CN110200199B - Self-cooling type ultrahigh-pressure solid-solid phase change sterilization method for frozen solid - Google Patents
Self-cooling type ultrahigh-pressure solid-solid phase change sterilization method for frozen solid Download PDFInfo
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- 239000007790 solid phase Substances 0.000 title claims abstract description 17
- 230000008859 change Effects 0.000 title claims description 21
- 238000004806 packaging method and process Methods 0.000 claims abstract description 18
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- 238000009461 vacuum packaging Methods 0.000 claims abstract description 10
- 239000000110 cooling liquid Substances 0.000 claims abstract description 9
- 238000007710 freezing Methods 0.000 claims abstract description 6
- 230000008014 freezing Effects 0.000 claims abstract description 6
- 235000021055 solid food Nutrition 0.000 claims abstract description 5
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical group [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
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- 229910002651 NO3 Inorganic materials 0.000 claims description 2
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/20—Removal of unwanted matter, e.g. deodorisation or detoxification
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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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 self-cooling type ultrahigh pressure solid-solid phase transition sterilization method for frozen solids, wherein the solids are solid foods or solid medicines, and the method comprises the following steps: freezing a solid to be sterilized, putting the obtained frozen solid into a packaging bag, vacuumizing the packaging bag and then packaging; putting the obtained vacuum packaging bag filled with the frozen solid, ice cubes and cooling liquid into a sealing bag and then sealing; then the mixture is put into an inner cavity of ultrahigh pressure equipment to be pressurized to a set sterilization high pressure; then maintaining the pressure (5 +/-0.5) seconds under the set sterilization high pressure; after the pressure was released, the sample was taken out of the packaging bag. The method can effectively realize sterilization of the solid sample, can ensure that the sterilization effect is better than that of common ultrahigh pressure treatment under the same pressure condition, and can ensure that the texture of the sample material is not damaged.
Description
Technical Field
The invention belongs to the field of sterilization of foods and medicines, and particularly relates to a self-cooling ultrahigh-pressure solid-solid phase change sterilization method.
Background
The sterilization of food and medicine is to take raw materials or processed products of food or medicine as objects, and achieve the stabilization of the quality of the food and medicine by sterilizing and degerming microorganisms which are main factors causing the deterioration of the food and medicine, thereby effectively prolonging the quality guarantee period of the food and medicine. The research on sterilization of foods and medicines is always the focus of attention of people, and with the continuous improvement of the consumption level, how to rapidly sterilize foods and medicines under the condition of not changing various characteristics of the foods and the medicines is a technical problem concerned in related fields.
The sterilization technology (hereinafter, cold pressing and sterilization) under the simultaneous action of ultrahigh pressure and low temperature can sterilize rapidly and efficiently and greatly keep the physical and chemical properties of the treated object. However, the existing research shows that the cold pressing and sterilization are cooperated, an external circulation cold source needs to be constructed on the outer side of the ultrahigh pressure cavity to cool the ultrahigh pressure cavity, for example, when the high pressure cavity is 2L, the cooling time is about 1.5-2 hours; when the volume of the high-pressure cavity is increased, the cooling time is greatly prolonged; this results in a reduction in production efficiency, making the existing cold pressing sterilization method unsuitable for practical production. The above-mentioned cooling time theoretically depends on the change of pressure, and the temperature and pressure obey the two-phase line in the two-phase diagram of water-ice I. Under the above-mentioned prior art condition, if not cooling to the superhigh pressure cavity, can lead to the thing to be handled in superhigh pressure cavity and the superhigh pressure cavity because warm-pressing effect, the temperature risees at the in-process that steps up, leads to the thing to be handled not to take place the phase transition that designs, and the bactericidal effect is extremely poor.
Disclosure of Invention
The invention aims to provide a self-cooling ultrahigh-pressure solid-solid phase change sterilization method for frozen solids.
In order to solve the technical problems, the invention provides a self-cooling type ultrahigh pressure solid-solid phase change sterilization method for frozen solids, wherein the solids are solid foods or solid medicines, and the method comprises the following steps:
1) Freezing the solid to be sterilized until the central temperature of the obtained frozen solid is-4 to-15 ℃;
thereby ensuring that the water in the sample becomes completely ice in solid form;
2) Putting the frozen solid obtained in the step 1) into a packaging bag, vacuumizing the packaging bag and then packaging;
3) According to the frozen solid: ice blocks: cooling liquid =1: (0.8 ± 0.08): (0.2 +/-0.02) by mass, putting the vacuum packaging bag filled with the frozen solid obtained in the step 2), ice cubes and cooling liquid into a sealing bag, and sealing; then the mixture is put into an inner cavity of ultrahigh pressure equipment to be boosted to the set sterilization high pressure by the rule of boosting pressure (30 +/-3) MPa each time and keeping the pressure (5 +/-0.5) seconds after boosting; then maintaining the pressure (5 +/-0.5) seconds under the set sterilization high pressure;
the set sterilization high pressure is 260-270 Mpa;
that is, except for the last boosting, the rest boosting is performed according to the boosting rule, and the last boosting only needs to be performed until the set sterilization high pressure (final pressure) is reached, and is not restricted by the boosting rule;
4) And after pressure relief, taking out the sample in the packaging bag.
Note: the natural rapid pressure relief can be completed in about 3 seconds generally.
The sterilization high pressure set by the invention is the lowest pressure for ensuring the ice I to be converted into the ice III, and the phase change of the ice I to the ice III can be ensured under the pressure, so that the invention has good sterilization effect.
The invention belongs to self-cooling type ultrahigh pressure solid-solid phase change and sterilization phase change: ice i-ice iii, target to be treated: freezing the solid; and (3) sterilization time period: a boosting stage; sample after pressure release: completely freezing.
The invention relates to an improvement of a self-cooling type ultrahigh pressure solid-solid phase change sterilization method for frozen solids, which comprises the following steps: the cooling liquid is alcohol or salt water solution.
The invention relates to an improvement of a self-cooling type ultrahigh pressure solid-solid phase change sterilization method for frozen solids, which comprises the following steps: the salt is hydrochloride (including sodium chloride and potassium chloride), sulfate, and nitrate.
The invention relates to an improvement of a self-cooling type ultrahigh pressure solid-solid phase change sterilization method for frozen solids, which comprises the following steps: the packaging bag in the step 2) and the sealing bag (rubber sealing bag) in the step 3) are required to bear the pressure of the sterilization high pressure.
That is, the packaging bag and the sealing bag (rubber sealing bag) are not broken under the high sterilization pressure.
The sealing bag in step 3) can be selected from polyethylene sealing bag, polyurethane sealing bag and styrene butadiene rubber bag.
In the invention, the volume of the frozen solid is less than or equal to 35% of the volume of the inner cavity of the ultrahigh-pressure equipment; the ultra-high pressure vessel is available in a conventional commercial manner. The ice used in the invention is crushed ice with the volume of 1-2 cubic centimeters.
The invention aims to sterilize frozen solid samples (including frozen solid food or medicines and the like) in a mode of step pressure increasing and self-cooling by an ultrahigh pressure device. As a result, the finally obtained food or medicine can realize quick cold-pressing and sterilization in coordination within 3min under the condition of the volume of an industrialized ultrahigh-pressure cavity (for example, 80L). Meanwhile, the processing time of the invention is basically the same under the condition of ultrahigh pressure cavities with different volumes.
In the present invention, solid-solid phase transition means: change phase from ice i (solid) to ice iii (solid) as depicted in fig. 1.
By using the method, the temperature and pressure data of the object to be treated is obeyed to the part of a solid mark line in the graph, namely, the temperature is reduced along with the increase of the pressure in the initial stage, and the ice is kept below the phase line of water-ice I to ensure that the state of the water in the object to be treated is ice I. After reaching the set sterilization high pressure (260-280 MPa), the temperature rises along with the increase of the pressure. The reason is that the self-cooling substance at the outer side is changed into water and cooling liquid blend-ice I two-phase balance and water and cooling liquid blend-ice III two-phase balance, and meanwhile, a sudden change peak exists at the set sterilization high pressure (260-280 Mpa) temperature in the process, namely the self-phase change of the ice I to the ice III occurs in the object to be treated, and the transformation leads to sterilization. In fig. 1, the circled portion is a region where solid-solid phase transition occurs.
Namely, the invention simultaneously adds the phase change heat absorbed by the melting of ice blocks to reach the temperature of the substance to be treated lower than the phase change line of water-ice I (namely the substance to be treated does not have the ice-water melting process in the treatment process), determines the conversion from ice I to ice III through the temperature final temperature change under the set sterilization high pressure (260-280 MPa), and simultaneously proves the point of sterilization effect.
The method can effectively realize sterilization of the solid sample, can ensure that the sterilization effect is better than that of common ultrahigh pressure treatment under the same pressure condition, and simultaneously ensures that the hardness value of the sample is raised to a level lower than that of the common ultrahigh pressure treatment, namely, the texture of the material is not damaged.
Drawings
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Fig. 1 is a solid-solid phase transition diagram.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1 self-cooling type ultra-high pressure solid-solid phase transition sterilization method for solid
1) Transporting the fresh and live weever back to a laboratory, putting the fresh and live weever into a foam box filled with crushed ice to suffocate the weever to die, then removing heads, tails, viscera, skins and bones, washing the weever with distilled water, draining the weever, and finally cutting the weever into weever blocks of about (50 g +/-5) g to finish pretreatment; the whole process is completed within 15min from the death of the weever by suffocation to the end of pretreatment.
2) Freezing the weever blocks at-4 ℃ for 24h, wherein the central temperature of the weever blocks is-4 ℃, so that the water of the weever blocks is completely changed into ice in a solid form to obtain frozen weever blocks;
3) Immediately filling 1000g of frozen weever blocks into a vacuum packaging bag for vacuum packaging (packaging the packaging bag after vacuumizing),
note: the vacuum packaging bag has a volume of about 4000ml and an air suction rate of 20m 3 H, air exhaust time of 10s and electric heating sealing time of 1.5s. Therefore, the vacuum degree in the packaging bag can meet the vacuum requirement.
4) Immediately selecting 8 vacuum packaging bags with the frozen weever blocks obtained in the step 3), and respectively carrying out the following operations:
(1) the vacuum packaging bag with the frozen weever blocks, the crushed ice (800 g) and the alcohol (200 g) are placed into a rubber sealing bag, and then the rubber sealing bag is placed into the ultrahigh pressure equipment (namely, the rubber sealing bag is placed into an ultrahigh pressure cavity with ultrahigh pressure working fluid, which is a conventional use mode of the ultrahigh pressure equipment).
The alcohol is 75% (volume%) alcohol; the volume of the chamber of the ultra high pressure equipment is about 30L.
(2) Step boosting is carried out on ultrahigh pressure equipment by steps (each boosting step is 30MPa, and the boosting speed is about 200 MPa/min); and (3) performing ultrahigh pressure treatment at a rule of keeping the pressure for 5 seconds after each pressure rise until the pressure rises to 260Mpa (the pressure rises to the final pressure only at the last time without being restricted by the pressure rise step), keeping the pressure for 5 seconds after the final pressure is reached, releasing the pressure (quickly releasing the pressure), and taking out the vacuum packaging bag.
5) Opening a vacuum packaging bag in the super clean bench, and taking out the weever blocks; the detection is carried out in the following way:
taking four bags of weever blocks, and determining the total number of sample colonies according to GB4789.2-2016, and taking an average value;
taking out the other four bags, and cutting into 10mm pieces of three pieces per bag 3 Until the central temperature of the small fish blocks is equal to that of the ultra clean benchRoom temperature (equilibration time about 15 minutes); measuring the hardness value under the conditions of a flat-bottom cylindrical probe P/6, a testing speed of 1mm/s, a compression degree of 50%, a retention interval of 5s and a data collection rate of 200 points/second; taking an average value;
the results obtained are shown in Table 1.
In addition: detecting the perch blocks obtained in the step 1) according to the steps (directly carrying out the hardness value test without balancing for 15 minutes in advance); the results obtained (mean) were: hardness value of about 12.1; the total number of colonies was about 3.2X 10 7 Per gram;
colony count reduction = log of total number of untreated colonies-log of total number of colonies after treatment.
Table 1 is a log of the colony counts reduction for foods subjected to ultra-high pressure treatment via different routes.
Therefore, the process condition of the invention can be adopted to quickly and effectively sterilize solid food and medicines. Moreover, the sterilization effect is not increased along with the increase of the pressure and the pressure maintaining time, and a better combination of the pressure increasing gradient and the pressure maintaining time exists.
Comparative examples 1-1 to 1-6, the final pressure was changed, and the rest was the same as in example 1. Specific process parameters and results are shown in table 1.
According to the comparative example 1 series, it can be known that increasing the pressure within a certain range is beneficial to the improvement of the sterilization effect, and the sterilization effect is greatly increased from increasing the pressure to 260; however, the pressure is increased without obvious enhancement of the sterilization effect, the loss of the ultrahigh pressure equipment is increased, and the problem of increasing the production cost is further caused.
Comparative example 2-1 to comparative example 2-6, the final pressure dwell time was changed, and the rest was the same as example 1. Specific process parameters and results are shown in table 1.
From the comparative example 2 series, it can be seen that: properly increasing the final pressure maintaining time is beneficial to improving the sterilization effect, but further increasing the final pressure maintaining time after 5 seconds is over high is not obvious to improve the sterilization effect, and can bring about the problems of prolonging the production time and reducing the production efficiency.
Comparative example 3-1 to comparative example 3-4, the pressure-increasing gradient was changed, and the rest was the same as example 1. Specific process parameters and results are shown in table 1.
From the comparative example 3 series, it can be seen that: the pressure-boosting gradient is properly reduced, so that the sterilization effect is improved, the damage to the solid matters is reduced, but the pressure-boosting gradient smaller than 30MPa is not obvious in improvement of the sterilization effect and the damage to the solid matters, and the problems of prolonging the production time and reducing the production efficiency are solved.
Comparative examples 4-1 to 4-6, the step dwell time was changed and the rest was identical to example 1. Specific process parameters and results are shown in table 1.
From the comparative example 4 series, it can be seen that: properly increasing the step pressure maintaining time is beneficial to improving the sterilization effect and reducing the damage to the solid matter, and further improving the step pressure maintaining time after 5 seconds of ultrahigh time is not obvious in improving the sterilization effect and the damage reduction effect of the solid matter, and the problems of prolonging the production time and reducing the production efficiency can be brought.
Comparative examples 5-1 to 5-9, the mass ratio of 3 samples, crushed ice and alcohol was changed, and the remainder was the same as example 1. Specific process parameters and results are shown in table 1.
From the comparative example 5 series, it can be seen that: the optimal mass proportion relation of the solid treatment substance/the crushed ice/the alcohol exists, and the optimal sterilization effect can be achieved.
TABLE 1 log reduction in colony count for solids subjected to cold pressing with sterilization via different routes
Note: the final pressure temperature refers to the temperature of the weever blocks obtained by the final pressure and pressure maintaining in the step 4).
Comparative experiment: influence of ultrahigh pressure cavities with different volumes on sterilization effect:
the volume of the ultrahigh pressure cavity in the embodiment 1 is changed, and the rest is equal to that in the embodiment 1; the results obtained are compared with those of example 1 and are shown in Table 2.
TABLE 2,
Example 2, the 75% alcohol in example 1 was changed to 0.5mol/L sodium chloride solution and 0.5mol/L potassium chloride solution, respectively, and the amount used was not changed; the rest is equivalent to the embodiment 1; the results are shown in Table 3 for the comparative example to example 1.
TABLE 3
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (3)
1. A self-cooling type ultrahigh pressure solid-solid phase change sterilization method for frozen solids, wherein the solids are solid foods, and the method is characterized by comprising the following steps:
1) Freezing a solid to be sterilized until the central temperature of the obtained frozen solid is minus 15 to minus 4 ℃;
2) Putting the frozen solid obtained in the step 1) into a packaging bag, vacuumizing the packaging bag and then packaging;
3) According to frozen solid: ice blocks: cooling liquid =1: (0.8 ± 0.08): (0.2 +/-0.02) by mass, putting the vacuum packaging bag filled with the frozen solid obtained in the step 2), ice cubes and cooling liquid into a sealing bag, and sealing; then the mixture is put into an inner cavity of an ultrahigh pressure device to be boosted to a set sterilization high pressure according to the rule that the pressure is boosted (30 +/-3) MPa every time and is kept for 5 +/-0.5 seconds after being boosted; then maintaining the pressure (5 +/-0.5) seconds under the set sterilization high pressure;
the set sterilization high pressure is 260 to 270Mpa;
the cooling liquid is alcohol or salt water solution;
4) And after pressure relief, taking out the solid in the packaging bag.
2. The self-cooling ultrahigh pressure solid-solid phase change sterilization method for frozen solids according to claim 1, wherein the method comprises the following steps:
the salt is any one of the following: hydrochloride, sulfate, nitrate;
the hydrochloride is sodium chloride or potassium chloride.
3. The self-cooling type ultrahigh pressure solid-solid phase change sterilization method for the frozen solid according to claim 1 or 2, which is characterized in that:
the packaging bag in the step 2) and the sealing bag in the step 3) are required to be capable of bearing the sterilization high pressure.
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