Air permeable freeze-drying tube for aseptic freeze-drying
By designing a breathable freeze-drying tube and adopting a combination of breathable holes and waterproof breathable components, the problems of material contamination and loss during the freeze-drying process are solved, achieving high-efficiency breathability and quality assurance in aseptic freeze-drying.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- SUZHOU XIANJUE BIOTECHNOLOGY CO LTD
- Filing Date
- 2025-06-09
- Publication Date
- 2026-07-03
AI Technical Summary
During freeze-drying, especially for small-volume samples, existing technologies struggle to achieve both sterility and air permeability, leading to increased material loss and contamination risks, particularly during vacuum sublimation and air input processes.
A breathable freeze-drying tube for sterile freeze-drying was designed. The tube cap has a vent and is equipped with a waterproof and breathable component. It is fixed by an annular support structure. The waterproof and breathable component allows water to pass through in one direction. It is combined with a hydrophobic and breathable membrane material to ensure sterility and breathability. The tube cap and tube body are connected by threads.
The freeze-drying process effectively reduces material contamination and loss, improves product quality, and ensures the effect of aseptic freeze-drying.
Smart Images
Figure CN224455149U_ABST
Abstract
Description
Technical Field
[0001] This utility model belongs to the field of freeze-drying technology, specifically relating to a breathable freeze-drying tube for sterile freeze-drying. Background Technology
[0002] Freeze-drying, also known as lyophilization, is a technology that removes moisture from wet materials by freezing them at low temperatures and then sublimating the water into a gaseous state under vacuum. A wide variety of materials require freeze-drying, covering fields such as pharmaceuticals, food, biopharmaceuticals, and chemicals. During freeze-drying, ensuring material purity requires strict control over multiple aspects, including environmental management, material loading, material distribution, freeze-drying parameters, personnel operation, and material packaging. However, in practice, since most materials require aseptic processing, the containers used for processing must be completely sealed during the transfer to the freeze dryer after dispensing and during the post-freeze-drying packaging process. However, the vacuum sublimation step during freeze-drying necessitates that the containers not be completely sealed. Furthermore, the airflow introduced during the release of the vacuum in the freeze dryer can lead to unnecessary material loss and mixing between different materials. Especially in the freeze-drying process of small volume samples below 2ml, the current solutions to the above problems mainly focus on: 1. using vials as containers and using a fully automated freeze-drying system; 2. using EP tubes and adopting a semi-tight capping method, strengthening the environment and conducting strict operation training and assessment for personnel to ensure the cleanliness of the working environment. Otherwise, the semi-tight capping method has a high contamination rate, but the cost and effort invested are greatly increased.
[0003] Therefore, in view of the above-mentioned technical problems, it is necessary to provide a breathable freeze-drying tube for sterile freeze-drying.
[0004] The information disclosed in this background section is intended only to enhance the understanding of the overall background of this utility model and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Utility Model Content
[0005] The purpose of this invention is to provide a breathable freeze-drying tube for sterile freeze-drying.
[0006] To achieve the above objectives, the technical solution provided by a specific embodiment of this utility model is as follows:
[0007] A breathable freeze-drying tube for sterile freeze-drying includes a tube cap, a tube body with an opening, and a waterproof and breathable component. The tube cap has a vent hole. The waterproof and breathable component is fitted to the inside of the tube cap to isolate the opening of the tube body from the vent hole. The waterproof and breathable component allows moisture to pass through the opening to the vent hole. The tube cap is fitted with a support structure that restricts the waterproof and breathable component. The support structure includes at least a hollow annular body circumferentially disposed on the inner side of the inner wall of the tube cap. The annular body includes at least a first platform for engaging the waterproof and breathable component.
[0008] In one or more embodiments of this utility model, the waterproof and breathable component has a first bend portion formed outside the inner circumference of the first surface (the inner circumference refers to the outermost edge of the hollow structure of the annular body), and the first bend portion extends along the inner wall of the tube cap from the annular body toward the tube body.
[0009] In one or more embodiments of the present invention, the waterproof and breathable component also has a first bend at the outermost periphery of the first tabletop (the outermost periphery refers to the position of the inner wall of the connecting pipe cover).
[0010] In one or more embodiments of this utility model, the outermost periphery of the first bend is non-circular (non-circular characteristics mean that when the first bend is in a flat state, the outermost edge does not have a complete circle feature, and may have serrations, wavy shapes and other non-circular defect shapes, etc., which may be regular or irregular).
[0011] In one or more embodiments of this utility model, the fit between the annular body and the waterproof and breathable component is a suspended fit: the inner diameter of the tube cap in the plane where the first platform is located is R1, and the outer periphery of the first platform restricts the minimum first outer diameter R2, where R2≤R1.
[0012] In one or more embodiments of this utility model, the waterproof and breathable component is a hydrophobic and breathable semi-permeable membrane.
[0013] In one or more embodiments of the present invention, the vent is defined by a first edge of the top of the cap, the first edge defining a first hollow portion that extends through the top of the cap.
[0014] In one or more embodiments of this utility model, a plurality of ribs are further defined within the first hollow portion, and at least a portion of the ends of the ribs are connected to the first edge. When the ribs include structures with multiple different orientations, some of the ribs may intersect.
[0015] In one or more embodiments of this utility model, the cap and the body are connected by threads. Preferably, the inner wall of the cap has an internal thread structure for threaded connection with the body. The outer wall of the body at the opening has an external thread structure for threaded connection with the cap.
[0016] In one or more embodiments of this invention, at least a portion of the outer wall of the cap and / or the body of the tube is formed with a non-smooth functional portion. Preferably, the surface of the functional portion is formed with a pattern or unevenness to facilitate anti-slip and gripping.
[0017] Compared with the prior art, the breathable freeze-drying tube of this utility model for sterile freeze-drying is used in the freeze-drying process. Through the double isolation and breathable structure design, it can ensure drainage during the vacuum freeze-drying process, while also helping to reduce pollution and loss in the freeze-drying process and improve product quality. Attached Figure Description
[0018] To more clearly illustrate the technical solutions in the embodiments of this utility model or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in this utility model. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0019] Figure 1 This is a perspective view of a breathable freeze-drying tube for sterile freeze-drying in one embodiment of the present invention.
[0020] Figure 2 This is a front view of a breathable freeze-drying tube for sterile freeze-drying in one embodiment of the present invention;
[0021] Figure 3 This is a schematic diagram of the cap structure of a breathable freeze-drying tube for sterile freeze-drying in one embodiment of the present invention.
[0022] Figure 4 This is a top view of the cap of a breathable freeze-drying tube for sterile freeze-drying in one embodiment of the present invention.
[0023] Figure 5 This is a schematic diagram of the internal structure of the cap of a breathable freeze-drying tube for sterile freeze-drying in one embodiment of the present invention.
[0024] Figure 6 A comparative diagram showing the effect of tumor peri-tumor fibroblast (CAF) cell culture using a breathable freeze-drying tube for sterile freeze-drying in one embodiment of this utility model.
[0025] Figure 7 This image shows a comparison of the effects of primary human umbilical vein endothelial cells (HUVECs) cultured in a breathable freeze-drying tube used for sterile freeze-drying in one embodiment of this invention. Detailed Implementation
[0026] To enable those skilled in the art to better understand the technical solutions of this utility model, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this utility model, and not all embodiments. Based on the embodiments of this utility model, all other embodiments obtained by those skilled in the art without creative effort should fall within the protection scope of this utility model.
[0027] like Figure 1-5 As shown, in one embodiment of this utility model, a breathable freeze-drying tube for sterile freeze-drying includes a tube cap 1. The tube cap 1 has a vent structure on its upper part for water to pass through during vacuum sublimation in the freeze-drying process. A layered waterproof and breathable component 3 is disposed inside the tube cap 1 to ensure that sublimated water is discharged unidirectionally from the inside of the tube to the outside during the freeze-drying process. To support the waterproof and breathable component 3, a supporting structure 12 is provided inside the tube cap 1. The supporting structure may be circumferentially disposed on the inner side of the inner wall of the tube cap (in this case, it can be as follows: ...). Figure 5 As shown in b, it can be set along the inner mark of the pipe cap, or it can be set off from the inner wall as shown in a. In this case, the hollow annular body (R2≤R1) includes a first platform for joining the waterproof and breathable parts. That is, the waterproof and breathable parts can be connected to the first platform by means of adhesive, welding or other methods to form a fixed structure.
[0028] As a preferred option, the waterproof and breathable component can be a membrane made of expanded polytetrafluoroethylene (e-PTFE) with hydrophobic and breathable properties, such as a filter membrane with 0.22μm micropores. This provides sterile gas exchange within the tube body 2, increases the permeability of gases such as air, carbon dioxide, and water vapor, and the hydrophobic filter membrane does not affect the sealing and breathability after contact with liquid, reducing the risk of contamination.
[0029] As a preferred embodiment, the outer surface of the side wall of the pipe cap 1 has an anti-slip pattern 13 to prevent slippage when opening and unscrewing the cap. The inner surface of the side wall of the pipe cap 1 has a threaded structure to connect with the thread at the opening of the pipe body 2.
[0030] As a preferred option, such as Figure 5The waterproof and breathable component shown in Figure b has a first bend 31 formed outside the inner circumference of the first platform. The first bend 31 extends from the annular body towards the tube body along the inner wall of the tube cap. The size of the first bend 31 can be determined according to the product size specifications and sealing effect, such as folding the edge of a filter membrane with 0.22μm micropores by 0.2mm. That is to say, the edge of the first bend 31 can be in a folded state, thereby satisfying the effect of compression reinforcement and having stronger adaptability to changes in internal pressure during vacuum freeze drying. At this time, in order to reduce the unevenness caused by folding, the outermost circumference of the first bend can be a non-smooth shape such as serrated or wavy.
[0031] As a preferred option, such as Figure 4 The vent shown has a first edge 14 at the top of the cap, which defines a first hollow portion extending through the top of the cap. A plurality of ribs 15 are also defined within the first hollow portion, with at least a portion of the ends of each rib 15 connected to the first edge 14. When the ribs include structures in multiple different directions, some of the ribs may intersect. The dimensions of diameters D1 and D2, and width L, etc., in the figure are determined according to the specific product design requirements, as long as they meet specific perforation and ventilation needs. For example, D1 can be 12.8±0.2mm, D2 can be 7.0±0.2mm, and L can be 1.0±0.1mm.
[0032] The freeze-drying process of the breathable freeze-drying tube of this invention can be as follows:
[0033] Step 1: Sterilize the lyophilized tubes with the new type of cap, dispense the sample into the lyophilized tubes, and tighten the caps;
[0034] Step 2: Freeze the sample freeze-dried tubes at -80℃ for at least 2 hours;
[0035] Step 3: Vacuum freeze drying;
[0036] Step 4: After the lyophilized sample tubes are disinfected by alcohol spray, the perforated caps for lyophilization are removed in the laminar flow hood and replaced with sterile caps without perforations.
[0037] The usage process and effects of this novel air-permeable freeze-drying tube are as follows:
[0038] Aseptic testing of frozen stem cell factor samples
[0039] Step 1: Add 1 ml of sample to 100 sterile, breathable lyophilized tubes with new caps, and lyophilize the 100 samples according to the steps above.
[0040] Step 2: Add 100 μl of sample to 100 sterile, breathable lyophilized tubes with new caps, and lyophilize the 100 samples according to the steps above.
[0041] Step 2: Add 1 ml of diluent to the lyophilized tube to reconstitute it.
[0042] Step 3: Take a T25 culture flask and add 16 ml of thioglycolate fluid medium and tryptic soy liquid medium, respectively. Inoculate 0.33 ml of the test sample into two T25 culture flasks containing thioglycolate fluid medium and one T25 culture flask containing tryptic soy liquid medium, and mix the liquids thoroughly. Perform the same inoculation procedure using PBS buffer as a negative control.
[0043] Step 4: Divide the thioglycolate fluid medium flask containing the inoculated samples into two equal parts. Incubate one part at 30–35°C and the other part at 20–25°C. Incubate the tryptic soy peptone liquid medium at 20–25°C.
[0044] Incubation. Incubate for no less than 14 days; after incubation, observe whether the culture medium is turbid. If the culture medium is turbid, it is impossible to judge whether there is microbial growth from the appearance. Observe whether there are bacteria under a microscope and take pictures for preservation. Spread the culture medium on tryptone soy agar (TSA) and Sabouraud dextrose agar (SDA) plates.
[0045] After 5 days of incubation, observe for bacterial colony growth. The lyophilized samples from this lyophilized tube showed a negative sterility test result, indicating a 100% sterility rate.
[0046] Test results
[0047] sample result 100 samples All negative negative control Negative Positive control Positive
[0048] Conclusion: All samples in the 100 lyophilized tubes were sterile. The novel cap-type sterile and breathable lyophilized tubes can effectively maintain the sterility of samples throughout the entire process of dispensing, pre-freezing at -80℃, and vacuum lyophilization.
[0049] Cell culture validation was performed using the above-mentioned lyophilized hydrogel sample. This hydrogel material serves as a support framework for 3D cell culture. The experimental validation steps are as follows:
[0050] (1) Prepare the necessary and corresponding culture media for cell culture;
[0051] (2) The gel material reagents freeze-dried in the sterile freeze-drying tubes are reconstituted and prepared into a solution of a certain concentration according to the instructions for use;
[0052] (3) Prepare the hydrogel-cell suspension according to the reagent addition order indicated in the instructions; and add the sample to a 24-well plate;
[0053] (4) UV curing;
[0054] (5) Add culture medium and incubate in a cell culture incubator;
[0055] (6) Replace the culture medium after 1 hour and put it back into the incubator;
[0056] (7) Change the culture medium regularly according to the cell culture conditions.
[0057] like Figure 6-7 As shown, the material freeze-dried using the breathable freeze-drying tube of this invention can be used for 3D cell culture to ensure a sterile environment for the cells.
[0058] It will be apparent to those skilled in the art that this invention is not limited to the details of the exemplary embodiments described above, and that it can be implemented in other specific forms without departing from the spirit or essential characteristics of this invention. Therefore, the embodiments should be considered illustrative and non-limiting in all respects, and the scope of this invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within this invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
[0059] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A breathable freeze-drying tube for sterile freeze-drying, comprising a tube cap, a tube body with an opening, and a waterproof and breathable component, characterized in that, The cap has a vent hole, and the waterproof and ventilated component is fitted to the inside of the cap to isolate the opening of the pipe body from the vent hole. The waterproof and ventilated component allows water to pass through the opening to the vent hole. The cap is fitted with a support structure that restricts the waterproof and ventilated component. The support structure includes at least a hollow annular body circumferentially disposed on the inner wall of the cap. The annular body includes at least a first platform for engaging the waterproof and ventilated component. The vent hole is defined by a first edge at the top of the cap. The first edge defines a first hollow portion that extends through the top of the cap. The first hollow portion also defines a plurality of ribs. At least a portion of the ends of the ribs are connected to the first edge. When the ribs include structures in multiple different directions, some of the ribs are intersecting.
2. The breathable freeze-drying tube for aseptic lyophilization according to claim 1, characterized in that, The waterproof and breathable component also has a first bend outside the inner circumference of the first platform, and the first bend extends from the annular body toward the tube body along the inner wall of the tube cap.
3. The breathable freeze-drying tube for aseptic lyophilization according to claim 2, characterized in that, The waterproof and breathable component also has a first bend near the outermost periphery of the first countertop.
4. The breathable freeze-drying tube for aseptic lyophilization according to claim 3, characterized in that, The outermost periphery of the first bend is non-circular.
5. The breathable freeze-drying tube for aseptic lyophilization according to claim 1, characterized in that, The fit between the annular body and the waterproof and breathable component is a suspended fit: the inner diameter of the tube cap within the surface of the first platform is R1, and the outer periphery of the first platform restricts the minimum first outer diameter R2, where R2≤R1.
6. The breathable freeze-drying tube for aseptic lyophilization according to claim 1, characterized in that, The waterproof and breathable component is a semi-permeable membrane.
7. The breathable freeze-draw tube for aseptic lyophilization of claim 1, wherein, The cap and the body of the pipe are connected by threads.
8. The breathable freeze-draw tube for aseptic lyophilization of claim 1, wherein, At least a portion of the outer sidewall of the tube cap and / or tube body has an uneven functional portion.