CN110200199A - For the method for disinfection of the Self-cooling super-pressure solid-solid phase change of frost solid - Google Patents

For the method for disinfection of the Self-cooling super-pressure solid-solid phase change of frost solid Download PDF

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Publication number
CN110200199A
CN110200199A CN201910579414.7A CN201910579414A CN110200199A CN 110200199 A CN110200199 A CN 110200199A CN 201910579414 A CN201910579414 A CN 201910579414A CN 110200199 A CN110200199 A CN 110200199A
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solid
pressure
frost
packaging bag
disinfection
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CN110200199B (en
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于勇
李异凡
胡力晖
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Zhejiang University ZJU
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Zhejiang University ZJU
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L5/00Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
    • A23L5/20Removal of unwanted matter, e.g. deodorisation or detoxification
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)
  • Food Preservation Except Freezing, Refrigeration, And Drying (AREA)

Abstract

The invention discloses a kind of method for disinfection of Self-cooling super-pressure solid-solid phase change for frost solid, solid is solid food or solid medicine, include the following steps: that the solid first by processing to be sterilized freezes, resulting frost solid is put into packaging bag, post package is vacuumized to packaging bag;Sealing after the vacuum packaging bag of resulting built-in frost solid and rubble ice, coolant liquid are put into togerther in hermetic bag;It is then placed in the sterilization high pressure that setting is boosted in extra-high tension unit inner cavity;Then pressure maintaining (5 ± 0.5) second under the sterilization high pressure of the setting;After release, the sample in packaging bag is taken out.Sterilization to solid sample can effectively be realized using method of the invention, and can guarantee that bactericidal effect is better than common ultra high pressure treatment under same pressure condition, and can guarantee that the quality of specimen material is not destroyed.

Description

For the method for disinfection of the Self-cooling super-pressure solid-solid phase change of frost solid
Technical field
The invention belongs to food and drug to sterilize field, and in particular to a kind of sterilization side of Self-cooling super-pressure solid-solid phase change Method.
Background technique
Food, drug sterilization are exactly raw material using food or drug or processed goods as object, by causing food, drug The sterilization and degerming of rotten principal element --- microorganism, reach the stabilisation of food, drug quality, to effectively extend food The shelf-life of product, drug.The research that food, drug are sterilized is always emphasis concerned by people, with constantly mentioning for the level of consumption Height, how under conditions of not changing food, drug items characteristic quick sterilization, be related fields concern technical problem.
Sterilization technology (hereinafter referred cold pressing Synergistic biocidal) under super-pressure and low temperature act on simultaneously can be rapidly and efficiently The physicochemical property of ground sterilization while greatly reservation process object itself.But it is existing research shows that cold pressing Synergistic biocidal is needed in super-pressure Building outer loop cold source cools down to super-pressure cavity on the outside of cavity, such as when high-pressure chamber is 2L, temperature fall time is about needed Want 1.5-2 hours;When the volume of high-pressure chamber increases, temperature fall time but will then be greatly prolonged;This will lead to reduction production effect Rate, so that existing cold pressing Synergistic biocidal method is not suitable for actual production.Above-mentioned temperature fall time theoretically depends on the change of pressure Change, temperature and pressure garments two phase lines from two phasors of water-ice I.Under the conditions of the above-mentioned prior art, if not to super-pressure chamber Body cools down, and will lead to super-pressure cavity and the intracorporal object to be processed of super-pressure chamber due to temperature and pressure effect, in boost process Temperature increases, and causes object to be processed that designed phase transformation does not occur, and bactericidal effect is very poor.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Self-cooling super-pressure solid-solid phase changes for frost solid Method for disinfection.
In order to solve the above technical problem, the present invention provides a kind of Self-cooling super-pressure solid-solid phase changes for frost solid Method for disinfection, solid be solid food or solid medicine, include the following steps:
1), the solid first by processing to be sterilized freezes, until the central temperature of resulting frost solid is -4~-15 ℃;
To guarantee that the water in sample becomes the ice of solid forms completely;
2), the resulting frost solid of step 1) is put into packaging bag, post package is vacuumized to packaging bag;
3), according to frost solid: ice cube: coolant liquid=1:(0.8 ± 0.08): the mass ratio of (0.2 ± 0.02), by step 2) sealing after the vacuum packaging bag of resulting built-in frost solid and ice cube, coolant liquid are put into togerther in hermetic bag;It is then placed in With (30 ± 3) MPa that boosts every time in extra-high tension unit inner cavity, the rule of pressure (5 ± 0.5) second is kept to boost to setting after boosting Sterilization high pressure;Then pressure maintaining (5 ± 0.5) second under the sterilization high pressure of the setting;
The sterilization high pressure set is 260~270Mpa;
That is, remaining boosting only needs to meet according to above-mentioned boosting rule, last time boosting other than last time is boosted The sterilization high pressure (final pressure pressure) for rising to the setting, without the constraint by above-mentioned boosting rule;
4), after release, the sample in packaging bag is taken out.
Note: it for natural quick pressure releasing, can be completed within generally about 3 seconds or so.
Set sterilization high pressure of the invention is to ensure that ice I is changed into the minimum pressure of ice III, can ensure to send out under the pressure Raw ice I is changed into the phase transformation of ice III, there is good bactericidal effect.
The invention belongs to Self-cooling super-pressure solid-solid phase changes, sterilize phase transformation: I-ice of ice III, target to be processed: frost solid; Sterilizing time section: boost phase;Sample after pressure release: frost completely.
The improvement of method for disinfection as the Self-cooling super-pressure solid-solid phase change for frost solid of the invention: coolant liquid It for alcohol or is salts solution.
The improvement of method for disinfection as the Self-cooling super-pressure solid-solid phase change for frost solid of the invention: the salt For hydrochloride (including sodium chloride, potassium chloride), sulfate, nitrate.
The improvement of method for disinfection as the Self-cooling super-pressure solid-solid phase change for frost solid of the invention: the step It is rapid 2) in packaging bag, the hermetic bag (rubber seal bag) in step 3) be required to bear the pressure of the sterilization high pressure.
That is, packaging bag, hermetic bag (rubber seal bag) are not in breakage in the case where sterilizing high pressure.
Hermetic bag in step 3), such as polymeric seal bag, polyurethane seal bag, butadiene-styrene rubber bag can be selected.
In the present invention, volume≤extra-high tension unit cavity volume 35% of the frost solid;Ultrahigh pressure vessel can It is obtained using conventional commercially available mode.The trash ice that ice cube used in the present invention is 1~2 cubic centimetre of volume.
The purpose of the present invention is set frost solid sample (solid food or drug including frost etc.) by super-pressure The standby form with ladder boosting from cooling is sterilized.As a result, it has been found that finally obtaining food or drug can be in industrialization super-pressure Under the conditions of cavity volume (for example, 80L), quickly cold pressing Synergistic biocidal is realized within 3min.The present invention is in not co-content simultaneously Super-pressure cavity under the conditions of processing the time it is essentially identical.
In the present invention, solid-solid phase change refers to: from (solid) Xiang Bianwei of ice I ice III (solid), as described in Figure 1.
Using this method, object temperature and pressure data to be processed submit to entity indicia line part in figure, i.e., initial stage temperature with Pressure increase and reduce, ice be maintained at guarantees under I phase line of water-ice object internal water to be processed state be ice I.Reach killing for setting After bacterium high pressure (260~280Mpa), temperature increases with pressure and is increased.This is because outside is from temperature reducing substance by water, cold at this time But liquid blend-I biphase-equilibrium of ice becomes water, coolant liquid blend-III biphase-equilibrium of ice, while in the process in the sterilization of setting High pressure (260~280Mpa) temperature has a mutation peak, i.e., phase transformation of the ice I to ice III occurs for object itself to be processed, which leads Cause sterilization.In Fig. 1, circle mark part is the region that solid-solid phase change occurs.
That is, the present invention by simultaneously be added ice melting absorption the heat of transformation reach substance to be processed temperature be lower than water- I phase change line of ice (ice does not occur during processing for object i.e. to be processed to the melting process of water), in the sterilization high pressure (260 of setting ~280Mpa) under the conditions of the conversion that ice I has occurred and arrives ice III determined by the variation of temperature final temperature, while bactericidal effect is also proved This point.
Sterilization to solid sample can effectively be realized using method of the invention, and can guarantee that bactericidal effect is better than with isobaric Common ultra high pressure treatment under the conditions of power, while sample hardness value rises level and is lower than common ultra high pressure treatment, that is, guarantee material Quality is not destroyed.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 is solid-solid phase change figure.
Specific embodiment
The present invention is described further combined with specific embodiments below, but protection scope of the present invention is not limited in This:
Embodiment 1, for solid Self-cooling super-pressure solid-solid phase change method for disinfection
1) it, transports fresh and alive perch back laboratory, is put into the bubble chamber for filling with trash ice, make its death by suffocation, then through going Head truncates, goes internal organ and peeling, processing of boning, and is cleaned and is drained with distilled water, is finally cut into the perch of about (50g ± 5) g Block completes pre-treatment;Terminate from perch death by suffocation to pre-treatment, overall process is completed in 15min.
2), perch block is freezed for 24 hours in -4 DEG C, at this time -4 DEG C of the central temperature of perch block, to guarantee the water of perch block Become the ice of solid forms completely, perch block must be freezed;
3), the frost perch block of about 1000g is packed into immediately in vacuum packaging bag, is vacuum-packed and (packaging bag is taken out Vacuum post package),
Note: the volume of above-mentioned vacuum packaging bag is about 4000ml, speed of exhaust 20m3/ h, pumpdown time 10s, electric heating envelope Mouth time 1.5s.Therefore vacuum degree can reach the requirement of vacuum in packaging bag.
4) above-mentioned steps 3, are selected immediately) it is resulting with frost vacuum packaging bag 8 of perch block, it carries out respectively as follows Operation:
1., a vacuum packaging bag and trash ice (800g) and alcohol (200g) with frost perch block is put into a rubber In hermetic bag, then by rubber seal bag be put into extra-high tension unit (that is, be put into the super-pressure cavity equipped with super-high pressure work liquid, This is the conventional usage mode of extra-high tension unit).
The alcohol is 75% (volume %) alcohol;The cavity volume of extra-high tension unit is about 30L.
2., extra-high tension unit (each boosting ladder for 30MPa, rate of pressure rise is about 200MPa/min) is boosted with ladder; Pressure maintaining 5 seconds rules carry out ultra high pressure treatment after boosting every time, until rising to final pressure pressure is that 260Mpa (boost by last time Need to only meet and rise to the final pressure pressure, without the constraint by above-mentioned boosting ladder), reach after final pressure pressure maintaining 5 seconds, then Vacuum packaging bag is taken out in release (quick pressure releasing).
5) vacuum packaging bag, is opened in super-clean bench, takes out perch block;It is detected in the following way:
Wherein four bags of perch block is taken to be averaged referring to the measurement of GB4789.2-2016 progress sample total plate count;
Other four bags, after the flesh of fish is taken out are taken, appoints for every bag and takes three pieces to be cut into 10mm3Square, place until small fish block Central temperature is equal to room temperature locating for super-clean bench (equilibration time is about 15 minutes);With flat cylinder probe P/6, test rate 1mm/s, compression degree 50%, stop interval 5s, the condition that the rate of data collection is 200 points/second are measured hardness number;It makes even Mean value;
Acquired results are as described in Table 1.
Another: the resulting perch block of step 1) is detected according to above-mentioned steps, and (hardness number directly proceeds without elder generation when testing Balance 15 minutes);Acquired results (average value) are as follows: hardness number is about 12.1;Its total plate count is about 3.2 × 107A/gram;
Total plate count log value after total plate count decreasing value=untreated total plate count log value-processing.
Table 1 is the total plate count reduction logarithm that the food of ultra high pressure treatment is carried out through different approaches.
As it can be seen that quickly and effectively sterilization processing can be carried out to solid food, drug using process conditions of the invention. Moreover, the bactericidal effect not simple increment with the increase of pressure and dwell time, there are preferably boost gradient and a pressure maintainings The combination of time.
Comparative example 1-1~comparative example 1-6 changes final pressure pressure, remaining is equal to embodiment 1.Specific process parameter and knot Fruit is as described in Table 1.
According to 1 series of comparative example, it can be seen that increasing the promotion that pressure is conducive to bactericidal effect in a certain range, increase pressure Power to 260 bactericidal effects have great growth;But it is further added by the enhancing that pressure has no obvious bactericidal effect later, and will increase superelevation Equipment loss is pressed, the problem of improving production cost is more brought.
Comparative example 2-1~comparative example 2-6 changes the final pressure dwell time, remaining is equal to embodiment 1.Specific process parameter It is as described in Table 1 with result.
According to 2 series of comparative example, it can be seen that: the appropriate increase final pressure dwell time is conducive to promote bactericidal effect, but superelevation 5 It is unobvious to bactericidal effect promotion that the final pressure dwell time is further increased after second, and can be brought and be extended the production time, reduce production The problem of efficiency.
Comparative example 3-1~comparative example 3-4 changes boosting gradient, remaining is equal to embodiment 1.Specific process parameter and knot Fruit is as described in Table 1.
According to 3 series of comparative example, it can be seen that: the appropriate boosting gradient that reduces is conducive to promote bactericidal effect, and to solids Matter damage reduces, but unobvious to bactericidal effect and reduction solid matter damage effect promotion less than the boosting gradient of 30MPa, and The problem of bringing and extend the production time, reducing production efficiency.
Comparative example 4-1~comparative example 4-6 changes the ladder dwell time, remaining is equal to embodiment 1.Specific process parameter It is as described in Table 1 with result.
According to 4 series of comparative example, it can be seen that: the appropriate increase ladder dwell time is conducive to promote bactericidal effect, and to solid Body species damages reduce, and but further increase the ladder dwell time after superelevation 5 seconds to bactericidal effect and reduce solid matter damage The problem of it is unobvious to hurt effect promoting, and can bring and extend the production time, reduce production efficiency.
Comparative example 5-1~comparative example 5-9 changes sample, trash ice and alcohol this mass ratio relationship, remaining is equal to Embodiment 1.Specific process parameter and result are as described in Table 1.
According to 5 series of comparative example, it can be seen that: there are an optimal solids treatment object/trash ice/alcohol mass ratios to close System, can be optimal bactericidal effect.
Table 1, the total plate count that the solid that cold pressing Synergistic biocidal is handled is carried out through different approaches reduce logarithm
Note: final pressure temperature, the temperature of the perch block after referring to the final resulting final pressure pressure pressure maintaining of step 4).
Comparative experiments: not influence of the super-pressure cavity of co-content to bactericidal effect:
Change the volume of super-pressure cavity in embodiment 1, remaining is equal to embodiment 1;Pair of acquired results and embodiment 1 Than as described in Table 2.
Table 2,
75% alcohol in embodiment 1 is changed to 0.5mol/L sodium chloride solution, 0.5mol/L chlorination by embodiment 2 respectively Potassium solution, dosage are constant;Remaining is equal to embodiment 1;Acquired results and the comparison of embodiment 1 are as described in Table 3.
Table 3
The above list is only a few specific embodiments of the present invention for finally, it should also be noted that.Obviously, this hair Bright to be not limited to above embodiments, acceptable there are many deformations.Those skilled in the art can be from present disclosure All deformations for directly exporting or associating, are considered as protection scope of the present invention.

Claims (4)

1. for frost solid Self-cooling super-pressure solid-solid phase change method for disinfection, solid be solid food or solid medicine, It is characterized in that including the following steps:
1), the solid first by processing to be sterilized freezes, until the central temperature of resulting frost solid is -4~-15 DEG C;
2), the resulting frost solid of step 1) is put into packaging bag, post package is vacuumized to packaging bag;
3), according to frost solid: ice cube: coolant liquid=1:(0.8 ± 0.08): the mass ratio of (0.2 ± 0.02), by step 2) institute Sealing after the vacuum packaging bag and ice cube, coolant liquid of the built-in frost solid obtained are put into togerther in hermetic bag;It is then placed in superelevation It presses with (30 ± 3) MPa that boosts every time in equipment inner cavity, keeps the rule of pressure (5 ± 0.5) second to boost to killing for setting after boosting Bacterium high pressure;Then pressure maintaining (5 ± 0.5) second under the sterilization high pressure of the setting;
The sterilization high pressure set is 260~270Mpa;
4), after release, the solid in packaging bag is taken out.
2. the method for disinfection of the Self-cooling super-pressure solid-solid phase change according to claim 1 for frost solid, feature It is:
Coolant liquid is alcohol or is salts solution.
3. the method for disinfection of the Self-cooling super-pressure solid-solid phase change according to claim 2 for frost solid, feature It is:
The salt is hydrochloride (including sodium chloride, potassium chloride), sulfate, nitrate.
4. the method for disinfection of any Self-cooling super-pressure solid-solid phase change for frost solid according to claim 1~3, It is characterized in that:
The hermetic bag in packaging bag, step 3) in the step 2) is required to that the pressure of the sterilization high pressure can be born.
CN201910579414.7A 2019-06-29 2019-06-29 Self-cooling type ultrahigh-pressure solid-solid phase change sterilization method for frozen solid Active CN110200199B (en)

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CN110214887A (en) * 2019-06-28 2019-09-10 浙江大学 For the device and method of liquid Self-cooling ultrahigh-pressure sterilization
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