CN106259957A - A kind of lyophilizing donkey milk powder and preparation method thereof - Google Patents

A kind of lyophilizing donkey milk powder and preparation method thereof Download PDF

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Publication number
CN106259957A
CN106259957A CN201610742362.7A CN201610742362A CN106259957A CN 106259957 A CN106259957 A CN 106259957A CN 201610742362 A CN201610742362 A CN 201610742362A CN 106259957 A CN106259957 A CN 106259957A
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donkey milk
temperature
lyophilizing
sterilization
donkey
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张明
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Xinjiang Kunlun Natural Food Engineering Co Ltd
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Xinjiang Kunlun Natural Food Engineering Co Ltd
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Priority to CN201610742362.7A priority Critical patent/CN106259957A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C9/00Milk preparations; Milk powder or milk powder preparations
    • A23C9/16Agglomerating or granulating milk powder; Making instant milk powder; Products obtained thereby
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23CDAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; MAKING THEREOF
    • A23C1/00Concentration, evaporation or drying
    • A23C1/06Concentration by freezing out the water
    • A23C1/08Freeze-drying

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)

Abstract

Open a kind of lyophilizing donkey milk powder of the present invention and preparation method thereof, making frost donkey milk by fresh donkey milk, sterilization temperature is 72 DEG C 85 DEG C, temperature retention time 15s 45s, at vacuum 0.07MPa 0.085MPa, temperature is, at 50 DEG C 65 DEG C, donkey milk is concentrated into density at 1.04kg/m3‑1.08kg/m3In the range of, temperature is down to 50 DEG C 30 DEG C, in vacuum less than under 200Pa, the speed of 2 DEG C 4.5 DEG C of the most averagely heating up with material progressively heats lyophilized plate and rises to 40 DEG C to donkey milk temperature, lyophilised preparation lyophilizing donkey milk powder, confirm through functional trial, causing the mice suffering from diabetes to have reduction blood glucose effect to by STZ, in serum, SOD and GSH-Px activity is significantly improved, and Content of MDA significantly reduces, serum TG content decreases, and has wide applicability.

Description

A kind of lyophilizing donkey milk powder and preparation method thereof
Technical field
The invention belongs to the technical field of milk powder producing technology, more specifically, the present invention relates to a kind of lyophilizing donkey milk powder system Make the technical field of method.
Background technology
Along with the raising day by day of people's life level, the food resource of rich in nutritive value, natural nuisance-free is needed by people Ask the most urgent.Donkey milk as a kind of low fat, low cholesterol, high calcium, beauty treatment, the natural dairy of defying age, to the heart of human body, The multiple organs such as stomach, spleen, lung, liver, prostate have health-care effect, and its nutritional labeling ratio, close to the 99% of human milk, is referred to as Close to the Ruzhong treasure of breast milk, in donkey milk, calcium phosphorus ration is 1.77:1, and the 2:1 of human milk is very much like, easily absorbs, donkey Containing the several amino acids of needed by human body in milk, essential fatty acid content is higher, additionally, rich in trace element in donkey milk Selenium, for 5.2 times of milk, belongs to natural selenium-rich food, according to research reports, containing substantial amounts of epithelial cell growth factor in donkey milk EGF, has and improves effect that body immunity is built up one's resistance to disease.
Vacuum lyophilization is called for short lyophilizing, is that wet stock or solution are frozen into solid-state at a lower temperature, then exists Make moisture therein be directly sublimed into gaseous state without liquid under vacuum, finally make the dry technology of material dewatering.
Owing to the number of animals raised of the donkey that gives milk at present is less, the phase of giving milk is shorter, and the culturing area of donkey more disperses, and adds region Many unfavorable factors such as reason, new fresh donkey milk cannot meet the demand in market, and donkey milk powder then arises at the historic moment.Traditional donkey milk powder Hot-working production method production efficiency is low, and power consumption is high, destroys part nutritional labeling in donkey milk, and containing additive, does not meets The demand of natural environmental-protective dairy market.Therefore, the manufacture method of a kind of suitable donkey milk powder is needed badly.
Summary of the invention
For deficiency and the problem of existence of prior art present situation, in order to solve the problems referred to above, the invention provides one Lyophilizing donkey milk powder manufacture method, compared with prior art, a kind of lyophilizing donkey milk powder manufacture method production efficiency that the present invention provides High, without adding, the donkey milk powder uniform color produced, be creamy white or light yellow, loose porous, without caking, local flavor with fresh Lac Equi Asini is essentially identical, confirms through functional trial, causes the mice suffering from diabetes to have reduction blood glucose effect, in serum to by STZ SOD and GSH-Px activity is significantly improved, and Content of MDA significantly reduces, and serum TG content decreases, and has extensively Practicality.
A kind of lyophilizing donkey milk powder manufacture method that the present invention provides, the concrete techniques below step that uses:
(1) storage of raw material: the use sterile filling car fresh pollution-free donkey milk of collection, sterilization treatment 300s under 200MPa, Preserve at-30 DEG C 0 DEG C, form frost donkey milk;
(2) raw material ice pretreatment: aseptic cleaning ice can, adds frost donkey milk, sealing ice can, starts stirring Device, stirs 10min-20min with the rotating speed of 200r/min-300r/min;
(3) ice is changed: be passed through hot water or vapours by liquid heating or steam heating to the interlayer circulation changing ice can Change ice can being heated to freeze donkey milk melt completely, the donkey milk temperature after heating controls at 50 DEG C-70 DEG C;
(4) emulsifying: aseptic cleaning colloid mill, the donkey milk after changing ice sucks colloid mill by sanitary pump, and colloid mill operates Cross homogenizer after 3min and proceed to storage tank;
(5) sterilization: be 0.15MPa-0.3MPa at pressure, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and send Material pipe pasteurization to leaving water temperature 85 DEG C-98 DEG C, return water temperature reach more than 60 DEG C, the donkey milk in storage tank is pumped into plate Formula sterilization machine sterilizes, and the sterilization temperature of board-like sterilization machine sterilization is 72 DEG C-85 DEG C, temperature retention time 15s-45s, the donkey after sterilization Milk, is directly accessed freeze dryer quantitative automatic feeding device sabot and rinses 5min's for lyophilizing or access through 90 DEG C of heat water-sprayings For concentrating in intermediate storage tank;
(6) concentrate: be 0.15MPa-0.3MPa at pressure, clean and thickener and milk are circulated when being 98 DEG C with sterilization temperature Pipeline pasteurization reaches 80 DEG C to water temperature in contracting machine, constant temperature 5min, in vacuum-0.07MPa-0.085MPa, temperature It is, at 50 DEG C-65 DEG C, donkey milk is concentrated into density at 1.04kg/m3-1.08kg/m3In the range of;
(7) freeze dryer charging: the donkey milk after sterilization or concentration is accessed freeze dryer quantitative automatic feeding device dress lyophilized plate, Sabot thickness uniformity;
(8) pre-freeze: start freeze dryer refrigeration compressor, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-50 DEG C--and 30 DEG C, continue to use air-cooled water-cooled joint refrigeration to continue refrigeration 1h-3h, pre-freeze time < 6h;
(9) lyophilizing: in vacuum less than under 200Pa, the speed of 2 DEG C-4.5 DEG C of the most averagely heating up with material progressively adds Hot lyophilized plate rises to 40 DEG C to donkey milk temperature, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, at 3h Within temperature of charge risen to 60 DEG C-70 DEG C be incubated again, fidelity sky 2h-4h, obtain lyophilizing donkey milk powder, be cooled to room temperature;
(10) test package: sampling inspection donkey milk powder be creamy white or light yellow, loose porous, without caking, local flavor with new After fresh Lac Equi Asini is essentially identical, by donkey milk powder by every bag of 20g or 10g metering pack on powder packing machine, pack with vacuum seal Machine automatic vacuum, adding hot-seal, mounted box packs, and preserves at 0-25 DEG C.
Change ice can as described in above-mentioned steps (2) and (3), including tank body and supporting leg, supporting leg is welded on the lower section of tank body, tank Arranging material liquid outlet and air vent below body, tank wall side arranges air inlet, and tank body is provided above charging aperture and observation window, Tank body is spindle, and inside is divided into interlayer and interior room by dividing plate, and tank interior arranges agitator, and agitator includes puddler, stirs Mixing that dish and paddle, puddler and agitator disk are vertical to be correspondingly arranged, paddle is evenly distributed on agitator disk.
The change ice can that the present invention provides, interlayer is connected with air inlet and gas outlet.
The change ice can that the present invention provides, paddle is quant shape, the orthogonal setting of adjacent paddle.
Use the lyophilizing donkey milk powder that manufacture method described above makes, be creamy white or light yellow, loose porous, without knot Block, local flavor are essentially identical with fresh Lac Equi Asini, confirm through functional trial, cause the mice suffering from diabetes to have reduction blood to by STZ Sugar effect, in serum, SOD and GSH-Px activity is significantly improved, and Content of MDA significantly reduces, and serum TG content is Reduce.
The technical scheme using the present invention to provide can reach following beneficial effect:
A kind of lyophilizing donkey milk powder manufacture method that the present invention provides, makes work through orthogonal test and response phase method assay optimization Skill, a kind of lyophilizing donkey milk powder manufacture method production efficiency that the present invention provides is high, nothing is added, and the donkey milk powder color and luster produced is equal Even, be creamy white or light yellow, loose porous, without caking, local flavor essentially identical with fresh Lac Equi Asini, through functional trial confirmation, Causing the mice suffering from diabetes to have reduction blood glucose effect to by STZ, in serum, SOD and GSH-Px activity is significantly improved, blood Clear MDA content significantly reduces, and serum TG content decreases, and has wide applicability.
Accompanying drawing illustrates:
Fig. 1 is shown as precooling temperature and continues the cooling time response surface curve chart to lyophilizing donkey milk powder sensory evaluation.
Fig. 2 is shown as precooling temperature and the programming rate response surface curve chart to lyophilizing donkey milk powder sensory evaluation per hour.
Fig. 3 is shown as precooling temperature and the warming temperature response surface curve chart to lyophilizing donkey milk powder sensory evaluation.
Fig. 4 is shown as continuing cooling time and the programming rate response surface curve to lyophilizing donkey milk powder sensory evaluation per hour Figure.
Fig. 5 is shown as continuing cooling time and the warming temperature response surface curve chart to lyophilizing donkey milk powder sensory evaluation.
Fig. 6 is shown as programming rate and the warming temperature response surface curve chart to lyophilizing donkey milk powder sensory evaluation per hour.
Fig. 7 is shown as the change ice can structural representation that the present invention provides.
Fig. 8 is shown as the agitator structure schematic diagram that the present invention provides.
In Fig. 7 and Fig. 8,1 supporting leg, 2 tank bodies, 21 air inlets, 22 observation windows, 23 charging apertures, 24 stirrings Device, 241 agitator disks, 242 paddles, 243 puddlers, 25 air vents, 26 material liquid outlets, in 3 room, 4 folders Layer.
Detailed description of the invention
1-8 and embodiment below in conjunction with the accompanying drawings, is described in further detail the detailed description of the invention of the present invention, but this Bright it is not limited to following embodiment.
Donkey milk in the present invention can be bought by public channel, the sterile filling car of employing, agitator, colloid mill, health Pump, board-like sterilization machine, storage tank, feed pipe, thickener, milk circulating line, freeze dryer and powder packing machine etc. are this area Common equipment.
All material, reagent and the instrument selected in the present invention are all well known in the art, but are not intended to the reality of the present invention Executing, other reagent more well known in the art and equipment are applied both to the enforcement of implementation below of the present invention.
Embodiment one: the manufacture method of lyophilizing donkey milk powder
Use sterile filling car to collect fresh pollution-free donkey milk, sterilization treatment 300s under 200MPa, protect at-30 DEG C Deposit, form frost donkey milk;Aseptic cleaningization ice can, adds frost donkey milk, sealing ice can, starts agitator, with 200r/ The rotating speed stirring 10min of min;It is passed through hot water or heat steaming to the interlayer circulation changing ice can by liquid heating or steam heating Vapour is heated to freezing donkey milk to change ice can and melts completely, and the donkey milk temperature after heating controls at 50 DEG C;Aseptic cleaning colloid mill, will Change the donkey milk after ice and suck colloid mill by sanitary pump, cross homogenizer after colloid mill operating 3min and proceed to storage tank;At pressure it is 0.15MPa, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe pasteurization to leaving water temperature in 85 DEG C, times Coolant-temperature gage reaches more than 60 DEG C, and the donkey milk in storage tank pumps into the sterilization of board-like sterilization machine, the sterilization temperature of board-like sterilization machine sterilization Degree is 72 DEG C, temperature retention time 15s, the donkey milk after sterilization, is directly accessed freeze dryer quantitative automatic feeding device sabot and makes for lyophilizing With or access in 90 DEG C of heat water-sprayings rinse the intermediate storage tank of 5min for concentration;It is 0.15MPa at pressure, cleans and kill When bacterium temperature is 98 DEG C, thickener and milk circulating line pasteurization are reached 80 DEG C to water temperature in contracting machine, constant temperature 5min, At vacuum-0.07MPa, temperature is, at 50 DEG C, donkey milk is concentrated into density at 1.04kg/m3In the range of;After sterilizing or concentrate Donkey milk access freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot thickness uniformity;Start freeze dryer refrigerant compression Machine, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-50 DEG C, continues to use air-cooled water-cooled joint refrigeration to continue refrigeration 1h, in advance Freeze the time < 6h;In vacuum less than under 200Pa, the speed of 2 DEG C of the most averagely heating up with material progressively heats lyophilized plate to donkey Milk temperature rises to 40 DEG C, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, by material temperature within 3h Degree rise to 60 DEG C be incubated again, fidelity sky 2h, obtain lyophilizing donkey milk powder, be cooled to room temperature;Sampling inspection donkey milk powder be creamy white or After light yellow, loose porous, nothing caking, local flavor are essentially identical with fresh Lac Equi Asini, by donkey milk powder by every bag on powder packing machine 20g or 10g measures pack, by vacuum sealing packing machine automatic vacuum, adds hot-seal, and mounted box packs, and preserves at 0 DEG C.
Embodiment two: the manufacture method of lyophilizing donkey milk powder
Use sterile filling car to collect fresh pollution-free donkey milk, sterilization treatment 300s under 200MPa, preserve at 0 DEG C, Form frost donkey milk;Aseptic cleaningization ice can, adds frost donkey milk, sealing ice can, starts agitator, with 300r/min Rotating speed stirring 20min;It is passed through hot water or vapours to the interlayer circulation changing ice can by liquid heating or steam heating Change ice can being heated to freeze donkey milk melt completely, the donkey milk temperature after heating controls at 70 DEG C;Aseptic cleaning colloid mill, generalization Donkey milk after ice sucks colloid mill by sanitary pump, crosses homogenizer and proceed to storage tank after colloid mill operating 3min;At pressure it is 0.3MPa, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe pasteurization to leaving water temperature in 98 DEG C, times Coolant-temperature gage reaches more than 60 DEG C, and the donkey milk in storage tank pumps into the sterilization of board-like sterilization machine, the sterilization temperature of board-like sterilization machine sterilization Degree is 85 DEG C, temperature retention time 45s, the donkey milk after sterilization, is directly accessed freeze dryer quantitative automatic feeding device sabot and makes for lyophilizing With or access in 90 DEG C of heat water-sprayings rinse the intermediate storage tank of 5min for concentration;It is 0.3MPa at pressure, cleans and kill When bacterium temperature is 98 DEG C, thickener and milk circulating line pasteurization are reached 80 DEG C to water temperature in contracting machine, constant temperature 5min, In vacuum 0.085MPa, temperature is, at 65 DEG C, donkey milk is concentrated into density at 1.08kg/m3In the range of;After sterilizing or concentrate Donkey milk access freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot thickness uniformity;Start freeze dryer refrigerant compression Machine, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-30 DEG C, continues to use air-cooled water-cooled joint refrigeration to continue refrigeration 3h, in advance Freeze the time < 6h;In vacuum less than under 200Pa, the speed of 4.5 DEG C of the most averagely heating up with material progressively heats lyophilized plate extremely Donkey milk temperature rises to 40 DEG C, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, by material within 3h Temperature rise to 70 DEG C be incubated again, fidelity sky 4h, obtain lyophilizing donkey milk powder, be cooled to room temperature;Sampling inspection donkey milk powder is creamy white Or light yellow, loose porous, without caking, local flavor and fresh Lac Equi Asini essentially identical after, by donkey milk powder by every on powder packing machine Bag 20g or 10g metering pack, by vacuum sealing packing machine automatic vacuum, adds hot-seal, and mounted box packs, and preserves at 25 DEG C.
Embodiment three: the manufacture method of lyophilizing donkey milk powder
Use sterile filling car to collect fresh pollution-free donkey milk, sterilization treatment 300s under 200MPa, preserve at-5 DEG C, Form frost donkey milk;Aseptic cleaningization ice can, adds frost donkey milk, sealing ice can, starts agitator, with 280r/min Rotating speed stirring 18min;It is passed through hot water or vapours to the interlayer circulation changing ice can by liquid heating or steam heating Change ice can being heated to freeze donkey milk melt completely, the donkey milk temperature after heating controls at 55 DEG C;Aseptic cleaning colloid mill, generalization Donkey milk after ice sucks colloid mill by sanitary pump, crosses homogenizer and proceed to storage tank after colloid mill operating 3min;At pressure it is 0.18MPa, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe pasteurization to leaving water temperature in 89 DEG C, times Coolant-temperature gage reaches more than 60 DEG C, and the donkey milk in storage tank pumps into the sterilization of board-like sterilization machine, the sterilization temperature of board-like sterilization machine sterilization Degree is 80 DEG C, temperature retention time 20s, the donkey milk after sterilization, is directly accessed freeze dryer quantitative automatic feeding device sabot and makes for lyophilizing With or access in 90 DEG C of heat water-sprayings rinse the intermediate storage tank of 5min for concentration;It is 0.25MPa at pressure, cleans and kill When bacterium temperature is 98 DEG C, thickener and milk circulating line pasteurization are reached 80 DEG C to water temperature in contracting machine, constant temperature 5min, At vacuum-0.02MPa, temperature is, at 60 DEG C, donkey milk is concentrated into density at 1.05kg/m3In the range of;After sterilizing or concentrate Donkey milk access freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot thickness uniformity;Start freeze dryer refrigerant compression Machine, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-45 DEG C, continues to use air-cooled water-cooled joint refrigeration to continue refrigeration 2h, in advance Freeze the time < 6h;In vacuum less than under 200Pa, the speed of 3 DEG C of the most averagely heating up with material progressively heats lyophilized plate to donkey Milk temperature rises to 40 DEG C, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, by material temperature within 3h Degree rise to 62 DEG C be incubated again, fidelity sky 3h, obtain lyophilizing donkey milk powder, be cooled to room temperature;Sampling inspection donkey milk powder be creamy white or After light yellow, loose porous, nothing caking, local flavor are essentially identical with fresh Lac Equi Asini, by donkey milk powder by every bag on powder packing machine 20g or 10g measures pack, by vacuum sealing packing machine automatic vacuum, adds hot-seal, and mounted box packs, and preserves at 22 DEG C.
Embodiment four: the manufacture method of lyophilizing donkey milk powder
Use sterile filling car to collect fresh pollution-free donkey milk, sterilization treatment 300s under 200MPa, protect at-25 DEG C Deposit, form frost donkey milk;Aseptic cleaningization ice can, adds frost donkey milk, sealing ice can, starts agitator, with 220r/ The rotating speed stirring 16min of min;It is passed through hot water or heat steaming to the interlayer circulation changing ice can by liquid heating or steam heating Vapour is heated to freezing donkey milk to change ice can and melts completely, and the donkey milk temperature after heating controls at 65 DEG C;Aseptic cleaning colloid mill, will Change the donkey milk after ice and suck colloid mill by sanitary pump, cross homogenizer after colloid mill operating 3min and proceed to storage tank;At pressure it is 0.27MPa, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe pasteurization to leaving water temperature in 92 DEG C, times Coolant-temperature gage reaches more than 60 DEG C, and the donkey milk in storage tank pumps into the sterilization of board-like sterilization machine, the sterilization temperature of board-like sterilization machine sterilization Degree is 76 DEG C, temperature retention time 30s, the donkey milk after sterilization, is directly accessed freeze dryer quantitative automatic feeding device sabot and makes for lyophilizing With or access in 90 DEG C of heat water-sprayings rinse the intermediate storage tank of 5min for concentration;It is 0.2MPa at pressure, cleans and kill When bacterium temperature is 98 DEG C, thickener and milk circulating line pasteurization are reached 80 DEG C to water temperature in contracting machine, constant temperature 5min, In vacuum 0.03MPa, temperature is, at 60 DEG C, donkey milk is concentrated into density at 1.05kg/m3In the range of;After sterilizing or concentrate Donkey milk access freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot thickness uniformity;Start freeze dryer refrigerant compression Machine, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-40 DEG C, continues to use air-cooled water-cooled joint refrigeration to continue refrigeration 2.6h, Pre-freeze time < 6h;In vacuum less than under 200Pa, the speed of 4 DEG C of the most averagely heating up with material progressively heats lyophilized plate extremely Donkey milk temperature rises to 40 DEG C, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, by material within 3h Temperature rise to 66 DEG C be incubated again, fidelity sky 3.5h, obtain lyophilizing donkey milk powder, be cooled to room temperature;Sampling inspection donkey milk powder is milky white Color or light yellow, loose porous, without caking, local flavor and fresh Lac Equi Asini essentially identical after, donkey milk powder is pressed by powder packing machine Every bag of 20g or 10g metering pack, by vacuum sealing packing machine automatic vacuum, adds hot-seal, and mounted box packs, and stores at 18 DEG C Hide.
Embodiment five: the manufacture method of lyophilizing donkey milk powder
Use sterile filling car to collect fresh pollution-free donkey milk, sterilization treatment 300s under 200MPa, protect at-15 DEG C Deposit, form frost donkey milk;Aseptic cleaningization ice can, adds frost donkey milk, sealing ice can, starts agitator, with 250r/ The rotating speed stirring 12min of min;It is passed through hot water or heat steaming to the interlayer circulation changing ice can by liquid heating or steam heating Vapour is heated to freezing donkey milk to change ice can and melts completely, and the donkey milk temperature after heating controls at 60 DEG C;Aseptic cleaning colloid mill, will Change the donkey milk after ice and suck colloid mill by sanitary pump, cross homogenizer after colloid mill operating 3min and proceed to storage tank;At pressure it is 0.2MPa, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe pasteurization to leaving water temperature in 96 DEG C, times Coolant-temperature gage reaches more than 60 DEG C, and the donkey milk in storage tank pumps into the sterilization of board-like sterilization machine, the sterilization temperature of board-like sterilization machine sterilization Degree is 85 DEG C, temperature retention time 40s, the donkey milk after sterilization, is directly accessed freeze dryer quantitative automatic feeding device sabot and makes for lyophilizing With or access in 90 DEG C of heat water-sprayings rinse the intermediate storage tank of 5min for concentration;It is 0.16MPa at pressure, cleans and kill When bacterium temperature is 98 DEG C, thickener and milk circulating line pasteurization are reached 80 DEG C to water temperature in contracting machine, constant temperature 5min, In vacuum 0.07MPa, temperature is, at 62 DEG C, donkey milk is concentrated into density at 1.06kg/m3In the range of;After sterilizing or concentrate Donkey milk access freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot thickness uniformity;Start freeze dryer refrigerant compression Machine, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-35 DEG C, continues to use air-cooled water-cooled joint refrigeration to continue refrigeration 1.2h, Pre-freeze time < 6h;In vacuum less than under 200Pa, the speed of 3.5 DEG C of the most averagely heating up with material progressively heats lyophilized plate Rise to 40 DEG C to donkey milk temperature, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, by thing within 3h Material temperature degree rise to 69 DEG C be incubated again, fidelity sky 2.5h, obtain lyophilizing donkey milk powder, be cooled to room temperature;Sampling inspection donkey milk powder is breast After white or light yellow, loose porous, nothing caking, local flavor are essentially identical with fresh Lac Equi Asini, by donkey milk powder on powder packing machine By every bag of 20g or 10g metering pack, by vacuum sealing packing machine automatic vacuum, adding hot-seal, mounted box packs, at 10 DEG C Storage.
Embodiment six: the manufacture method of lyophilizing donkey milk powder
A kind of lyophilizing donkey milk powder manufacture method, the concrete techniques below step that uses:
(1) storage of raw material: the use sterile filling car fresh pollution-free donkey milk of collection, sterilization treatment 300s under 200MPa, Preserve at-30 DEG C 0 DEG C, form frost donkey milk;
(2) raw material ice pretreatment: aseptic cleaning ice can, adds frost donkey milk, sealing ice can, starts stirring Device, stirs 10min-20min with the rotating speed of 200r/min-300r/min;
(3) ice is changed: be passed through hot water or vapours by liquid heating or steam heating to the interlayer circulation changing ice can Change ice can being heated to freeze donkey milk melt completely, the donkey milk temperature after heating controls at 50 DEG C-70 DEG C;
(4) emulsifying: aseptic cleaning colloid mill, the donkey milk after changing ice sucks colloid mill by sanitary pump, and colloid mill operates Cross homogenizer after 3min and proceed to storage tank;
(5) sterilization: be 0.15MPa-0.3MPa at pressure, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and send Material pipe pasteurization to leaving water temperature 85 DEG C-98 DEG C, return water temperature reach more than 60 DEG C, the donkey milk in storage tank is pumped into plate Formula sterilization machine sterilizes, and the sterilization temperature of board-like sterilization machine sterilization is 72 DEG C-85 DEG C, temperature retention time 15s-45s, the donkey after sterilization Milk, is directly accessed freeze dryer quantitative automatic feeding device sabot and rinses 5min's for lyophilizing or access through 90 DEG C of heat water-sprayings For concentrating in intermediate storage tank;
(6) concentrate: be 0.15MPa-0.3MPa at pressure, clean and thickener and milk are circulated when being 98 DEG C with sterilization temperature Pipeline pasteurization reaches 80 DEG C to water temperature in contracting machine, constant temperature 5min, in vacuum-0.07MPa-0.085MPa, temperature It is, at 50 DEG C-65 DEG C, donkey milk is concentrated into density at 1.04kg/m3-1.08kg/m3In the range of;
(7) freeze dryer charging: the donkey milk after sterilization or concentration is accessed freeze dryer quantitative automatic feeding device dress lyophilized plate, Sabot thickness uniformity;
(8) pre-freeze: start freeze dryer refrigeration compressor, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-50 DEG C--and 30 DEG C, continue to use air-cooled water-cooled joint refrigeration to continue refrigeration 1h-3h, pre-freeze time < 6h;
(9) lyophilizing: in vacuum less than under 200Pa, the speed of 2 DEG C-4.5 DEG C of the most averagely heating up with material progressively adds Hot lyophilized plate rises to 40 DEG C to donkey milk temperature, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, at 3h Within temperature of charge risen to 60 DEG C-70 DEG C be incubated again, fidelity sky 2h-4h, obtain lyophilizing donkey milk powder, be cooled to room temperature;
(10) test package: sampling inspection donkey milk powder be creamy white or light yellow, loose porous, without caking, local flavor with new After fresh Lac Equi Asini is essentially identical, by donkey milk powder by every bag of 20g or 10g metering pack on powder packing machine, pack with vacuum seal Machine automatic vacuum, adding hot-seal, mounted box packs, and preserves at 0-25 DEG C.
Embodiment seven: the change ice can that the manufacture method of lyophilizing donkey milk powder uses
See accompanying drawing 7 to accompanying drawing 8, the change ice can as described in above-described embodiment one to embodiment six, including tank body (2) and Lower limb (1), supporting leg (1) is welded on the lower section of tank body (2), and tank body (2) lower section arranges material liquid outlet (26) and air vent (25), tank body Outer wall side arranges air inlet (21), and tank body (2) is provided above charging aperture (23) and observation window (22), tank body (2) in spindle, Inside is divided into interlayer (4) and interior room (3) by dividing plate, and tank body (2) is internal arranges agitator (24), and agitator (24) includes puddler (243), agitator disk (241) and paddle (242), puddler (243) and agitator disk (241) be vertically correspondingly arranged, paddle (242) it is evenly distributed on agitator disk (241).
The change ice can that the present invention provides, interlayer (4) is connected with air inlet (21) and gas outlet (25).
The present invention provide change ice can, paddle (242) in quant shape, adjacent paddle (242) orthogonal setting.
Embodiment eight: the process optimization of lyophilizing donkey milk powder
It is respectively adopted following different technological parameter and prepares lyophilizing donkey milk powder:
Scheme one: in concentration step: concentrate pressure 0.15MPa, vacuum-0.07MPa, temperature 50 C, density 1.04kg/ m3;In pre-freeze and step of freeze drying: precooling temperature-50 DEG C, continue cooling time 1h, promote temperature 2 DEG C, warming temperature 60 per hour ℃。
Scheme two: in concentration step: concentrate pressure 0.3MPa, vacuum 0.085MPa, temperature 65 DEG C, density 1.08kg/ m3;In pre-freeze and step of freeze drying: precooling temperature-30 DEG C, continue cooling time 3h, promote temperature 4.5 DEG C, warming temperature per hour 70℃。
Scheme three: in concentration step: concentrate pressure 0.25MPa, vacuum-0.02MPa, temperature 60 C, density 1.05kg/ m3;In pre-freeze and step of freeze drying: precooling temperature-45 DEG C, continue cooling time 2h, promote temperature 3 DEG C, warming temperature 62 per hour ℃。
Scheme four: in concentration step: concentrate pressure 0.2MPa, vacuum 0.03MPa, temperature 55 DEG C, density 1.07kg/ m3;In pre-freeze and step of freeze drying: precooling temperature-40 DEG C, continue cooling time 2.6h, promote temperature 4 DEG C, warming temperature per hour 66℃。
Scheme five: in concentration step: concentrate pressure 0.16MPa, vacuum 0.07MPa, temperature 62 DEG C, density 1.06kg/ m3;In pre-freeze and step of freeze drying: precooling temperature-35 DEG C, continuing cooling time 1.2h, promote temperature 3.5 DEG C per hour, heat up temperature Spend 69 DEG C.
Lyophilizing donkey milk powder is prepared by the preparation method that five different schemes of above-mentioned offer provide according to embodiment six respectively:
On above-mentioned experiment basis, the lyophilizing donkey milk powder of preparation carries out sensory evaluation, and standard is shown in Table 1.
Table 1: lyophilizing donkey milk powder sensory evaluation scores table
1. orthogonal optimization lyophilizing donkey milk powder processing technology
Design experiment of single factor, probes into concentration pressure, vacuum, temperature in lyophilizing donkey milk powder processing technology concentration step respectively Degree and the density impact on lyophilizing donkey milk powder sensory evaluation.Four factor three horizontal quadratures are carried out real on the basis of experiment of single factor Testing, orthogonal test factor and level are shown in Table 2.
Table 2: orthogonal test factor and water-glass
Orthogonal optimization lyophilizing donkey milk powder processing technology result of the test and analysis in table 3.
Table 3: orthogonal experiments and analysis
By the extreme difference of relatively each index, each influence factor's primary and secondary order is B > A > D > C, i.e. lyophilizing donkey milk powder processing technology In concentration step, vacuum is lyophilizing donkey milk powder sensory evaluation major influence factors, next to that concentrate pressure, density and temperature degree, K1, k2, k3 value according to index each in table 3 and the result of trendgram, determine that each factor optimum level is combined as A1B2C1D2, i.e. Optimization technique in lyophilizing donkey milk powder manufacturing process is: in concentration step, concentration pressure 0.15MPa-0.3MPa, vacuum- 0.07MPa-0.085MPa, temperature 50 C-65 DEG C, density 1.04kg/m3-1.08kg/m3;Preferably, concentrate pressure 0.15MPa, Vacuum 0.0075MPa, temperature 50 C, density 1.06kg/m3
2. response phase method optimizes lyophilizing donkey milk powder processing technology, and experimental factor and level are shown in Table 4:
Table 4: response surface experiments factor and water-glass
Table 5: response surface experiments design and result
Response surface experiments design and result:
Carrying out design of experiment analysis according to Box-Benhnken center combination design principle, it the results are shown in Table 5.Pass through Design Expert8.0.6 uses the method for polynomial fitting to be fitted the experimental data of table 5, obtains sensory evaluation scores R in advance Cold temperature (A), continue cooling time (B), per hour the multinomial regression model of secondary of programming rate (C) and warming temperature (D) be:
R=38.00-1.17A+0.42B-0.92C-0.83D+0.25AB+AC+0.75AD-1.25BC+ 0.25BD- 5.75A2-3.87B2-7.62C2-7.25D2
In response surface analysis, each factor reciprocal action is referring specifically to accompanying drawing 1 to accompanying drawing 6.From orthogonal test and response surface experiments The result optimizing lyophilizing donkey milk powder processing technology understands, and lyophilizing donkey milk powder is: in concentration step, concentrates pressure 0.15MPa- 0.3MPa, vacuum-0.07MPa-0.085MPa, temperature 50 C-65 DEG C, density 1.04kg/m3-1.08kg/m3;Pre-freeze and freezing In dry step, precooling temperature-50 DEG C-30 DEG C, continues cooling time 1-3h, promotes temperature 2-4.5 DEG C, warming temperature per hour 60-75℃。
Embodiment nine: the functional trial of lyophilizing donkey milk powder
Healthy male mice identical for body weight is divided into 5 groups, often group 10.Normal cultivate one week after be all trained by STZ causes the mice suffering from diabetes.One group is as a control group, every day gavage 0.01ml/g normal saline;One group as medicine group, Every day, gavage was by the 125mg/kg metformin hydrochloride solution 0.01ml/g of normal saline;One group as donkey milk group, every day The donkey milk powder of gavage 0.01ml/g present invention offer and the donkey milk of distilled water by volume mass ratio 1:1ml/g mixing;One group of conduct Milk group, every day gavage 0.01ml/g milk;Group, the 125mg/kg of gavage every day above-mentioned donkey milk preparation are combined in last group conduct Metformin hydrochloride solution 0.01ml/g;. every day timing gavage mice once, and, every 3d claims weight to determine continuation gavage Amount. fasting 12h (can't help water) after gavage 35d continuously, blood sampling detection indices.
Table 6: the impact of variant process group activity index each on type 1 diabetes mice
Note: in table, the dosage of each group is 0.01ml/ (g d), and number of animals is 10;Compare with model group, * * p < 0.01, * p < 0.05.
Result: experimental result is shown in Table 6, compares with matched group, and lyophilizing donkey milk powder prepared by the present invention causes suffering from sugar to by STZ The mice of urine disease has reduction blood glucose effect, and in serum, SOD and GSH-Px activity is significantly improved, and Content of MDA significantly drops Low, serum TG content decreases.
A kind of lyophilizing donkey milk powder manufacture method that the present invention provides, makes work through orthogonal test and response phase method assay optimization Skill, a kind of lyophilizing donkey milk powder manufacture method production efficiency that the present invention provides is high, nothing is added, and the donkey milk powder color and luster produced is equal Even, be creamy white or light yellow, loose porous, without caking, local flavor essentially identical with fresh Lac Equi Asini, through functional trial confirmation, Causing the mice suffering from diabetes to have reduction blood glucose effect to by STZ, in serum, SOD and GSH-Px activity is significantly improved, blood Clear MDA content significantly reduces, and serum TG content decreases, and has wide applicability.
As it has been described above, the present invention can preferably be realized, the above embodiments are only to the present invention side of being preferable to carry out Formula is described, and is not defined the scope of the present invention, and on the premise of designing spirit without departing from the present invention, this area is general Lead to various deformation and improvement that technical scheme is made by technical staff, the protection domain that present invention determine that all should be fallen into In.

Claims (5)

1. a lyophilizing donkey milk powder manufacture method, the concrete techniques below step that uses:
(1) storage of raw material: collecting fresh pollution-free donkey milk with sterile filling car, sterilization treatment 300s under 200MPa, in-30 Preserve at DEG C 0 DEG C, form frost donkey milk;
(2) raw material ice pretreatment: aseptic cleaning ice can, adds frost donkey milk, sealing ice can, starts agitator, 10min-20min is stirred with the rotating speed of 200r/min-300r/min;
(3) ice is changed: be passed through hot water or vapours to change by liquid heating or steam heating to the interlayer circulation changing ice can Ice can is heated to freezing donkey milk and melts completely, and the donkey milk temperature after heating controls at 50 DEG C-70 DEG C;
(4) emulsifying: aseptic cleaning colloid mill, the donkey milk after changing ice sucks colloid mill, colloid mill operating 3min by sanitary pump Rear homogenizer of crossing proceeds to storage tank;
(5) sterilization: be 0.15MPa-0.3MPa at pressure, cleans when being 98 DEG C with sterilization temperature board-like sterilization machine and feed pipe Pasteurization to leaving water temperature 85 DEG C-98 DEG C, return water temperature reach more than 60 DEG C, the donkey milk in storage tank is pumped into board-like killing Bacterium machine sterilizes, and the sterilization temperature of board-like sterilization machine sterilization is 72 DEG C-85 DEG C, temperature retention time 15s-45s, the donkey milk after sterilization, directly Access freeze dryer quantitative automatic feeding device sabot and rinse the centre of 5min for lyophilizing or access through 90 DEG C of heat water-sprayings For concentrating in storage tank;
(6) concentrate: be 0.15MPa-0.3MPa at pressure, clean when being 98 DEG C with sterilization temperature thickener and milk circulating line Pasteurization reaches 80 DEG C to water temperature in contracting machine, constant temperature 5min, and at vacuum-0.07MPa-0.085 MPa, temperature is 50 At DEG C-65 DEG C, donkey milk is concentrated into density at 1.04kg/m3-1.08kg/m3In the range of;
(7) freeze dryer charging: the donkey milk after sterilization or concentration is accessed freeze dryer quantitative automatic feeding device dress lyophilized plate, sabot Thickness uniformity;
(8) pre-freeze: start freeze dryer refrigeration compressor, uses oily cold refrigeration to freeze to donkey milk, and temperature is down to-50 DEG C--and 30 DEG C, Continue to use air-cooled water-cooled joint refrigeration to continue refrigeration 1h-3h, pre-freeze time < 6h;
(9) lyophilizing: in vacuum less than under 200Pa, the speed of 2 DEG C-4.5 DEG C of the most averagely heating up with material progressively heats freezes Dry pan rises to 40 DEG C to donkey milk temperature, simultaneously freeze dryer catch reservoir by catch water pipe collecting distillation steam, within 3h Temperature of charge is risen to 60 DEG C-70 DEG C be incubated again, fidelity sky 2h-4h, obtain lyophilizing donkey milk powder, be cooled to room temperature;
(10) test package: sampling inspection donkey milk powder is creamy white or light yellow, loose porous, without caking, local flavor and fresh donkey After breast is essentially identical, by donkey milk powder by metering pack on powder packing machine, with vacuum sealing packing machine automatic vacuum, heating Sealing, mounted box packs, and preserves at 0-25 DEG C.
The change ice can used in a kind of lyophilizing donkey milk powder manufacture method the most as claimed in claim 1, it is characterised in that described Changing ice can and include tank body and supporting leg, supporting leg is welded on the lower section of tank body, arranges material liquid outlet and air vent, outside tank body below tank body Wall side arranges air inlet, and tank body is provided above charging aperture and observation window, and tank body is spindle, internal by dividing plate be divided into interlayer and Interior room, tank interior arranges agitator, and agitator includes that puddler, agitator disk and paddle, puddler and agitator disk are vertical right Should arrange, paddle is evenly distributed on agitator disk.
The change ice can used in a kind of lyophilizing donkey milk powder manufacture method the most as claimed in claim 2, it is characterised in that described Interlayer is connected with air inlet and gas outlet.
The change ice can used in a kind of lyophilizing donkey milk powder manufacture method the most as claimed in claim 2, it is characterised in that described Paddle is quant shape, the orthogonal setting of adjacent paddle.
Lyophilizing donkey milk powder prepared by a kind of lyophilizing donkey milk powder manufacture method the most as claimed in claim 1.
CN201610742362.7A 2016-08-28 2016-08-28 A kind of lyophilizing donkey milk powder and preparation method thereof Pending CN106259957A (en)

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CN108308280A (en) * 2018-03-07 2018-07-24 西北师范大学 A method of preparing donkey milk freeze-dried powder under cryogenic
CN109169925A (en) * 2018-09-28 2019-01-11 东阿阿胶股份有限公司 Purposes of the donkey milk in preparation adjuvant treatment health-care product for curing diabetes
CN109463453A (en) * 2018-10-29 2019-03-15 东阿阿胶股份有限公司 A kind of preparation method of probiotics donkey milk powder
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CN110353048A (en) * 2019-08-27 2019-10-22 河北天烨食品科技有限公司 A kind of efficiently freeze-drying milk powder processing method
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CN110448571A (en) * 2019-09-06 2019-11-15 新疆医科大学 Purposes of the donkey milk in the diabetes B for preventing and improving high fat diet induction
CN111076504A (en) * 2019-12-27 2020-04-28 通标标准技术服务(天津)有限公司 Method for freeze-drying heat-sensitive substance
CN111449139A (en) * 2020-04-08 2020-07-28 杭州联星贸易有限公司 Formula donkey milk powder containing N-acetylneuraminic acid
CN112358538A (en) * 2020-11-09 2021-02-12 甘肃黑驴王子生物科技有限公司 Enrichment method of epidermal growth factor in fresh donkey milk
CN114111231A (en) * 2021-11-17 2022-03-01 东富龙科技集团股份有限公司 Continuous freeze-drying equipment of developments system ice particle

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