk, greatly can reduce the speed of ultrafiltration, and in the MPC series of products of gained, calcium content is higher, the heat endurance of product is poor; From comparative example 2, if emulsification salt addition is less than 0.1% (w/w), and add the ratio of natrium citricum and tertiary sodium phosphate not in prescribed limit, colloid calcium is then not enough to change into ion state calcium, in the MPC product of gained, calcium content is relatively high, and product is thermally-stabilised poor; From comparative example 3, add emulsification salt in skimmed milk and regulate pH not in prescribed limit, although remarkable impact can not be caused on the basis of product, the heat endurance of product can be affected.
Should be understood that, after having read foregoing of the present invention, those skilled in the art can make various changes or modifications correlated condition of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.

Claims (10)

1. prepare a method for the lactoprotein concentrate of high thermal stability, it is characterized in that, it comprises the following steps:
(1) raw milk degreasing is got, emulsification salt is added in skimmed milk, the quality percent by volume that described emulsification salt quality accounts for described degreasing raw milk volume is 0.1-0.5%, described emulsification salt is be selected from any two or three in natrium citricum, sodium pyrophosphate and tertiary sodium phosphate, and the mass ratio of described natrium citricum and sodium pyrophosphate is 2: 3-3: 2; The mass ratio of described natrium citricum and tertiary sodium phosphate is 3: 7-7: 3; The mass ratio of described sodium pyrophosphate and tertiary sodium phosphate is 3: 2-4: 1,50-55 DEG C 50-100 rev/min and stirs 5-10 minute, and regulate pH to 5.0-6.5, sterilization, obtains sterilization skimmed milk;
(2) evaporation and concentration after the 10-40 DEG C of ultrafiltration of described for step (1) sterilization skimmed milk or filter wash are concentrated, spraying dry.
2. method as claimed in claim 1, it is characterized in that, described raw milk is fresh milk or reconstituted milk, and described fresh milk is preferably raw milk.
3. method as claimed in claim 1, it is characterized in that, in described raw milk, the content of protein is 3.0-3.5%; And/or the content of fat is 3.5-4.2% in described raw milk; And/or the content of lactose is 4.0-4.95% in described raw milk; And/or the content of ash content is 0.6-0.8% in described raw milk, described percentage is the mass percent accounting for raw milk gross mass.
4. method as claimed in claim 1, it is characterized in that, the mass ratio of described natrium citricum and sodium pyrophosphate is 1: 1-3: 2; The mass ratio of described natrium citricum and tertiary sodium phosphate is 3: 7-1: 1; The mass ratio of described sodium pyrophosphate and tertiary sodium phosphate is 4: 1.
5. method as claimed in claim 1, it is characterized in that, in described step (1), described degreasing is centrifugal degreasing.
6. method as claimed in claim 4, it is characterized in that, the temperature of described degreasing is 40-60 DEG C; And/or the centrifugal rotating speed of described degreasing is 7000-12000 rev/min; And/or the centrifugal feed rate of described degreasing is 90-120 l/h.
7. method as claimed in claim 1, is characterized in that, adjust pH described in described step (1) 1 mol/L NaOH or HCl standard liquid regulate; And/or described pH value is 5.5-6.0; And/or the temperature of described stirring is 50-53 DEG C; And/or the rotating speed of described stirring is 50-80 rev/min; And/or the time of described stirring is 5-8 minute; And/or the temperature of described sterilization is 130-140 DEG C; And/or the time of described sterilization is 3-5 second.
8. method as claimed in claim 1, it is characterized in that, described in described step (2), the molecular cut off of the filter membrane of ultrafiltration is 5-30kDa; And/or the filter membrane of described ultrafiltration is regenerated cellulose film; And/or the temperature of described ultrafiltration is 10-40 DEG C; And/or the pressure of described ultrafiltration is 1.5 × 10 5-3 × 10 5handkerchief; And/or the cycles of concentration of described ultrafiltration is concentrated 3-7 times; And/or described filter wash is concentrated to be comprised: fill in the trapped fluid of described ultrafiltration with the isopyknic deionized water of permeate after ultrafiltration concentration further, repeat 2-4 time; And/or described evaporation and concentration is film vacuum evaporation and concentration; And/or described spraying dry adopts vertical spray drying tower to carry out; And/or described spray-dired EAT is 110-140 DEG C; And/or described spray-dired temperature of outgoing air is 60-90 DEG C; And/or described spray-dired pressure is 0.8-1.2bar; And/or described spray-dired feed rate is 0.6-1.4 kg/hr.
9. method as claimed in claim 8, it is characterized in that, the temperature of described film vacuum evaporation and concentration is 60-70 DEG C.
10. a lactoprotein concentrate for high stability, is characterized in that, it is according to as described in any one of claim 1-9 obtained by method.
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