JP7252151B2 - Method for measuring the amount of hydrogen peroxide on the inner surface of a container - Google Patents

Description

The present invention relates to a method for measuring the amount of hydrogen peroxide sprayed on the inner surface of a container to sterilize the inner surface of the container in an aseptic filling machine that fills containers such as PET bottles with contents.

In an aseptic filling machine that fills a container such as a bottle with a content such as a beverage, the method for sterilizing the inner surface of the container is to bring the inner surface of the container into contact with a liquid sterilizing agent containing peracetic acid, hydrogen peroxide gas. Alternatively, there are methods such as spraying mist or a mixture thereof, and irradiating the container with electron beams or ultraviolet rays. Among various methods, the method of blowing a gas or mist of hydrogen peroxide solution or a mixture thereof onto the container is widely used because it is the most reliable sterilization method.

The method of spraying a hydrogen peroxide solution gas or mist or a mixture thereof on a container gasifies the hydrogen peroxide solution and sprays the gasified hydrogen peroxide gas on the container. It may also contain In this method, the sterilization ability varies depending on the amount of hydrogen peroxide gas or mist sprayed onto the container, or a mixture thereof. If the amount of hydrogen peroxide on the inner surface of the container is small, sterilization will be insufficient, and if it is excessive, the hydrogen peroxide solution will be wasted and economically unreasonable. The amount of hydrogen peroxide inside the container must be an appropriate amount.

In order to properly maintain the amount of hydrogen peroxide on the inner surface of the container, the amount of hydrogen peroxide on the inner surface of the container must be measured. Conventionally, the amount of hydrogen peroxide on the inner surface of a container is measured by putting water in the container and allowing it to stand for 24 hours, then measuring the amount of hydrogen peroxide dissolved in the water using a hydrogen peroxide concentration measuring device (Patent document 1).

JP 2015-116816 A

In the method for measuring the amount of hydrogen peroxide on the inner surface of the container described in Patent Document 1, the data obtained by measuring the amount of hydrogen peroxide on the inner surface of the container varies. Similar data could not be obtained even if the amount of spraying to the container was constant. Therefore, there is a need for a method of accurately measuring the amount of hydrogen peroxide that is sprayed onto the container.

The present invention is an aseptic filling machine that fills a sterilized container with sterilized contents in an aseptic atmosphere and seals the container with a sterilized lid material. Hydrogen peroxide is sprayed on the inner surface of the container to sterilize the container. It is an object of the present invention to provide a method for measuring the amount of hydrogen peroxide on the inner surface of a container for accurately measuring the amount of hydrogen peroxide in water gas, mist, or a mixture thereof.

The method for measuring the amount of hydrogen peroxide on the inner surface of a container according to the present invention is an aseptic filling machine that sterilizes a container by spraying a hydrogen peroxide solution gas or mist or a mixture thereof, in a container sterilization section of the aseptic filling machine, The air rinsing section sprays sterile air onto the container to which the hydrogen peroxide solution gas or mist or a mixture thereof has been sprayed, and the container is covered with a cover material that has been sterilized in the sealing section without filling anything in the filling section. is discharged from the discharge part, the lid member of the sealed container is removed, the container is filled with sterile water that does not contain metal ions in a sterile atmosphere, and the container filled with sterile water is The container is sealed with a cover material that has been sterilized in a sterile atmosphere, the sealed container is stored for a certain period of time, and the amount of hydrogen peroxide in the sterile water is measured.

Further, in the method for measuring the amount of hydrogen peroxide on the inner surface of a container according to the present invention, it is preferable to measure oxygen generated by decomposing the hydrogen peroxide in the sterile water with catalase by an electrode method.

According to the present invention, in an aseptic filling machine that sterilizes containers by spraying hydrogen peroxide gas or mist or a mixture thereof, the inner surface of the container sprayed with hydrogen peroxide gas or mist or a mixture thereof The amount of hydrogen peroxide can be measured accurately.

BRIEF DESCRIPTION OF THE DRAWINGS It is a top view which shows the outline of the aseptic filling machine which concerns on embodiment of this invention. The steps of the heating part and the molding part of the aseptic filling machine according to the embodiment of the present invention are shown, (A) is the preform supply process, (B) is the preform heating process, and (C) is the blow molding process. , (D) indicates the container removal step. The process of the sterilization part and the filling part of the aseptic filling machine according to the embodiment of the present invention is shown, (E-1) is a hydrogen peroxide water gas spraying process performed by shielding the container with a tunnel, (E-2) (F-1) is the air rinsing process with the container upright, (F-2) is the container upside down. (G) shows the filling process, and (H) shows the sealing process. 1 shows a hydrogen peroxide water gas generator incorporated in an aseptic filling machine according to an embodiment of the present invention;

Embodiments for carrying out the present invention will be described below with reference to the drawings.

FIG. 1 shows an aseptic filling machine according to an embodiment of the present invention. Aseptic filling machine for sterilizing containers, preform feeding to preform heating section, preform to container molding section, molded container inspection section, container sterilization section for container sterilization, sterilized container The air rinsing part, the filling part that fills the sterilized container with the contents sterilized by the contents sterilization device in an aseptic atmosphere, the sealing part that seals the container filled with the contents in an aseptic atmosphere with a sterilized lid material, and An outline of an aseptic filling machine consisting of a discharge section for discharging sealed containers will be described with reference to FIG. The present invention relates to a measuring method for measuring the amount of hydrogen peroxide on the inner surface of a container sprayed with hydrogen peroxide gas or mist or a mixture thereof for sterilization in a container sterilization section of an aseptic filling machine.

As shown in FIG. 1, the aseptic filling machine according to the embodiment includes a preform supply device 4 that supplies preforms 1, a heating unit 6 that heats the preforms 1 to a temperature for molding them into containers 2, and a heated preform. A molding unit 16 for molding the reform 1 into a container 2, an inspection wheel 23 for inspecting the molded container, a container sterilization unit 30 for sterilizing the molded container 2, an air rinse unit 34 for air rinsing the sterilized container 2, and an air rinse. A filling unit 39 that fills the container 2 with sterilized contents in an aseptic atmosphere, a lid material sterilization unit 52 that sterilizes the lid material 3 that is a sealing member, and a lid material 3 that sterilizes the container 2 filled with the contents. It comprises a sealing part 44 for sealing in a sterile atmosphere by means of a vacuum, a discharge part 47 for placing the sealed containers 2 on a discharge conveyor 50 and an exit part 51 for discharging the containers 2 by the discharge conveyor 50 into a non-sterile zone. Here, the inspection wheel 23 and the air rinse section 34 may not be provided.

The heating part 6 is the heating part chamber 12, the molding part 16 and the inspection wheel 23 are the molding part chamber 17, the container sterilization part 30 is the container sterilization part chamber 33, the air rinse part 34 is the air rinse part chamber 36, and the filling part 39 is the filling part chamber 41. , the seal 44 is shielded by a seal chamber 46 , the discharge 47 by a discharge chamber 49 , and the outlet 51 by an outlet chamber 53 . An atmosphere shielding chamber 27 is provided between the forming section chamber 17 and the container sterilizing section chamber 33 so that the hydrogen peroxide solution gas or mist generated in the container sterilizing section 30 or a mixture thereof does not flow into the forming section 16 . ing. Gas or mist of the hydrogen peroxide solution generated in the container sterilization section chamber 33 or a mixture thereof does not flow into the forming section chamber 17 because the atmosphere shielding chamber 27 is evacuated. Here, the heating section 6 and the molding section 16 may be shielded by a single chamber. Also, the lid material sterilization section 52 and the sealing section 44 may be shielded by a single chamber. Additionally, the seal 44 and the exhaust 47 may also be shielded by a single chamber.

During the operation of the aseptic filling machine, the container sterilization section chamber 33, the air rinse section chamber 36, the filling section chamber 41, the sealing section chamber 46, the discharge section chamber 49, and the exit section chamber 53 are sterilized by the sterilization filter. By supplying air and making the pressure in each chamber positive, the sterility of the aseptic filling machine is maintained. The pressure to maintain the positive pressure is the highest in the filling section chamber 41, and is set lower toward the air rinse section chamber 36, the container sterilization section chamber 33, and the upstream. In addition, it is set lower toward the downstream from the sealing section chamber 46, the discharging section chamber 49, and the outlet section chamber 53. By evacuating the atmosphere-isolated chamber 27, the pressure in the atmosphere-isolated chamber 27 is maintained substantially equal to the atmospheric pressure. For example, if the pressure inside the filling section chamber 41 is 20 Pa to 40 Pa, the pressure inside the other chambers is lower than the pressure inside the filling section chamber 41 .

The container sterilization chamber 33, air rinse chamber 36, filling chamber 41, sealing chamber 46, discharge chamber 49, and exit chamber 53, which must maintain a sterile atmosphere during the operation of the aseptic filling machine, are operated aseptically. sterilized before. That is, SOP processing is performed. Thereafter, aseptic air is supplied to keep the inside of each chamber in an aseptic atmosphere. Since the container sterilization section chamber 33 is sprayed with hydrogen peroxide gas or mist or a mixture thereof during operation of the aseptic filling machine, it does not have to be sterilized before the operation of the aseptic filling machine.

In the embodiment, the preform 1 is supplied to the aseptic filling machine and molded into the container 2 in the aseptic filling machine. I don't mind if it's a machine.

First, the preform 1 shown in FIG. 2(A) is continuously conveyed to the heating section 6 at a desired speed by the preform supply conveyor 5 from the preform supply device 4 shown in FIG.

The preform 1 in this embodiment is a test tube-like cylindrical body with a bottom, and is provided with a mouth portion 1a similar to the container 2 shown in FIG. 2(D) at the beginning of molding. A male thread is formed in the mouth portion 1a at the same time when the preform 1 is molded. Further, the preform 1 is formed with a support ring 1b for transportation under the opening 1a. The preform 1 or container 2 is gripped by the gripper 22 via this support ring 1b and travels through the aseptic filling machine. The preform 1 is molded by injection molding, compression molding, or the like. The material of the preform 1 is thermoplastic resin such as polyethylene terephthalate, polyethylene naphthalate, polypropylene, polyethylene, etc. It may be a single resin or a mixture thereof, or may contain recycled thermoplastic resin. Further, in order to impart barrier properties, a thermoplastic resin such as a polyamide containing an aromatic amine such as an ethylene-vinyl alcohol copolymer or m-xylylenediamine as a monomer may be included as a layer or as a mixture.

The preform 1 supplied to the heating section 6 is conveyed by wheels 7 and 8 provided with a large number of grippers 22 at a constant pitch, and reaches a heating section conveying wheel 9 . Here, as shown in FIG. 2(B), the preform 1 is released from the gripper 22, and the spindle 19 is inserted into the opening 1a of the preform 1 and conveyed.

The preform 1 is heated to a temperature suitable for subsequent blow molding by an infrared heater 14 or other heating means, as shown in FIG. 2(B). Preferably, the temperature is between 90°C and 130°C.

The temperature of the mouth portion 1a of the preform 1 is kept below 70° C. in order to prevent deformation and the like.

As shown in FIG. 2B, a spindle 19 is inserted into the opening 1a of the preform 1, heated by an infrared heater 14, and transported by an endless chain 13 while rotating. The spindles 19 are provided on the endless chain 13 at regular intervals. An endless chain 13 is rotated by pulleys 10 and 11 . By inserting a mandrel instead of the spindle 19 into the preform 1, it is possible to transport the preform 1 while rotating it in an inverted state.

The heated preform 1 is released from the spindle 19 , gripped by the gripper 22 and transported via the wheel 15 to the forming wheel 18 of the forming station 16 . The preform 1 is blow-molded into the container 2 by the mold 20 provided on the molding wheel 18, as shown in FIG. 2(C). A plurality of molds 20 and blow nozzles 21 are arranged around the forming wheel 18, and rotate around the forming wheel 18 at a constant speed as the forming wheel 18 rotates. When the heated preform 1 arrives, the mold 20 sandwiches the preform 1 . Subsequently, the blow nozzle 21 is joined to the preform 1 , and a stretching rod (not shown) is guided to a hole provided in the blow nozzle 21 and inserted into the preform 1 . The preform 1 is vertically stretched by the inserted stretching rod stretching the bottom of the preform 1, and at the same time, a gas such as air is blown into the preform 1 from the blow nozzle 21 to stretch it horizontally. The preform 1 is longitudinally stretched and transversely stretched in the mold 20 to form the container 2 . As shown in FIG. 2D, the molded container 2 is taken out from the mold 20, the support ring 1b is gripped by the gripper 22 provided on the inspection wheel 23, and transferred to the inspection wheel 23.

The molded container 2 was inspected for temperature, container body, support ring 1b, container mouth top, container bottom, etc. by inspection equipment 24 provided around an inspection wheel 23, and judged to be abnormal. In that case, it is discharged to the outside of the aseptic filling machine by a discharge device (not shown). The inspection of the container is performed in the molding section chamber 17, but it may be shielded by a separate chamber as the inspection section.

In the container temperature inspection, the surface temperature of the container 2 is inspected to determine whether the container 2 is good or bad. The temperature sensor is, for example, an infrared thermometer (IR camera), but other thermometers can also be used. In order to properly sterilize the container 2, it is necessary that residual heat remains in the container 2 when the container is molded. The temperature detected by the temperature sensor is preferably 40° C. or higher.

Further, the body of the container, the support ring 1b, the top surface of the mouth of the container, and the bottom of the container are photographed by a camera, and the state of each part is inspected. The captured image is processed by an image processing device to determine the presence or absence of abnormalities such as scratches, foreign matter, deformation, and discoloration. A container 2 exceeding the allowable range is determined to be abnormal.

Containers 2 that are not judged to be abnormal by the inspection by the inspection equipment 24 are separated from the molding unit 16 and the container so that the gas or mist of the hydrogen peroxide solution generated in the container sterilization unit 30 or a mixture thereof does not flow into the molding unit 16 . It is conveyed to the container sterilization section 30 via the wheels 25 and 26 in the atmosphere shielded chamber 27 provided between the sterilization sections 30 .

The containers 2 conveyed to the container sterilization section 30 are sterilized on the wheels 28 . FIG. 3(E-1) shows a step of spraying hydrogen peroxide solution gas onto the container 2 for sterilizing the container 2. FIG. A hydrogen peroxide water gas blowing nozzle 31 is provided to blow the hydrogen peroxide water gas onto the container 2 . The hydrogen peroxide water gas spray nozzle 31 is fixed so that the nozzle hole at the tip thereof can face the opening of the mouth portion 1a of the container 2 running directly below. If necessary, a hydrogen peroxide water gas blowing tunnel 32 is provided below the hydrogen peroxide water gas blowing nozzle 31 along the running path of the container 2 as shown in FIG. 3(E-1). The number of the hydrogen peroxide water gas blowing nozzles 31 may be one or plural. The gas of the hydrogen peroxide solution sprayed onto the container 2 flows into the container 2 to sterilize the inner surface of the container 2 . At this time, as the container 2 travels through the hydrogen peroxide water gas spraying tunnel 32, the hydrogen peroxide water gas or mist or a mixture thereof also flows to the outer surface of the container 2, and the outer surface of the container 2 is sterilized. be done.

Further, as shown in FIG. 3(E-2), the hydrogen peroxide water gas spraying nozzle 31 is caused to follow the transportation of the container 2, and the hydrogen peroxide water gas spraying nozzle 31 is inserted into the inside of the container 2 to A gas or mist of hydrogen oxide water or a mixture thereof may be directly sprayed onto the inner surface of the container 2 . The hydrogen peroxide solution gas or mist overflowing from the container 2 or a mixture thereof collides with a guide member 31 a provided surrounding the hydrogen peroxide solution gas spray nozzle 31 , and flows onto the outer surface of the container 2 . contact the outer surface of the The guide member 31a is provided with a flange portion coaxial with the hydrogen peroxide water gas spray nozzle 31 and an annular wall portion protruding from the flange portion to the outer circumference.

The hydrogen peroxide solution gas or mist or a mixture thereof is hydrogen peroxide solution gasified by the hydrogen peroxide solution gas generator 55 shown in FIG. is a mixture of The hydrogen peroxide water gas generator 55 includes a hydrogen peroxide water supply unit 56 that is a two-fluid spray nozzle that supplies hydrogen peroxide water in the form of drops, and a hydrogen peroxide water supply unit 56 that supplies hydrogen peroxide water. A vaporization unit 57 is provided for heating the hydrogen water to a decomposition temperature or less to vaporize it. The hydrogen peroxide solution supply unit 56 introduces the hydrogen peroxide solution and the compressed air from the hydrogen peroxide solution supply path 56a and the compressed air supply path 56b, respectively, and sprays the hydrogen peroxide solution into the vaporization part 57. ing. The vaporization part 57 is a pipe having a heater 57a sandwiched between the inner and outer walls, and heats and vaporizes the hydrogen peroxide solution blown into the pipe. The vaporized hydrogen peroxide solution gas is ejected from the hydrogen peroxide solution gas blowing nozzle 31 to the outside of the vaporization unit 57 . Instead of the heater 57a, the vaporizing portion 57 may be heated by dielectric heating.

As for the operating conditions of the hydrogen peroxide solution supply unit 56, for example, the pressure of the compressed air is adjusted within the range of 0.05 MPa to 0.6 MPa. Further, the hydrogen peroxide solution may be dropped by gravity or pressurized, and the supply amount can be freely set. min. ~100 g/min. supplied in the range of Also, the inner surface of the vaporizing portion 57 is heated from 140° C. to 450° C., thereby vaporizing the sprayed hydrogen peroxide solution.

The hydrogen peroxide solution gas is sprayed onto the container 2 from the hydrogen peroxide solution gas spray nozzle 31 as shown in FIG. 3(E). The amount of the hydrogen peroxide solution gas or mist, or a mixture thereof, is arbitrary, but the spraying amount is determined by the amount of hydrogen peroxide solution supplied to the hydrogen peroxide solution gas generator 55 and the spraying time. A plurality of hydrogen peroxide water gas generators 55 may be provided. The spray amount also varies depending on the size of the container 2 .

The hydrogen peroxide solution contains hydrogen peroxide, and its content is suitably in the range of 0.5% by mass to 65% by mass. If it is less than 0.5% by mass, the bactericidal power may be insufficient, and if it exceeds 65% by mass, it becomes difficult to handle safely. In addition, more preferably 0.5% by mass to 40% by mass, 40% by mass or less is easier to handle, and the concentration is low, so the amount of hydrogen peroxide remaining in the container 2 after sterilization is reduced. can.

The amount of hydrogen peroxide adhering to the inner surface of the container 2 is preferably 30 μL/container to 150 μL/container, more preferably 50 μL/container to 100 μL/container as the amount of hydrogen peroxide water containing 35% by mass of hydrogen peroxide. is. The hydrogen peroxide concentration of the hydrogen peroxide solution gas sprayed onto the container 2 is preferably 2 mg/L to 20 mg/L, more preferably 5 mg/L to 10 mg/L.

Hydrogen peroxide water contains hydrogen peroxide and water, and alcohols such as methyl alcohol, ethyl alcohol, isopropyl alcohol, normal propyl alcohol and butyl alcohol, ketones such as acetone, methyl ethyl ketone and acetylacetone, glycol ethers, etc. 1 or 2 or more may be included.

The container 2 sterilized by the container sterilizing section 30 is conveyed to the air rinse section 34 via the wheel 29 as shown in FIG. In the air rinse wheel 35 shown in FIG. 1, the container 2 is sprayed with aseptic air by the air rinse nozzle 38 as shown in FIG. 3 (F-1). The sterilized air may be normal temperature, but it is preferable to heat it. The sterilized air discharges hydrogen peroxide remaining inside the container 2, decomposes the remaining hydrogen peroxide, further enhances the sterilization effect, and also has the effect of removing any foreign matter present inside the container 2. Also, as shown in FIG. 3(F-2), the container 2 may be turned upside down and sterile air may be blown into the container 2. FIG. In this case, foreign matter is more effectively removed than in the upright state. Furthermore, similar to the hydrogen peroxide water spray nozzle 31 in FIG. 3(E-2), by providing a guide member surrounding the air rinse nozzle 38, the hydrogen peroxide is introduced into the container 2 and overflows from the mouth 1a. The sterilized air collides with the guide member, rinsing the outer peripheral portion of the mouth portion 1a as well, thereby increasing the temperature of the outer peripheral portion of the mouth portion 1a and increasing the sterilization effect of the outer peripheral portion of the mouth portion 1a. The air rinse nozzle 38 may be vertically movable to blow sterile air into the container 2 .

The container 2 that has been air-rinsed by the air-rinsing section 34 is conveyed to the filling section 39 via a wheel 37 as shown in FIG. In the filling section 39, the filling wheel 40 shown in FIG. 1 fills the container 2 with the contents through the filling nozzle 42 as in the filling step shown in FIG. 3(G). The contents are sterilized in advance, and a certain amount of contents such as beverages are filled into the container 2 by a filling nozzle 42 that travels synchronously with the container 2 .

The aseptic filling machine includes a content preparation device and a content sterilization device for sterilizing the content.

The blending device is for blending beverages such as tea beverages and fruit beverages at desired mixing ratios, but since it is a known device, detailed description thereof will be omitted.

The filling section 39 has a large number of filling nozzles 42 arranged around a filling wheel 43 that rotates at high speed in a horizontal plane. A fixed amount of beverage is filled from the filling nozzle 42 into the container 2 traveling in synchronism with the peripheral speed of the filling wheel 43 .

The container 2 filled with contents is conveyed to the sealing section 44 via the filling wheel 43 shown in FIG. In the sealing wheel 45 provided in the sealing section 44, the lid material 3, which is a sealing member sterilized by the lid material sterilizing section 52, is sterilized by the sterilized lid material conveying path 54 as in the sealing step shown in FIG. It is supplied to the sealing wheel 45 via the lid material supply wheel 54a and the lid material receiving wheel 54b, and is wrapped around the opening 1a of the container 2 by a capper (not shown) to seal the container 2. As shown in FIG.

The sealed container 2 is placed on the discharge conveyor 50 by the discharge wheel 48 and discharged from the outlet 51 to the outside of the aseptic filling machine.

In the aseptic filling machine as described above, the container 2 sprayed with hydrogen peroxide gas or mist or a mixture thereof is discharged to the outside of the aseptic filling machine by a sterilized container rejector 58 provided in the aseptic filling machine. Immediately after the discharge, the container 2 is sealed with a sterilized lid member 3 so that the discharged container 2 is not contaminated with bacteria or the like. In a space such as a clean bench or a clean room where an aseptic atmosphere is maintained, the sealed container 2 is detached from the lid member 3, filled with a required amount of sterile water, and sealed with the sterilized lid member 3. - 特許庁

The amount of sterile water filled in the container 2 is 1/100 to 1 of the capacity of the container. If it is less than 1/100, the extraction of hydrogen peroxide becomes insufficient due to poor contact of water with the surface of the bottle. Alternatively, sterile water may be filled in an amount exceeding the capacity. For example, the mouth portion 1a of the container 2 may be filled up to the middle. In the case of partial fill volumes, it is preferred to shake the container 2 periodically during storage of the container 2 filled with sterile water.

Sterile water is water obtained by heating ion-exchanged water, distilled water, water filtered by an ultrafiltration membrane at a temperature of 120.1°C or higher for 4 minutes or more, or water filtered by a reverse osmosis membrane. It is water that does not contain organic substances, metal ions, bacteria, etc. The sterilized water to be filled in the container 2 is normal temperature, but it may be heated. Heating the sterilized water promotes the extraction of hydrogen peroxide adsorbed in the resin forming the container 2 into the sterilized water. The temperature to be heated is 40°C to 70°C. If the container 2 made of polyethylene terephthalate is filled with sterile water at a temperature exceeding 70° C., which is close to the glass transition point, the container 2 shrinks, making it difficult to accurately measure the amount of hydrogen peroxide.

The sterilized lid material 3 means spraying hydrogen peroxide water gas or mist or a mixture thereof, contacting with a liquid containing a compound having a sterilizing effect such as peracetic acid, sodium hypochlorite, ozone, The cover material 3 is sterilized by irradiation with electromagnetic waves having sterilizing ability such as rays and ultraviolet rays, exposure to ethylene oxide gas, or the like.

The container 2 filled with sterile water and sealed is stored at a predetermined temperature for a certain period of time. The defined temperature is room temperature or a temperature to be heated. Storage time can be shortened by heating. For example, by setting the temperature to 40° C. to 70° C., the storage time can be shortened to 1/10 to 1/50 compared to storage at room temperature. This is because heating promotes the extraction of hydrogen peroxide adsorbed in the resin forming the container 2 into sterile water. The certain period of time is, for example, 24 hours to 72 hours at room temperature. If the time is less than 24 hours, the hydrogen peroxide adsorbed in the resin constituting the container is not sufficiently extracted into sterile water. Moreover, exceeding 72 hours does not increase the amount of hydrogen peroxide extracted into sterile water, which is a waste of time.

The aseptic water in container 2 filled with aseptic water and stored for a certain period of time is measured for the amount of hydrogen peroxide by a measuring instrument that measures oxygen generated by decomposing hydrogen peroxide contained in the aseptic water with catalase using an electrode method. be. Catalase is an enzyme that rapidly decomposes hydrogen peroxide into oxygen and water. The oxygen generated here is measured by an electrode method, and the amount of decomposed hydrogen peroxide is measured. When measuring the amount of hydrogen peroxide by the electrode method, the sterile water must be 40°C or less, and if the sterile water is heated and stored, it must be cooled to 40°C or less. be.

Catalase is present in almost all aerobic microorganisms and is also present in some anaerobic microorganisms. Therefore, when the container 2 sprayed with hydrogen peroxide water gas or mist or a mixture thereof is filled with water containing microorganisms, the hydrogen peroxide is decomposed by catalase contained in the microorganisms before the amount of hydrogen peroxide is measured. There is a risk that the amount of hydrogen peroxide cannot be measured accurately. Therefore, aseptic water in which microorganisms such as fungi have been sterilized must be filled into the container 2 sprayed with hydrogen peroxide gas or mist or a mixture thereof.

When an enzyme is exposed to high temperatures, the three-dimensional structure of the active site changes and it ceases to function. It is thought that heating the water to a high temperature to sterilize the water does not cause the function of catalase contained in microorganisms such as bacteria contained in the water to be lost to decompose hydrogen peroxide. In addition, the death of microorganisms does not produce new enzymes. Although the water filtered by the reverse osmosis membrane is not heated, the sterilized water does not contain catalase because microorganisms such as bacteria are removed from the water.

Decomposition of hydrogen peroxide is accelerated by heat and light. In order to prevent decomposition, it is preferable not to heat and store the container 2 filled with sterile water. However, moderate heating is effective for shortening the storage time. Moreover, it is preferable to store the container 2 filled with sterile water in a light-shielded place.

Hydrogen peroxide water exhibits acidity, but is most stable at a pH of about 4, and decomposes at both high and low pH. Therefore, sterile water is preferably free of inorganic and organic acidic and basic substances that affect pH. Moreover, since hydrogen peroxide reacts with and decomposes various organic substances, the sterilized water preferably does not contain organic substances. Furthermore, it has been reported that hydrogen peroxide is decomposed by metal ions such as iron, copper, zinc, calcium and magnesium. Therefore, sterile water is preferably free of metal ions.

In addition to the oxygen electrode method in which hydrogen peroxide is decomposed by catalase and the amount of oxygen produced is measured, there is a method for measuring the amount of hydrogen peroxide by potassium permanganate titration, and by adding titanium sulfate to an aqueous solution containing hydrogen peroxide, A method of forming a complex compound of hydrogen and titanium ions and measuring the UV absorption spectrum of the complex compound as absorbance, after contacting a sample solution containing hydrogen peroxide with a platinum-supported hydrogen peroxide decomposition catalyst. A method of measuring the dissolved oxygen concentration in the treatment liquid with an optical oxygen sensor and measuring the amount of hydrogen peroxide in the sample solution from the dissolved oxygen concentration may also be used. Any method may be used as long as it is possible to quantify hydrogen peroxide.

In the aseptic filling machine, the container 2 sprayed with hydrogen peroxide water gas or mist or a mixture thereof is discharged outside the aseptic filling machine by a sterilized container rejector 58 provided in the aseptic filling machine, and the container 2 is discharged. Although the method for measuring the amount of hydrogen peroxide on the inner surface has been described, the amount of hydrogen peroxide may be measured for the container 2 as follows. The method for measuring the amount of hydrogen peroxide in the sterilized water filled in the container 2 is the same as the method described above.

The container 2 sprayed with hydrogen peroxide gas or mist or a mixture thereof in the container sterilization unit 30 of the aseptic filling machine is not air-rinsed by the air-rinsing unit 34 and is not filled with anything by the filling unit 39. Next, the container 2 is sealed with the cover material 3 sterilized in the sealing part 44, the sealed container 2 discharged from the outlet part 51 is filled with sterile water in a sterile atmosphere, and the container 2 filled with sterile water is After storage for a certain period of time, measure the amount of hydrogen peroxide in the sterile water.

The container 2 sprayed with hydrogen peroxide gas or mist or a mixture thereof in the container sterilization unit 30 of the aseptic filling machine is not air-rinsed in the air rinse unit 34, and sterile water is supplied from the filling nozzle 42 in the filling unit 39. , the container 2 is sealed with the lid material 3 sterilized in the sealing part 44, and after storing the sealed container 2 discharged from the discharge part 47 for a certain period of time, the amount of hydrogen peroxide in the sterile water is measured. As the sterile water to be filled in the filling section 39, sterile water obtained by a heat sterilization device for sterilizing the contents of the aseptic filling machine is used. In addition to the heat sterilization apparatus for sterilizing the contents, aseptic water obtained by a heat sterilization apparatus that manufactures aseptic water provided with an aseptic filling machine may be used. If the filling in the sterile water filling unit 39 is performed after the CIP processing and SIP processing of the content supply system pipe is completed and before the content is filled, the sample can be collected without contamination of bacteria and organic matter. This is preferable because it can be done.

The air rinsing unit 34 blows aseptic air to the container 2 sprayed with hydrogen peroxide gas or mist or a mixture thereof in the container sterilizing unit 30 of the aseptic filling machine, and the filling unit 39 does not fill anything. Then, the container 2 is sealed with the cover material 3 sterilized in the sealing part 44, the sealed container 2 discharged from the discharge part 47 is filled with sterile water in a sterile atmosphere, and the container 2 filled with sterile water is After storage for a certain period of time, measure the amount of hydrogen peroxide in the sterile water. Sterile air may be heated. By blowing sterilized air onto the container 2, the gas or mist of the hydrogen peroxide solution sprayed onto the container 2 or a part of the mixture thereof is dispersed and removed, but the hydrogen peroxide adsorbed onto the container 2 is removed. The remaining amount of hydrogen peroxide is to be measured.

The container sterilization unit 30 of the aseptic filling machine sprays hydrogen peroxide water gas or mist or a mixture thereof, and the air rinse unit 34 blows aseptic air, and the filling unit 39 sprays aseptic water from the filling nozzle 42. , the container 2 is sealed with the lid material 3 sterilized in the sealing part 44, and after storing the sealed container 2 discharged from the discharge part 47 for a certain period of time, the amount of hydrogen peroxide in the sterile water is measured.

In FIG. 1, the molded container 2 is sterilized by spraying a hydrogen peroxide solution gas or mist or a mixture thereof, and the preform 1 is sprayed with a hydrogen peroxide solution gas or mist or a mixture thereof. The present invention can also be applied to the measurement of the amount of hydrogen peroxide on the inner surface of the sterilized preform 1 by spraying a mixture of the above. The present invention is also applicable to a container 2 obtained by molding a sterilized preform 1. Furthermore, it is also applicable to sterilizing the preform 1, blow-molding the sterilized preform 1 into the container 2, and spraying the molded container 2 with gas or mist of hydrogen peroxide water, or a mixture thereof.

2 Container 3 Lid material 30 Container sterilization unit 31 Hydrogen peroxide gas spray nozzle 34 Air rinse unit 39 Filling unit 44 Sealing unit 47 Discharge unit 52 Lid material sterilization unit 55 Hydrogen peroxide water gas generation Vessel 58... Sterilization container rejector

Claims (2)

In an aseptic filling machine that sterilizes containers by spraying gas or mist of hydrogen peroxide water or a mixture thereof,
In the container sterilization section of the aseptic filling machine, aseptic air is blown in the air rinsing section to the container sprayed with the hydrogen peroxide gas or mist or a mixture thereof, and nothing is filled in the filling section. The container is sealed with a lid material sterilized in the sealing part, discharged from the discharge part,
removing the lid member sealing the discharged container in an aseptic atmosphere, filling the container with sterile water containing no metal ions in an aseptic atmosphere,
sealing the container filled with the sterile water with a lid material sterilized in a sterile atmosphere;
storing the sealed container for a certain period of time;
A method for measuring the amount of hydrogen peroxide on the inner surface of a container, comprising measuring the amount of hydrogen peroxide in the sterile water. In the method for measuring the amount of hydrogen peroxide in a container according to claim 1,
A method for measuring the amount of hydrogen peroxide on the inner surface of a container, wherein oxygen generated by decomposing the hydrogen peroxide in the sterile water with catalase is measured by an electrode method.

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