JPH10314276A - Freeze vacuum drying method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a freeze vacuum drying method which can be used in an emergency by maintaining a consistent sterilized state from a freeze vacuum drying process to the time of use. SOLUTION: In a plural-chamber separating container 1 in which chambers are separated by readily openable partition parts and coupled together, the chambers 2, 3 filled with contents not subjected to freeze vacuum drying are sealed, while the other chambers are filled with contents to be subjected to freeze vacuum drying; with the latter chambers opened, cooling is effected to freeze and hold the contents in a vacuum to freeze dry them, after which the chambers are sealed.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

FIELD OF THE INVENTION The present invention relates to a multi-chamber separation container in which separate chambers are filled with the contents to be freeze-dried and other contents,
The present invention provides a method for freeze-vacuum drying one of two substances filled in one container by freeze-vacuum drying.

[0002]

2. Description of the Related Art Conventionally, it has been widely practiced to mix a freeze-dried substance with a liquid at the time of use in medical parts and the like. Various methods for freeze-vacuum drying have been proposed, but there are no satisfactory methods yet. For example, a vial is filled with a chemical solution, solidified by a batch-type freeze-vacuum drying machine in a state of a half stopper of a rubber stopper, and sealed by a final stopper. 4 1
988. Japanese Patent Application Laid-Open No. 5-306216 proposes that a chemical solution is filled in a plastic container, solidified by a batch-type freeze vacuum drying machine, and sealed by heat sealing with a plastic film or the like. However, if the material thus freeze-dried and vacuum-dried is filled in one container, it must be opened at the time of use and the liquid filled in the other container must be injected, so that it is impossible to mix under aseptic conditions, There is a problem that the use is complicated and it is difficult to use in an emergency. Further, a metal tray is filled with the content to be dried and dried by moving it on a plate at a different temperature in a vacuum to dry by a continuous freeze vacuum drying machine.
7-5641. This method requires a step of filling a dried substance into a container, a step of opening the container at the time of use and injecting a liquid filled in another container, and it is difficult to maintain a sterile state, and furthermore, it is difficult to use in an emergency. is there. Japanese Patent Application Laid-Open No. 4-36485 discloses a method in which a chemical solution is subjected to a batch-type freeze-vacuum drying treatment, and the container is filled and sealed in a multi-chamber separation container.
Although this is proposed in Japanese Patent Publication No. 1 (Kokai), there is also a problem that it is difficult to maintain an aseptic state since a step of filling a dried substance into a plurality of separation chamber containers is required.

[0003]

SUMMARY OF THE INVENTION The present invention secures a sterile state consistently from the freeze-drying step to the time of use, improves the micro-filling of the freeze-dried product and stabilizes the filling amount, and maintains the sterility during use. A freeze-vacuum drying method using a multi-compartment separation vessel capable of rapidly and easily preparing a solution is provided.

[0004]

According to the present invention, there is provided a method for sealing a chamber filled with contents which are not subjected to freeze-vacuum drying in a multi-chamber separation container which is separated and connected by an easily-openable partition. A freeze-vacuum drying method, characterized in that the chamber is filled with the contents to be subjected to freeze-vacuum drying, and in a state where the chamber is opened, the contents are cooled, the contents are frozen, kept in vacuum, freeze-dried, and then sealed. Sealing a chamber filled with aseptic contents not subjected to freeze-vacuum drying in a sterile multi-chamber separation container, and then filling other chambers with aseptic contents subjected to freeze-vacuum drying in a sterile environment,
The freeze-drying method according to item 1. 3. The chamber filled with the contents not subjected to freeze-vacuum drying is sealed, and then the entire multi-chamber separation container is sterilized, and then the other chamber is filled with the sterile contents subjected to freeze-vacuum drying.
Freezing vacuum drying method described in the paragraph. 4. 4. The freeze-vacuum drying method according to any one of claims 1 to 3, wherein the contents of the multi-chamber separation container not subjected to freeze-vacuum drying are also frozen in a sealed state. 5. 5. The freeze-vacuum drying method according to any one of items 1 to 4, wherein the contents to be subjected to freeze-vacuum drying have been previously sterilized. 6. 6. The freeze vacuum drying method according to any one of items 1 to 5, wherein an inert gas is introduced into the chamber of the container in the step of filling and sealing. 7. 0.5kg / 15mm-1.2 for multi-chamber separation container
7. The freeze vacuum drying method according to any one of items 1 to 6, which is a container having an easy-opening partition having a weak sealing strength of Kg / 15 mm. 8. Multi-chamber separation container is 1.3Kg / 15mm-3.0
The freeze-drying method according to any one of Items 1 to 7, which is a container having a peripheral portion having a sealing strength of Kg / 15 mm. 9. The freeze-vacuum according to any one of items 1 to 8, wherein the freeze-vacuum drying treatment is a treatment that is continuously performed by sequentially passing a plurality of treatment chambers having a controlled temperature and pressure through a plurality of separation chambers. Drying method. 10. 9. The freeze-vacuum drying method according to any one of items 1 to 8, wherein the freeze-vacuum drying treatment is a batch treatment in which the treatment is performed by sequentially changing the treatment temperature and pressure of the treatment device containing the multi-chamber separation container. 11. 11. The freezing vacuum according to any one of items 1 to 6, or 9 or 10, wherein the peripheral portion and the partition portion of the multi-chamber separation container are held and reinforced by a reinforcing jig during freezing and freeze-vacuum drying is performed. Drying method. 12. 12. The freeze-vacuum drying method according to any one of items 1 to 11, wherein the freeze-vacuum drying is performed while preventing the transfer of heat to contents that are not subjected to freeze-vacuum drying. 13. Freezing vacuum drying method The freeze vacuum drying method according to any one of items 1 to 12, wherein the contact area of the frozen contents with the drying atmosphere is increased to promote the sublimation of the frozen water. . About.

[0005]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS In the present invention, a multi-chamber container is used. This container is composed of a plurality of chambers, and the chambers are separated from each other by an easily-openable partition so that the contents are mixed during storage. This is because, at the time of use, the partition can be easily opened and the contents can be mixed without opening the container. The contents to be filled into a certain chamber of the multi-chamber separation container and not subjected to freeze-vacuum drying are, for example, a liquid that dissolves or freezes the freeze-dried contents. Since a chamber filled with contents not subjected to freeze-vacuum drying is not dried, it is reasonable to seal and pass through the freeze-vacuum drying step. By sterilizing the entire container, bacteria are prevented from being introduced from the container in subsequent steps. The sterilization method is not particularly limited, but a pressurized moist heat method, an ultraviolet irradiation method, a chemical method, an ozone method, an electron beam irradiation method and the like are appropriately used.

Next, the contents to be subjected to freeze-vacuum drying are filled in the empty room, cooled in the opened state and frozen, but the whole container is sterilized, so that the aseptic state is maintained. Filling and freeze vacuum drying are preferably performed in a sterile environment. Since the content to be subjected to freeze-vacuum drying is filled in a liquid state, by adjusting the liquid concentration, it is possible to easily fill a small amount of the freeze-vacuum-dried product and stabilize the filling amount. If an inert gas is introduced into the chamber of the container and oxygen is expelled in the step of filling and sealing, the storage stability is improved. If the contents to be subjected to freeze-vacuum drying are sterilized in advance, the effect of ensuring a sterile state is great. By maintaining the vacuum after freezing, the frozen water is sublimated and dried. In the present invention, the contents that are not subjected to freeze-vacuum drying may be frozen, or heat may be prevented from being transferred to the contents by, for example, a heat insulating material or the like.

The multi-chamber container used in the present invention includes, for example, a multi-chamber tray having a sheet-forming single-layer or laminated sheet having an easily-opening partition, a multi-chamber separation container having an extrusion-molded easy-opening partition, and the like. A container formed of at least two layers of laminated plastic films and having large and small chambers separated by a joining portion, wherein the joining force of the inner plastic layer separating and dividing the container into the large and small chambers has an inner layer and an outer surface. A container such as a multi-chamber separation container is used, which is larger than the adhesive force for laminating the layers, and is characterized in that cuts are respectively provided in the inner layers of both chambers. The partition of each chamber is an easily openable partition, and can be formed, for example, by laminating and sealing a combination of a synthetic resin forming a container and a synthetic resin having low adhesiveness. Examples of combinations of plastic layers forming a bonding surface having a low bonding force include polyethylene and polypropylene, a blend of polypropylene and polypropylene, a copolymer of a polypropylene-based polymer and a styrene-based thermoplastic elastomer, polyethylene and PE-PP-St. And a copolymer of polypropylene and an ethylene-olefin copolymer elastomer.

Preferably, the sealing strength of the partition is 0.5 kg.
/15mm-1.2Kg/15mm, 0.5Kg
/ 15mm or less, the internal pressure rises during freeze vacuum drying,
If the partition is broken and the contents that are not subjected to freeze-vacuum drying are also freeze-dried, easy communication becomes difficult at 1.2 kg / 15 mm or more. Also, a container formed of at least two layers of plastic laminated film and composed of large and small chambers separated and divided by a joint portion, wherein the joining force of the inner plastic layer separating and dividing the container into large and small chambers is equal to the inner layer. In the case of a container such as a multi-chamber separation container which is larger than the adhesive force for laminating the outer layer and is provided with cuts in the inner layer of both chambers, the sealing strength of the partition is 0.5 kg / 15 mm. Above is necessary, and if it is 0.5 kg / 15 mm or less, the partition portion is damaged due to the increase of the internal pressure during freeze-vacuum drying, and the contents that are not freeze-vacuum-dried are also freeze-dried, making it difficult to use. By making the partition part easily openable in this way, when pressure is applied to the container from the outside at the time of use, the partition part opens and the contents are mixed, so that mixing can be performed without opening the container and sterile state in an emergency There is an advantage that it can be used immediately while keeping the same. 1.3Kg / 15mm-3.0K perimeter of multi-chamber separation chamber
g / 15mm sealing strength, but 1.3Kg / 15m
If it is less than m, there is a risk that the peripheral portion will open when the partition is opened during use, and a strength of 3.0 kg / 15 mm or more is not required.

The freeze-vacuum drying treatment may be performed continuously or in a batch system. In the case of continuous processing, it may be passed through a plurality of processing zones with adjusted temperature and pressure, and the freeze and drying may be performed continuously.In the case of batch processing, the temperature and pressure of the processing apparatus containing the containers are sequentially adjusted. Change and freeze and dry. When performing freezing vacuum drying, if the contact area between the vacuum atmosphere and the frozen material is increased, the sublimation of the frozen water is promoted, so that the effect of shortening the drying time is great. As a method of increasing the contact area of the frozen material, a method of applying a stress to the frozen material from outside the container and crashing the frozen material, holding the opening of the container with a jig, and pressing the jig in a direction to shrink the opening. A method by which a jig is provided so that the opening of the container is not closed before freezing, and a sterile gas is introduced from the opening after freezing, thereby opening a gap between the frozen material and the container wall. Can be

In addition, since the partitioning portion and the peripheral portion of the container may be opened due to an increase in volume during freezing, it is preferable to use a reinforcing jig for holding and protecting the sealing portion. In this case, there is an advantage that the partition does not open due to malfunction during handling even if the sealing strength of the partition is 0.5 kg / lower. When a reinforcing jig is used for the partition, the sealing strength of the partition is 0.2 kg / l.
It is preferably from 5 mm to 1.2 kg / 15 mm,
If it is less than 0.2 kg / 15 mm, the partition part will be damaged during transportation, and the medicine separated in multiple chambers will be mixed, making it difficult to use.
If it is 2 kg / 15 mm or more, easy communication during use becomes difficult.

[0011]

EXAMPLES Next, the present invention will be specifically described with reference to examples.

Used Container The container shown in FIG. 1 is a container, which is separated into a large capacity chamber 2 and a small capacity chamber 3 by a joint 6.
4 is a cut provided in the inner layer of the large capacity chamber, and 5 is a cut provided in the inner layer of the small capacity chamber. The cut is formed in a straight line along the joint and in accordance with the shape of the joint. Reference numeral 5 is provided near the junction. Reference numeral 10 denotes a joint located at the periphery of the container. If this portion has a weak bonding force, there is a risk of liquid leakage.

FIG. 2 shows a longitudinal section of the container shown in FIG. A tab 7 is provided at a position near the joint on the outer surface of the small chamber 3. FIG. 3 is an enlarged view of a joint portion of the container of the present invention. The inner surface layer 9 is joined to each other at a joint portion 6 to be partitioned into both chambers. In this example, the seal portion 11 is formed by heat sealing. In this example, an inner and outer laminated film is used. The inner surface layer 9 is laminated and adhered to the outer surface layer 8, and 12 is a bonded portion between them. Reference numeral 4 denotes a notch provided in the inner layer of the large-capacity chamber and reaches a bonding portion with the outer layer. Reference numeral 5 denotes a notch provided in the inner layer of the small capacity chamber, which reaches the bonding portion with the outer layer, and is provided near the bonding portion 6. When the small-capacity chamber is pressurized, the internal pressure is applied to the inner surface, but the bonding portion 6 does not peel and is not opened because the bonding force is large. On the other hand, the internal pressure acts as a peeling force between the inner layer and the outer layer through the cut 5 of the small chamber. Since the bonding strength between the inner layer and the outer layer is smaller than the bonding strength of the bonding portion 6, both layers are easily separated. When the tab provided on the outer layer of the small chamber is pulled while applying pressure to the small chamber in this way, the tension of the tab is applied to the outer layer. Since it acts as a force, delamination occurs. When the generated delamination extends and reaches the cut 4 of the large capacity chamber, a communication path is formed between the inner and outer layers, and the contents of both chambers are mixed. As described above, the pressurization of the small capacity chamber and the pulling of the tab are two.
Since the opening is performed by a combination of the two means, the opening due to an erroneous operation such as pressurization and dropping during distribution is prevented. The multi-chamber separation container used in the present invention is formed, for example, by subjecting a 50 μm polypropylene homopolymer (PP) film to a 25 μm linear low-density polyethylene (LLDPE) film provided with cuts at predetermined positions by heat bonding at 180 ° C. A laminate of PP / LLDPE was formed. L of this laminate
LDPE with an inner surface of 100mm x 240mm
Room separation container, the large room of this container is 100 mm x 1
The chamber was 30 mm and 100 mm x 110 mm.

When the partition reinforcing jig 13 shown in FIG. 4 is used, the sealing strength of the partition can be reduced to 0.5 kg / 15 mm or less. Numeral 14 denotes two press-offs, and when the opposing surfaces are brought into contact with each other in a convex shape, the pressing force is linearly applied and the reinforcing effect is increased. Reference numeral 15 denotes a holding tool which holds the holding plate so as to be detachable. The holding tool only needs to be able to hold the pressed state of the holding plate, and other suitable members are used.

FIG. 5 shows a state in which a reinforcing jig 13 is attached to a partition portion of the multi-chamber separation container. Since the reinforcing jig is detachably attached in this manner, it can be easily removed at the time of opening. When the reinforcing jig is used, the sealing strength of the partition portion can be reduced, so that the opening during use becomes easy.

Freezing vacuum dryer Freezing vacuum dryer is a throw-in cooler (ECS-80C)
Programmed low-temperature constant temperature bath (NCB-340)
0) (Freon-based medium: F)
C-77) was introduced into a multi-chamber separation vessel stage (stage angle: 0 to 20 degrees) in a freeze-vacuum dryer, and then cooled to -50 ° C.
A freezing vacuum drying (model FDU-830, vacuum pump: GCD-1305XAN) manufactured by Tokyo Rika, which was modified so that the temperature could be adjusted to any temperature from to 50 ° C. Freezing vacuum dryer (FDU-830 type) manufactured by Tokyo Rika Oil rotary pump (GCD-1305XAN) Programmed precision low temperature oven (NCB-3400) Throw-in cooler (ECS-80C) Multi-chamber separation vessel stage (stage angle: 5 to 20) Degree) Medium: FC-77 (Freon type)

Example 1 A 50 μm polypropylene homopolymer (hereinafter referred to as PP) film and a 25 μm film having a cut at a predetermined position were provided.
m low-density linear low-density polyethylene (hereinafter referred to as LLDPE) film at 180 ° C by heat bonding.
A laminate of DPE was formed. Furthermore, a 12 μm biaxially stretched polyethylene terephthalate film (hereinafter referred to as PET) was bonded to the PP side of PP / LLDPE via a urethane-based adhesive to form a three-layer laminate of PET / PP / LLDPE. With the LLDPE of this laminate as the inner surface, the sealing strength at the periphery is 2.3 kg / 15 mm, and the outer size is 1 kg.
It is a two-chamber separation container of 00 mm × 240 mm, the large room is 100 mm × 130 mm, and the small room is 100 mm × 110.
mm, a container consisting of two chambers provided with tabs on the outer layer was molded, 50 ml of water was poured into the large chamber of the container, the container was sealed, and the entire container was irradiated with ultraviolet light and sterilized.
Was placed in a freeze-vacuum drier, and freeze-vacuum drying was performed under the condition of FIG. 4 in a state where the compartment was opened. Cooled from room temperature 20 ° C to -45 ° C and kept at this temperature for 2 hours. The pressure was reduced to a degree of vacuum of 0.04 torr. After 2 hours, the temperature is raised to -5 ° C and the degree of vacuum is set to 0.0
Vacuum drying is performed while maintaining this state at 4 torr for 8 hours. Then maintain the degree of vacuum as it is and keep the temperature at 20 ° C.
After 2 hours, the temperature rises to 45 ° C and after 2 hours 2
Lower to 0 ° C., hold for 6 hours, then return to atmospheric pressure. Next, the opening of the small chamber containing the dried and powdered coffee particles was heat-sealed and packaged. By pulling the tab of the multi-chamber separation container separately storing the water and the powdered coffee, the weakly joined surface of the easily-openable partition portion was peeled off, and the water and the coffee powder were mixed to obtain a coffee liquid.

Example 2 The procedure of Example 1 was repeated except that the sealing strength of the partition was 0.5 kg / 15 mm. The two-chamber separation container was capable of performing freeze-vacuum drying of the coffee liquid without causing breakage of the partition portion and the peripheral portion.

Example 3 The procedure of Example 1 was repeated except that the sealing strength of the partition was 1.0 kg / 15 mm. The two-chamber separation container was capable of performing freeze-vacuum drying of the coffee liquid without causing breakage of the partition portion and the peripheral portion.

Example 4 Example 4 was the same as Example 1 except that the sealing strength at the periphery was 0.7 kg / 15 mm. The two-chamber separation container was capable of performing freeze-vacuum drying of the coffee liquid without causing breakage of the partition portion and the peripheral portion.

Example 5 The procedure of Example 1 was repeated except that the sealing strength at the periphery was set at 1.0 kg / 15 mm. The two-chamber separation container was capable of performing freeze-vacuum drying of the coffee liquid without causing breakage of the partition portion and the peripheral portion.

Example 6 The sealing strength of the partition part was 0.2 kg / 15 mm, and the partition reinforcing jig shown in FIG. 4 was used for the partition part. The ascorbic acid aqueous solution was freeze-dried and vacuum-dried in the same manner as in Example 1 using the multi-chamber separation container shown in Example 1 except that the aqueous solution of ascorbic acid powdered by vacuum drying was used. As a result, a freeze-vacuum-dried powder of ascorbic acid was produced without any problems such as breakage of the partition portion and the peripheral portion.

Example 7 The sealing strength of the partition was 0.4 kg / 15 mm, and the partition reinforcing jig shown in FIG. 4 was used for the partition. The ascorbic acid aqueous solution was freeze-dried and vacuum-dried in the same manner as in Example 1 using the multi-chamber separation container shown in Example 1 except that the aqueous solution of ascorbic acid powdered by vacuum drying was used. As a result, a freeze-vacuum-dried powder of ascorbic acid was produced without any problems such as breakage of the partition portion and the peripheral portion.

Example 8 The sealing strength of the partition was 0.6 kg / 15 mm, and the partition reinforcing jig shown in FIG. 4 was used for the partition. The ascorbic acid aqueous solution was freeze-dried and vacuum-dried in the same manner as in Example 1 using the multi-chamber separation container shown in Example 1 except that the aqueous solution of ascorbic acid powdered by vacuum drying was used. As a result, a freeze-vacuum-dried powder of ascorbic acid was produced without any problems such as breakage of the partition portion and the peripheral portion.

Example 9 A flanged 2 was formed from an LLDPE sheet by a vacuum molding method.
A continuous tray was molded. The size of the tray is 90 x 70 x 15
mm (inner size: 70 × 55 × 15 mm), and the outer size of a small chamber filled with an ascorbic acid aqueous solution to be subjected to freeze vacuum drying treatment is 90 × 40 × 15 mm (inner size: 70 × 25 × 15 m).
In m), the flange has a width of 10 mm. The lid material is a PE in which a notch is provided at a predetermined position of the LLDPE used in Example 1.
T / PP / LLDPE was used. 50m of water in the large room of the container
, fill the LLDPE, seal, and sterilize the container and water by UV irradiation. A sterile 17wt filtered through a filter into a small chamber sealed on both sides with the lid of the container
5 ml of an ascorbic acid aqueous solution was filled from the unsealed flange portion. The sealing strength of the peripheral part of this container was 2.3 kg / 15 mm, and the sealing strength of the partition part was 1.0 kg / 15 mm. As a result of performing the freeze-vacuum drying process using the freeze-vacuum dryer shown in Example 1, water that is not freeze-vacuum-dried without problems such as damage to the peripheral portion and the partition portion and freeze-vacuum-dried ascorbic acid powder are produced. Then, the unsealed flange portion of the small chamber of the container in which the ascorbic acid powder was produced was sealed.

Example 10 During the freeze-vacuum drying, the flange portion of the large chamber filled with water is held by a Teflon jig, and the container is not in contact with the multi-chamber separation container stage of the freeze vacuum dryer. The freeze-drying was performed in the same manner as in Example 5 except that the sample was freeze-dried. The water in the room was not frozen during the freeze vacuum drying process and was treated. As a result, water which was not freeze-vacuum dried and ascorbic acid powder which was freeze-vacuum dried without problems such as breakage of the peripheral portion and the partition portion were produced.

Example 11 During freezing vacuum drying, a jig for holding both ends of the opening of the small chamber is used to freeze the coffee liquid filled in the small chamber and then hold both ends of the opening of the small chamber. Performed except that the opening area of the small chamber was increased by shrinking the jig, and a gap was provided between the frozen coffee liquid and the wall of the multi-chamber separation container that was not in contact with the multi-chamber separation container stage. A freeze-vacuum drying treatment was performed in the same manner as in Example 1. As a result, the multi-chamber separation container could freeze-vacuum dry the coffee liquid in a very short time without any problems such as breakage of the partition and the peripheral edge.

Comparative Example 1 The procedure of Example 1 was repeated except that the sealing strength of the partition was 0.4 kg / 15 mm. The partition part of the two-chamber separation container was peeled off during the freeze-vacuum drying, and the freeze-drying of the coffee liquid in the separated state of the two liquids could not be performed.

Comparative Example 2 The procedure of Example 1 was repeated except that the sealing strength at the periphery was set at 0.4 kg / 15 mm. In this two-chamber separation container, the periphery for sealing the water not subjected to freeze-vacuum drying during freeze-vacuum drying was damaged, and the water was freeze-vacuum-dried.

[0030]

According to the present invention, there is provided a freeze-vacuum drying method which can ensure a sterile state consistent from the freeze-vacuum drying step to the time of use and can be used promptly even in an emergency.

[Brief description of the drawings]

FIG. 1 is a plan view of a multiple separation chamber container used in the present invention.

FIG. 2 is a cross-sectional view of a multiple separation chamber container used in the present invention.

FIG. 3 is an enlarged view of a partition portion of the multiple separation chamber container used in the present invention.

FIG. 4 is a perspective view of a partition part reinforcing jig used in the present invention.

FIG. 5 is an explanatory view of an embodiment in which a partition part reinforcing jig is used for a multi-chamber separation container.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Container 2 Large-capacity room 3 Small-capacity room 4 Large-capacity room side cut 5 Small-capacity room side cut 6 Joint 7 Tab 8 Outer layer 9 Inner layer 10 Peripheral laminated part 11 Inner layer joint 12 Inner and outer layer joint 13 Partition reinforcement Tool 14 Holding plate 15 Holder

Claims (13)

[Claims] 1. A multi-chamber separation container separated and connected by an easy-opening partition portion, the chamber filled with the content not subjected to freeze-vacuum drying is sealed, and the other chamber is filled with the content subjected to freeze-vacuum drying. A freeze-vacuum drying method, characterized in that in a state where the chamber is opened, the contents are cooled, the contents are frozen, kept in vacuum, freeze-dried, and then sealed. 2. A chamber filled with sterile contents not subjected to freeze-vacuum drying in a sterile multiple separation container is sealed, and then the other chamber is filled with sterile contents subjected to freeze-vacuum drying in a sterile environment. A freeze-vacuum drying method according to claim 1. 3. A chamber filled with contents that are not subjected to freeze-vacuum drying is sealed, and then the whole multi-chamber separation container is sterilized, and then the other chamber is filled with sterile contents subjected to freeze-vacuum drying. A freeze-vacuum drying method according to claim 1. 4. The method according to claim 1, wherein the contents of the multi-chamber separation container which are not subjected to freeze-drying are also frozen in a sealed state.
The freeze-drying method according to any one of claims 1 to 4. 5. The freeze-vacuum drying method according to claim 1, wherein the contents subjected to freeze-vacuum drying have been sterilized in advance. 6. The freeze-vacuum drying method according to claim 1, wherein an inert gas is introduced into the chamber of the container in the step of filling and sealing. 7. The multi-chamber separation container is 0.5 kg / 15 mm.
The freeze-vacuum drying method according to any one of claims 1 to 6, which is a container having an easy-opening partition having a weak sealing strength of ~ 1.2 kg / 15 mm. 8. The multi-chamber separation container has a capacity of 1.3 kg / 15 mm.
The freeze-vacuum drying method according to any one of claims 1 to 7, wherein the container has a peripheral portion having a sealing strength of ~ 3.0 kg / 15 mm. 9. The method according to claim 1, wherein the freeze-vacuum drying treatment is a treatment that is continuously performed by sequentially passing the plural-chamber separation container through a plurality of treatment zones whose temperature and pressure are adjusted. The described freeze vacuum drying method. 10. The process according to claim 1, wherein the freeze-vacuum drying process is a batch process in which the processing is performed by sequentially changing the processing temperature and pressure of the processing apparatus containing the multi-chamber separation container. Freeze vacuum drying method. 11. The freeze-drying method according to claim 1, wherein during the freezing, the peripheral portion and the partition portion of the multi-chamber separation container are held and reinforced by a reinforcing jig and freeze-vacuum drying is performed. Freeze vacuum drying method. 12. The freeze-vacuum drying method according to claim 1, wherein the freeze-vacuum drying is performed while preventing the transfer of heat to contents not subjected to the freeze-vacuum drying. 13. The freezing method according to claim 1, wherein the freezing and vacuum drying are performed to increase the contact area of the frozen contents with the drying atmosphere to promote sublimation of the frozen water. Vacuum drying method.