CN1739397A - Production process of freeze dried sea cucumber, sea cucumber capsule and sea cucumber mucopolysaccharide capsule - Google Patents
Production process of freeze dried sea cucumber, sea cucumber capsule and sea cucumber mucopolysaccharide capsule Download PDFInfo
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- CN1739397A CN1739397A CNA2004100503098A CN200410050309A CN1739397A CN 1739397 A CN1739397 A CN 1739397A CN A2004100503098 A CNA2004100503098 A CN A2004100503098A CN 200410050309 A CN200410050309 A CN 200410050309A CN 1739397 A CN1739397 A CN 1739397A
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Abstract
The present invention relates to food production, and is especially production process of serial sea cucumber food products. The production process of freeze dried sea cucumber includes the steps of processing material, soaking, pre-freezing through fast freezing at -50 to -80 DEG C until complete freezing, and freeze drying. The production process of dried sea cucumber capsule includes the steps of processing material, soaking, pre-freezing, freeze drying, low temperature superfine crushing, and encapsulating. The production process of sea cucumber mucopolysaccharide capsule includes the steps of processing material, soaking, low temperature superfine crushing and homogenizing, pre-freezing, extracting sea cucumber mucopolysaccharide, low temperature superfine crushing, and packing.
Description
Technical field
The present invention relates to a kind of food deep processing field, particularly a series of beche-de-mer products preparation technologies field.
Background technology
As everyone knows, sea cucumber is one of precious eight product in sea on China's history, and is equally celebrated for their achievements with bird's nest, shark's fin.Its healthy nutritive value is higher, and sea cucumber is rich in plurality of active ingredients simultaneously, has the immunity of enhancing, antitumor action.The crowd of beche-de-mer is in continuous increase.Sea cucumber in the market, main based on traditional dried sea-cucumber.The conventional dry sea cucumber exists complex procedures, destruction and a large amount of nutritional labeling that run off on making, and be subjected to time, the site limitation of strictness during edible cooking, its taste is not as fine and smooth, soft, the elasticity of bright sea cucumber, deliciousness, thereby influenced the nutrition health-care functions of sea cucumber, can not satisfy allegro people's demand.
Summary of the invention
Technical problem to be solved by this invention is to provide and can keeps the original nutritional labeling of fresh sea cucumber, avoids long-time storage, carries inconvenience, substantially improves the preparation technology of sea cucumber nutrient composition at human absorptivity, the freeze-drying sea cucumber of improving its human bioavailability, full holothurian capsule and sea cucumber mucopolysaccharide capsule.
The present invention is raw material with fresh sea cucumber, adopted modern high-new bioscience technology, its product has solved the demand of people to the instant product of sea cucumber, kept the original nutritional labeling of fresh sea cucumber, avoided long-time storage, carried inconvenient problem, improved the sea cucumber nutrient composition the human absorptivity, improved the bioavilability of human body.
Technical solution of the present invention can realize according to following mode:
The preparation technology of freeze-drying sea cucumber is characterized in, carries out successively as follows:
(a) raw material is handled;
(b) immersion treatment;
(c) precooling treatment: the sea cucumber raw material after will cleaning carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(d) freeze-drying is handled;
The product that (d) step can be obtained among the preparation technology of above-mentioned freeze-drying sea cucumber is inserted in the low temperature micronizer and is pulverized.
Among the preparation technology of above-mentioned freeze-drying sea cucumber, before (c) step, can carry out the ultramicro grinding homogenized earlier.
The preparation technology of full holothurian capsule is characterized in, carries out successively as follows:
(1) raw material is handled;
(2) immersion treatment;
(3) precooling treatment: carry out the ultramicro grinding homogenized earlier, the sea cucumber raw material after will cleaning again carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(4) freeze-drying is handled;
(5) low temperature ultramicro grinding;
(6), adopt capsule filling machine to carry out packing with the product in the step (5).Among the preparation technology of above-mentioned full holothurian capsule, described capsule filling machine is the hard shell capsules filling machine.Among the preparation technology of above-mentioned full holothurian capsule, the product in the step (6) is a soft capsule content, and described capsule filling machine is the soft capsule filling machine.
In the preparation technology of above-mentioned full holothurian capsule, the preparation technology of soft capsule content can carry out as follows:
Polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 3～5 minutes, the amplitude 4～8mm of vibration medium; And then full sea cucumber powder added in the pulverizer pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 5～7 minutes, the amplitude 4～8mm of vibration medium make soft capsule content; The weight ratio of above-mentioned full sea cucumber powder, polyethylene glycol (PEG) 4000, Tween 80 is followed successively by 1: 1: 4～6.
The preparation technology of sea cucumber mucopolysaccharide capsule is characterized in, carries out successively as follows:
(1) raw material is handled;
(2) immersion treatment;
(3) precooling treatment: carry out the ultramicro grinding homogenized earlier, the sea cucumber raw material after will cleaning again carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(4) extract sea cucumber mucopolysaccharide;
(5) freeze-drying is handled;
(6) the low temperature ultramicro grinding is handled;
(7), adopt capsule filling machine to carry out packing with the product in the step (6).
Among the preparation technology of above-mentioned sea cucumber mucopolysaccharide capsule, described capsule filling machine is the hard shell capsules filling machine.
Among the preparation technology of above-mentioned sea cucumber mucopolysaccharide capsule, the product in the step (7) is a soft capsule content, and described capsule filling machine is the soft capsule filling machine.
Among the preparation technology of above-mentioned sea cucumber mucopolysaccharide capsule, the preparation technology of soft capsule content is as follows:
Polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 3～5 minutes, the amplitude 4～8mm of vibration medium; And then the sea cucumber mucopolysaccharide powder added in the pulverizer pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 5～7 minutes, the amplitude 4～8mm of vibration medium make soft capsule content; The weight ratio of above-mentioned sea cucumber mucopolysaccharide powder, polyethylene glycol (PEG) 4000, Tween 80 is followed successively by 1: 1: 6～8.
Among the preparation technology of above-mentioned sea cucumber mucopolysaccharide capsule, the extraction process of described sea cucumber mucopolysaccharide is as follows:
(1) enzymolysis processing: will add HCl in the sea cucumber homogenate, transfer PH2.0～2.5, add pepsin, in 40～50 ℃ water-bath, stirred enzymolysis 5～8 hours, obtain the pepsin enzymolysis liquid, transfer PH8.0～9.0 with KOH again, then, add trypsase, in 40～50 ℃ water-bath, stirred enzymolysis 3～5 hours.Be cooled to rapidly below 30 ℃, obtain trypsin digestion liquid;
(2) centrifugal, flocculation treatment: above-mentioned sea cucumber trypsin digestion liquid is carried out high speed centrifugation separate, keep rufous liquid.Add HCl again, transfer PH6.8～7.2.Utilize fining agent then, in the B component in 1: 0.002 the ratio elder generation interpolation fining agent, stir after 5～10 minutes, static 3-5 hour, carry out high speed centrifugation and separate, keep supernatant, in the A component in 1: 0.004 the ratio interpolation interpolation earlier fining agent, stir after 5～10 minutes static 3-5 hour;
(3) precipitation with alcohol, processing: with above-mentioned supernatant, under stirring state gently, add 70～95% edible ethanols at leisure, to solution concentration 60%, static spending the night;
(4) dioxygen decolouring: above-mentioned sediment is added DDW, be configured to 2～5% solution, under 45～50 ℃ condition, drip hydrogen peroxide and decolour, be light yellow for extremely to solution.And then gently under the stirring state, add 70～95% edible ethanols at leisure, to solution concentration 40～70%, static spending the night carried out high speed centrifugation and separated, and keeps sediment.Sediment is carried out freeze drying, and ultramicro grinding is weighed, and promptly gets sea cucumber mucopolysaccharide.
The present invention is raw material with fresh sea cucumber, adopted modern high-new bioscience technology, its product has solved the demand of people to the instant product of sea cucumber, kept the original nutritional labeling of fresh sea cucumber, avoided long-time storage, carried inconvenient problem, improved the sea cucumber nutrient composition the human absorptivity, improved the bioavilability of human body.
One, the present invention has utilized the superfreeze vacuum drying technique to carry out the preparation of the instant product of a kind of full sea cucumber, and it is as follows that the full sea cucumber of its freeze-drying has characteristics:
1. dewater under the cryogenic vacuum condition, preservative free, its technical process and finished product are harmless, have excellent preservativity, its nutrition can replace FF fully.
2. the original color of bright sea cucumber, form and protein, vitamin can have been kept.Taste flavor, fine and tender taste, high resilience can be burnt to tender and not broken, and is greasy and not mashed, calipash arranged, the mouthfeel of snakeskin.
3. the normal temperature preservation can reach 10 years under the vacuumizing-inflating packing condition.Greatly reduce the storing cost, therefore no longer need complicated cold chain, do not need freezer/Refrigerated Transport instrument, low temperature sales counter and domestic refrigerator.
4. the moisture that accounts for the most of weight of food is removed, and is therefore in light weight, is convenient to transportation.
5. rehydration is rapid, has shortened cooking time, cook simple and easy to do, instant.
Two. the technology path that the present invention has utilized the low temperature superfine communication technique to combine with the superfreeze vacuum drying technique, carried out the preparation of the instant product of the full sea cucumber powder of freeze-drying, kept the original nutritional labeling of bright sea cucumber to the full extent, improved to the greatest extent the bioavilability of human body to the sea cucumber nutrient composition, the performance of ceiling effect sea cucumber nutrient.
Three. when extracting sea cucumber mucopolysaccharide, utilize the broken tissue homogenate technology of ultralow temperature micro mist, improved the degree of sea cucumber tissue homogenate, shortened enzymolysis time, improved the yield of mucopolysaccharide, and bioavilability.Adopted biological adsorption clarification technology, hydrogen peroxide decolouring and acetate to remove protein process simultaneously, saved a large amount of ethanol consumptions, reduce production cost, removed digestion back water-solubility protein enzyme in proteolytic enzyme and the sea cucumber from, further improved the yield of mucopolysaccharide.
Four. the preparation of soft, hard shell capsules, improved the diet style of sea cucumber, for allegro crowd provides the sea cucumber functional product.
Description of drawings
Fig. 1 is a process chart of the present invention;
The specific embodiment
One. the preparation of the full sea cucumber of freeze-drying:
1. raw material and processing: get more than 2 years the new fresh and alive sea cucumbers of growth, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. precooling treatment: will clean the back sea cucumber and carry out snap frozen, its requirement: cryogenic temperature :-75 ℃, cooling time with the whole deep colling of sea cucumber till.
4. freeze-drying is handled: the sea cucumber after the precooling is inserted in the ultra low temperature vacuum freeze drier.
4.1 require: the temperature of drying plate should be controlled at 75 ℃ at the vigorous dry initial stage of distillation, drying, and mid-term, the later stage of drying was at 45 ℃ at 60 ℃.
4.2 the judgement of dry terminal point: dry terminal point can be judged with following indication: temperature of charge and temperature of heating plate reach unanimity substantially and keep a period of time; Pump group (or cold-trap) vacuum meter and hothouse vacuum meter reach unanimity, and keep a period of time; Index when hothouse vacuum meter condenser temperature is returned to the equipment zero load basically also keeps a period of time; To the freeze dryer of big butterfly valve is arranged, can close big butterfly valve vacuum machine and not descend substantially or descend seldom.More than 4 judgment basis, can use separately, also capable of being combined or unite use.
4.3 water content :≤4% (weight percentage).
After 4.4 freeze-drying finished, nitrogen injection or dry air were abolished vacuum in the hothouse, shifted out the freeze-drying sea cucumber then immediately a relative humidity below 45%, 22～25 ℃ of temperature, and discharging in the few closed environment of dust is weighed.And in identical environment, carry out half-finishedly sorting and packing.Because the material after the freeze-drying has huge surface area, hygroscopicity is very strong, therefore need finish the operation of these operations under a comparatively dry environment.
5. packing is handled: with oxygen scavenger and drier, a relative humidity below 45%, 22～25 ℃ of temperature in the few closed environment of dust, adopt vacuum nitrogen filling clad aluminum foil bag packing with the freeze-drying sea cucumber.
Two. the full sea cucumber powder preparation of freeze-drying
Method one:
1. raw material and processing: get more than 2 years the new fresh and alive sea cucumbers of growth, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. precooling treatment: will clean the full sea cucumber in back and carry out snap frozen, its requirement: cryogenic temperature :-75 ℃, cooling time with the whole deep colling of sea cucumber till.
4. freeze-drying is handled: the sea cucumber after the precooling is inserted in the ultra low temperature vacuum freeze drier.
4.1 require: the temperature of drying plate should be controlled at 75 ℃ at the vigorous dry initial stage of distillation, and dry mid-term, the later stage of drying was at 45 ℃ at 60 ℃.
4.2 the judgement of dry terminal point: dry terminal point can be judged with following indication: temperature of charge and temperature of heating plate reach unanimity substantially and keep a period of time; Pump group (or cold-trap) vacuum meter and hothouse vacuum meter reach unanimity, and keep a period of time; Index when hothouse vacuum meter condenser temperature is returned to the equipment zero load basically also keeps a period of time; To the freeze dryer of big butterfly valve is arranged, can close big butterfly valve vacuum machine and not descend substantially or descend seldom.More than 4 judgment basis, can use separately, also capable of being combined or unite use.
4.3 water content :≤4% (weight percentage).
After 4.4 freeze-drying finished, nitrogen injection or dry air were abolished vacuum in the hothouse, shifted out the freeze-drying sea cucumber then immediately a relative humidity below 45%, 22～25 ℃ of temperature, and discharging in the few closed environment of dust is weighed.And in identical environment, carry out the operation of next process.
5. ultramicro grinding is handled: the full sea cucumber of freeze-drying is inserted in the low temperature micronizer pulverize its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, amplitude 6mm, the smashing fineness of vibration medium: 2000/CM
2And in relative humidity below 45%, 22～25 ℃ of temperature, discharging in the few closed environment of dust is weighed.Because the material after the freeze-drying has huge surface area, hygroscopicity is very strong, therefore need finish the operation of these operations under a comparatively dry environment.
6. packing is handled: with the packing in the full sea cucumber preparation of freeze-drying.
Method two:
1. raw material is handled: get the new fresh and alive sea cucumbers of growth more than 2 years, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. ultramicro grinding homogenized: after the aquatic foods product chopping after will handling, size approximately: 0.5～1.0cm
2, add in 3 times the DDW, put it into and carry out homogenate in the low temperature micronizer, its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium.
4. precooling treatment: the sea cucumber tissue fluid after will pulverizing carries out snap frozen, its requirement: cryogenic temperature :-75 ℃, cooling time with the whole deep colling of sea cucumber till.
5. freeze-drying is handled: the sea cucumber tissue after the precooling is inserted in the ultra low temperature vacuum freeze drier.
5.1 require: the temperature of drying plate should be controlled at 75 ℃ at the vigorous dry initial stage of distillation, and dry mid-term, the later stage of drying was at 45 ℃ at 60 ℃.
5.2 the judgement of dry terminal point: dry terminal point can be judged with following indication: temperature of charge and temperature of heating plate reach unanimity substantially and keep a period of time; Pump group (or cold-trap) vacuum meter and hothouse vacuum meter reach unanimity, and keep a period of time; Index when hothouse vacuum meter condenser temperature is returned to the equipment zero load basically also keeps a period of time; To the freeze dryer of big butterfly valve is arranged, can close big butterfly valve, the vacuum machine does not descend substantially or descends seldom.More than 4 judgment basis, can use separately, also capable of being combined or unite use.
5.3 water content :≤4% (weight percentage).
After 5.4 freeze-drying finished, nitrogen injection or dry air were abolished vacuum in the hothouse, shifted out the freeze-drying sea cucumber then immediately a relative humidity below 45%, 22～25 ℃ of temperature, and discharging in the few closed environment of dust is weighed.
6. secondary low temperature ultramicro grinding: the freeze-drying sea cucumber inserted in the low temperature micronizer pulverize its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 7 minutes, amplitude 6mm, the smashing fineness of vibration medium: 2000/CM
2And in relative humidity below 45%, 22～25 ℃ of temperature, discharging in the few closed environment of dust is weighed.Because the material after the freeze-drying has huge surface area, hygroscopicity is very strong, therefore need finish the operation of these operations under a comparatively dry environment.
7. packing is handled: with the packing in the full sea cucumber preparation of freeze-drying.
Three. the preparation of full sea cucumber hard shell capsules
1. raw material is handled: get the new fresh and alive sea cucumbers of growth more than 2 years, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. ultramicro grinding homogenized: after the aquatic foods product chopping after will handling, size approximately: 0.5～1.0cm
2, add in 3 times the DDW, put it into and carry out homogenate in the low temperature micronizer, its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium.
4. precooling treatment: the sea cucumber tissue fluid after will pulverizing carries out snap frozen, its requirement: cryogenic temperature :-75 ℃, cooling time with the whole deep colling of sea cucumber till.
5. freeze-drying is handled: the sea cucumber tissue fluid after the precooling is inserted in the ultra low temperature vacuum freeze drier.
5.1 require: the temperature of drying plate should be controlled at 75 ℃ at the vigorous dry initial stage of distillation, and dry mid-term, the later stage of drying was at 45 ℃ at 60 ℃.
5.2 the judgement of dry terminal point: dry terminal point can be judged with following indication: temperature of charge and temperature of heating plate reach unanimity substantially and keep a period of time; Pump group (or cold-trap) vacuum meter and hothouse vacuum meter reach unanimity, and keep a period of time; Index when hothouse vacuum meter condenser temperature is returned to the equipment zero load basically also keeps a period of time; To the freeze dryer of big butterfly valve is arranged, can close big butterfly valve, the vacuum machine does not descend substantially or descends seldom.More than 4 judgment basis, can use separately, also capable of being combined or unite use.
5.3 water content :≤4% (weight percentage).
After 5.4 freeze-drying finished, nitrogen injection or dry air were abolished vacuum in the hothouse, shifted out the freeze-drying sea cucumber then immediately a relative humidity below 45%, 22～25 ℃ of temperature, and discharging in the few closed environment of dust is weighed.
6. secondary low temperature ultramicro grinding: the freeze-drying sea cucumber inserted in the low temperature micronizer pulverize its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 7 minutes, amplitude 6mm, the smashing fineness of vibration medium: 2000/CM
2And in relative humidity below 45%, 22～25 ℃ of temperature, discharging in the few closed environment of dust is weighed.Because the material after the freeze-drying has huge surface area, hygroscopicity is very strong, therefore need finish the operation of these operations under a comparatively dry environment.
With freeze-drying sea cucumber powder a relative humidity below 45%, 22～25 ℃ of temperature in the few closed environment of dust, adopt full-automatic hard shell capsules filling machine to carry out the packing of sea cucumber hard shell capsules.
Four. the preparation of sea cucumber mucopolysaccharide hard shell capsules
1. raw material is handled: get the new fresh and alive sea cucumbers of growth more than 2 years, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. ultramicro grinding homogenized: after the aquatic foods product chopping after will handling, size approximately: 0.5～1.0cm
2, add in 3 times the DDW, put it into and carry out homogenate in the low temperature micronizer, its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium.
4. enzymolysis processing: will add HCl (concentration: 6mol/L) in the above-mentioned sea cucumber tissue homogenate, transfer PH2.0～2.5, and the adding pepsin (concentration: 0.3%, consumption: 1.6%), in 50 ℃ water-bath, stir enzymolysis 6 hours, and obtained the pepsin enzymolysis liquid.Use again KOH (concentration: 0.5mol/L) transfer PH8.0～9.0, then, add trypsase (concentration: 0.3%, consumption: 5%), in 50 ℃ water-bath, stirred enzymolysis 5 hours.Be cooled to rapidly below 30 ℃, obtain trypsin digestion liquid.
5. centrifugal, flocculation treatment: above-mentioned sea cucumber trypsin digestion liquid is separated with high speed centrifugation (6000 rev/mins), keep rufous liquid.Add HCl (concentration: 6mol/L), transfer PH6.8～7.2 again.Utilize ZTC-III natural clarifying agent (there is sale in market) then, in the B component among 1: 0.002 the interpolation ZTC-III of ratio elder generation, stir after 10 minutes, static 3 hours, separate with high speed centrifugation (6000 rev/mins), keep supernatant, in the A component among 1: 0.004 the interpolation ZTC-III of ratio elder generation, stir after 10 minutes static 3 hours.
6. precipitation with alcohol, processing: with above-mentioned supernatant, under stirring state gently, add 95% edible ethanol at leisure, to solution concentration 60%, static spending the night,
7. dioxygen decolouring: above-mentioned sediment is added DDW, be configured to 5% solution, under 45-50 ℃ condition, drip hydrogen peroxide and decolour, be light yellow for extremely to solution.And then gently under the stirring state, add 95% edible ethanol at leisure, to solution concentration 60%, static spending the night separated with high speed centrifugation (6000 rev/mins), keeps sediment.Sediment is carried out freeze drying, weigh, promptly get the thick mucopolysaccharide of sea cucumber.
8. purification sea cucumber mucopolysaccharide:
8.1 above-mentioned sediment is added DDW, be configured to 5% solution, add the solid potassium acetate, making the concentration in its solution is that 2.5mol/L refrigeration is spent the night, low temperature collecting precipitation thing,
8.2 getting a semiliquid of above-mentioned supernatant again dissolves sediment.Use 0.5mol/LN
aHO transfers PH9～11, drips hydrogen peroxide and decolour under 45～50 ℃ condition, is light yellow for extremely to solution.Cooling, centrifugal, and supernatant is cooled to below 4 ℃.
8.3 with the HCL of aforesaid liquid, transfer PH1.5～2.5 with 6mol/L, centrifugal, in supernatant, add the solid potassium acetate, making the concentration in its solution is that low temperature collecting precipitation thing is spent the night in 1.5～3.0mol/L refrigeration.
8.4 after sediment respectively washed 2 times with 80% ethanol, absolute ethyl alcohol, acetone respectively, carry out freeze drying, the pure product of sea cucumber mucopolysaccharide.
9. with sea cucumber mucopolysaccharide, a relative humidity below 45%, 22～25 ℃ of temperature in the few closed environment of dust, adopt full-automatic hard shell capsules filling machine to carry out the packing of sea cucumber mucopolysaccharide hard shell capsules.
Five. the preparation of full sea cucumber soft capsule
1. raw material is handled: get the new fresh and alive sea cucumbers of growth more than 2 years, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. ultramicro grinding homogenized: after the aquatic foods product chopping after will handling, size approximately: 0.5～1.0cm
2, add in 3 times the DDW, put it into and carry out homogenate in the low temperature micronizer, its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium.
4. precooling treatment: the sea cucumber after will pulverizing organizes slurries to carry out snap frozen, its requirement: cryogenic temperature :-75 ℃, cooling time with the whole deep colling of sea cucumber till.
5. freeze-drying is handled: organize slurries to insert in the ultra low temperature vacuum freeze drier sea cucumber after the precooling.
5.1 require: the temperature of drying plate should be controlled at 75 ℃ at the vigorous dry initial stage of distillation, and dry mid-term, the later stage of drying was at 45 ℃ at 60 ℃.
5.2 the judgement of dry terminal point: dry terminal point can be judged with following indication: temperature of charge and temperature of heating plate reach unanimity substantially and keep a period of time; Pump group (or cold-trap) vacuum meter and hothouse vacuum meter reach unanimity, and keep a period of time; Index when hothouse vacuum meter condenser temperature is returned to the equipment zero load basically also keeps a period of time; To the freeze dryer of big butterfly valve is arranged, can close big butterfly valve, the vacuum machine does not descend substantially or descends seldom.More than 4 judgment basis, can use separately, also capable of being combined or unite use.
5.3 water content :≤4% (weight percentage).
After 5.4 freeze-drying finished, nitrogen injection or dry air were abolished vacuum in the hothouse, shifted out the freeze-drying sea cucumber then immediately a relative humidity below 45%, 22～25 ℃ of temperature, and discharging in the few closed environment of dust is weighed.
6. the preparation of soft capsule content: earlier polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature-10 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium; And then holothurian freeze-dried powder added in the pulverizer pulverizer mill barrel temperature-10 ℃, pulverizing time: 7 minutes, the amplitude 6mm of vibration medium make soft capsule content; The weight ratio of above-mentioned dried sea-cucumber powder, polyethylene glycol (PEG) 4000, Tween 80 was followed successively by 1: 1: 5.
With full sea cucumber soft capsule content a relative humidity below 45%, 22～25 ℃ of temperature in the few closed environment of dust, adopt full-automatic soft capsule filling machine to carry out full sea cucumber soft capsule packing.
Six. the sea cucumber mucopolysaccharide preparation of soft capsule
1. raw material is handled: get the new fresh and alive sea cucumbers of growth more than 2 years, be no more than 3 hours leaving the seawater face, carry out the fresh and alive sea cucumbers internal organ, go muscle to remove to handle, remove silt, clean, weigh.
2. immersion treatment: the aquatic foods product after will handling are put into distilled water, its requirement: coolant-temperature gage＜45 ℃, the water surface will be higher than more than 1/3 of soak, normal pressure soaked 3 hours down, take out, clean, weigh.
3. ultramicro grinding homogenized: after the aquatic foods product chopping after will handling, size approximately: 0.5～1.0cm
2, add in 3 times the DDW, put it into and carry out homogenate in the low temperature micronizer, its requirement: pulverizer mill barrel temperature-25 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium.
4. enzymolysis processing: with add in the above-mentioned sea cucumber tissue homogenate HCl (concentration: 6mol/L), transfer PH2.0～2.5, add pepsin (concentration: 0.3%, consumption: 1.6%), in 50 ℃ water-bath, stirred enzymolysis 6 hours, obtain the pepsin enzymolysis liquid.Use again KOH (concentration: 0.5mol/L) transfer PH8.0～9.0, then, add trypsase (concentration: 0.3%, consumption: 5%), in 50 ℃ water-bath, stirred enzymolysis 3 hours.Be cooled to rapidly below 30 ℃, obtain trypsin digestion liquid.
5. centrifugal, flocculation treatment: above-mentioned sea cucumber trypsin digestion liquid is separated with high speed centrifugation (6000 rev/mins), keep rufous liquid.Add HCl (concentration: 6mol/L), transfer PH6.8～7.2 again.Utilize ZTC-III natural clarifying agent (there is sale in market) then, in the component among 1: 0.002 the interpolation ZTC-IIIB of ratio elder generation, stir after 10 minutes, static 3 hours, separate with high speed centrifugation (6000 rev/mins), keep supernatant, in the component among 1: 0.004 the interpolation ZTC-IIIA of ratio elder generation, stir after 10 minutes static 3 hours.
6. precipitation with alcohol, processing: with above-mentioned supernatant, under stirring state gently, add 95% edible ethanol at leisure, to solution concentration 60%, static spending the night,
7. dioxygen decolouring: above-mentioned sediment is added DDW, be configured to 5% solution, under 45-50 ℃ condition, drip hydrogen peroxide and decolour, be light yellow for extremely to solution.And then gently under the stirring state, add 95% edible ethanol at leisure, to solution concentration 60%, static spending the night separated with high speed centrifugation (6000 rev/mins), keeps sediment.Sediment is carried out freeze drying, weigh, promptly get the thick mucopolysaccharide of sea cucumber.
8. purification sea cucumber mucopolysaccharide:
8.1 above-mentioned sediment is added DDW, be configured to 5% solution, add the solid potassium acetate, making the concentration in its solution is that 1.5～3.0mol/L refrigeration is spent the night, low temperature collecting precipitation thing,
8.2 getting a semiliquid of above-mentioned supernatant again dissolves sediment.N with 0.5mol/L
aOH transfers PH9～11, drips hydrogen peroxide and decolour under 45～50 ℃ condition, is light yellow for extremely to solution.Cooling, centrifugal, and supernatant is cooled to below 4 ℃.
8.3 with HCL accent PH1.5～2.5 of aforesaid liquid with 6mol/L, centrifugal, in supernatant, add the solid potassium acetate, making the concentration in its solution is that low temperature collecting precipitation thing is spent the night in 1.5～3.0mol/L refrigeration.
8.4 after sediment respectively washed 2 times with 80% ethanol, absolute ethyl alcohol, acetone respectively, carry out freeze drying, the pure product of sea cucumber mucopolysaccharide.
9. the preparation of soft capsule content: earlier polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature-10 ℃, pulverizing time: 5 minutes, the amplitude 6mm of vibration medium; And then holothurian freeze-dried powder added in the pulverizer pulverizer mill barrel temperature-10 ℃, pulverizing time: 7 minutes, the amplitude 6mm of vibration medium make soft capsule content; The weight ratio of above-mentioned dried sea-cucumber powder, polyethylene glycol (PEG) 4000, Tween 80 was followed successively by 1: 1: 7.
10. with the sea cucumber mucopolysaccharide soft capsule content, a relative humidity below 45%, 22～25 ℃ of temperature in the few closed environment of dust, adopt full-automatic soft capsule filling machine to carry out full sea cucumber soft capsule packing.
Claims (12)
1, the preparation technology of freeze-drying sea cucumber is characterized in that, carries out successively as follows:
(a) raw material is handled;
(b) immersion treatment;
(c) precooling treatment: the sea cucumber raw material after will cleaning carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(d) freeze-drying is handled;
2, the preparation technology of freeze-drying sea cucumber according to claim 1 is characterized in that: the product that (d) step is obtained is inserted in the low temperature micronizer and is pulverized.
3, the preparation technology of freeze-drying sea cucumber according to claim 1 is characterized in that: carry out the ultramicro grinding homogenized before the c step earlier.
4, a kind of preparation technology of full holothurian capsule is characterized in that, carries out successively as follows:
(1) raw material is handled;
(2) immersion treatment;
(3) precooling treatment: carry out the ultramicro grinding homogenized earlier, the sea cucumber raw material after will cleaning again carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(4) freeze-drying is handled;
(5) low temperature ultramicro grinding;
(6), adopt capsule filling machine to carry out packing with the product in the step (5).
5, the preparation technology of full holothurian capsule according to claim 4 is characterized in that: described capsule filling machine is the hard shell capsules filling machine.
6, the preparation technology of full holothurian capsule according to claim 4 is characterized in that: the product in the step (6) is a soft capsule content, and described capsule filling machine is the soft capsule filling machine.
7, the preparation technology of full holothurian capsule according to claim 6 is characterized in that: the preparation technology of described soft capsule content is as follows:
Polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 3～5 minutes, the amplitude 4～8mm of vibration medium; And then full sea cucumber powder added in the pulverizer pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 5～7 minutes, the amplitude 4～8mm of vibration medium make soft capsule content; The weight ratio of above-mentioned full sea cucumber powder, polyethylene glycol (PEG) 4000, Tween 80 is followed successively by 1: 1: 4～6.
8, a kind of preparation technology of sea cucumber mucopolysaccharide capsule is characterized in that, carries out successively as follows:
(1) raw material is handled;
(2) immersion treatment;
(3) precooling treatment: carry out the ultramicro grinding homogenized earlier, the sea cucumber raw material after will cleaning again carries out snap frozen, and cryogenic temperature is controlled at-50 ℃～-80 ℃, cooling time with the whole deep colling of sea cucumber till;
(4) extract sea cucumber mucopolysaccharide;
(5) freeze-drying is handled;
(6) the low temperature ultramicro grinding is handled;
(7), adopt capsule filling machine to carry out packing with the product in the step (6).
9, the preparation technology of sea cucumber mucopolysaccharide capsule according to claim 8 is characterized in that: described capsule filling machine is the hard shell capsules filling machine.
10, the preparation technology of sea cucumber mucopolysaccharide capsule according to claim 8 is characterized in that: the product in the step (7) is a soft capsule content, and described capsule filling machine is the soft capsule filling machine.
11, the preparation technology of sea cucumber mucopolysaccharide capsule according to claim 10 is characterized in that: the preparation technology of described soft capsule content is as follows:
Polyethylene glycol (PEG) 4000, Tween 80 are inserted in the low temperature micronizer and ground, pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 3～5 minutes, the amplitude 4～8mm of vibration medium; And then the sea cucumber mucopolysaccharide powder added in the pulverizer pulverizer mill barrel temperature 0～-30 ℃, pulverizing time: 5～7 minutes, the amplitude 4～8mm of vibration medium make soft capsule content; The weight ratio of above-mentioned sea cucumber mucopolysaccharide powder, polyethylene glycol (PEG) 4000, Tween 80 is followed successively by 1: 1: 6～8.
12, according to Claim 8, the preparation technology of 9 or 10 described sea cucumber mucopolysaccharide capsules, it is characterized in that: the extraction process of described sea cucumber mucopolysaccharide is as follows:
(1) enzymolysis processing: will add HCl in the sea cucumber homogenate, transfer PH2.0～2.5, add pepsin, in 40～50 ℃ water-bath, stirred enzymolysis 5～8 hours, obtain the pepsin enzymolysis liquid, transfer PH8.0～9.0 with KOH again, then, add trypsase, in 40～50 ℃ water-bath, stirred enzymolysis 3～5 hours.Be cooled to rapidly below 30 ℃, obtain trypsin digestion liquid;
(2) centrifugal, flocculation treatment: above-mentioned sea cucumber trypsin digestion liquid is carried out high speed centrifugation separate, keep rufous liquid.Add HCl again, transfer PH6.8～7.2.Utilize fining agent then, in the B component in 1: 0.002 the ratio elder generation interpolation fining agent, stir after 5～10 minutes, static 3-5 hour, carry out high speed centrifugation and separate, keep supernatant, in the A component in 1: 0.004 the ratio interpolation interpolation earlier fining agent, stir after 5～10 minutes static 3-5 hour;
(3) precipitation with alcohol, processing: with above-mentioned supernatant, under stirring state gently, add 70～95% edible ethanols at leisure, to solution concentration 60%, static spending the night;
(4) dioxygen decolouring: above-mentioned sediment is added DDW, be configured to 2～5% solution, under 45～50 ℃ condition, drip hydrogen peroxide and decolour, be light yellow for extremely to solution.And then gently under the stirring state, add 70～95% edible ethanols at leisure, to solution concentration 40～70%, static spending the night carried out high speed centrifugation and separated, and keeps sediment.Sediment is carried out freeze drying, and ultramicro grinding is weighed, and promptly gets sea cucumber mucopolysaccharide.
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| CN101642264B (en) * | 2009-07-08 | 2010-07-28 | 本溪龙宝（集团）参茸有限公司 | Making process of active sea cucumbers |
| CN100998427B (en) * | 2006-12-31 | 2010-09-08 | 李朝武 | Method for processing active sea cucumber powder |
| CN101863997A (en) * | 2010-05-24 | 2010-10-20 | 南京中医药大学 | Method for preparing hojothuria leucospilota polysaccharide |
| CN102669748A (en) * | 2012-05-07 | 2012-09-19 | 海南加华海产生物制药集团有限公司 | Sea cucumber lyophiled powder capsule and production method thereof |
| CN103454270A (en) * | 2013-09-11 | 2013-12-18 | 大连海晏堂生物有限公司 | Detection method for sea cucumber polysaccharide |
| CN104814465A (en) * | 2015-04-29 | 2015-08-05 | 合肥不老传奇保健科技有限公司 | Freeze-dried instant trepang granules from trepang frozen complexes modified by false-particle powder and preparation method of freeze-dried instant trepang granules |
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| CN100998427B (en) * | 2006-12-31 | 2010-09-08 | 李朝武 | Method for processing active sea cucumber powder |
| CN101642264B (en) * | 2009-07-08 | 2010-07-28 | 本溪龙宝（集团）参茸有限公司 | Making process of active sea cucumbers |
| CN101863997A (en) * | 2010-05-24 | 2010-10-20 | 南京中医药大学 | Method for preparing hojothuria leucospilota polysaccharide |
| CN101863997B (en) * | 2010-05-24 | 2012-05-23 | 南京中医药大学 | Method for preparing hojothuria leucospilota polysaccharide |
| CN102669748A (en) * | 2012-05-07 | 2012-09-19 | 海南加华海产生物制药集团有限公司 | Sea cucumber lyophiled powder capsule and production method thereof |
| CN103454270A (en) * | 2013-09-11 | 2013-12-18 | 大连海晏堂生物有限公司 | Detection method for sea cucumber polysaccharide |
| CN104814465A (en) * | 2015-04-29 | 2015-08-05 | 合肥不老传奇保健科技有限公司 | Freeze-dried instant trepang granules from trepang frozen complexes modified by false-particle powder and preparation method of freeze-dried instant trepang granules |
| CN107029109A (en) * | 2017-04-27 | 2017-08-11 | 河南佳禾康生物食品科技有限公司 | One kind softening blood vessel enhancing flexible health products of blood vessel and preparation method thereof |
| CN107348316A (en) * | 2017-07-25 | 2017-11-17 | 宋若翰 | The system of processing and mode of a kind of food material |
| CN107373450A (en) * | 2017-07-25 | 2017-11-24 | 烟台东极生物科技有限公司 | A kind of ultra micro high calcium deep-sea collagen powder and its preparation method and application |
| CN107712692A (en) * | 2017-11-23 | 2018-02-23 | 黑龙江美丽石岛科技开发有限公司 | A kind of method that nutriment is extracted from unsalted dried sea cucumbers |
| CN110292584A (en) * | 2019-06-12 | 2019-10-01 | 安徽省神草堂国药有限公司 | A kind of fresh animal class freeze-drying wall-breaking method |
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