CN115824616A - On-line integrity test method for filter element of fine filter - Google Patents
On-line integrity test method for filter element of fine filter Download PDFInfo
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- CN115824616A CN115824616A CN202310102440.7A CN202310102440A CN115824616A CN 115824616 A CN115824616 A CN 115824616A CN 202310102440 A CN202310102440 A CN 202310102440A CN 115824616 A CN115824616 A CN 115824616A
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Abstract
The invention belongs to the technical field of filter element detection, and relates to a method for testing the online integrity of a filter element of a fine filter, which comprises the following steps: the method comprises the following steps of (1) sterilizing a testing device, (2) sterilizing a filter element, (3) testing a blank control group, (4) coating a plate on the blank control group, (5) and analyzing results of the plate coating detection (6). According to the test method provided by the invention, the simple test device is matched with bacterial colony detection, the on-line integrity test of the filter element of the fine filter can be realized without taking down the filter element, the sterile environment of the filter element cannot be damaged in the test process, the device and material cost used in the whole test process is lower, the test result is more visual, the integrity of the filter element is judged by checking whether the detection flat plate has bacteria, if the detection flat plate has bacteria, the filter element is complete, and if the detection flat plate has bacteria, the filter element is damaged.
Description
Technical Field
The invention belongs to the technical field of filter element detection, and particularly relates to a method for testing the on-line integrity of a filter element of a fine filter.
Background
Sterile air and nitrogen are necessary sterile gases in the fermentation industry, the preparation of the sterile gases is benefited by a filter, and a fine filter is the last guarantee for preparing the sterile gases. The shell of the cylinder body is generally made of stainless steel, and the interior of the cylinder body adopts PP melt-blown filter element, wire-wound filter element, folding filter element, titanium filter element, active carbon filter element and the like as filter elements. The core component of the fine filter is a filter element, and the integrity of the filter element is the fundamental guarantee of sterile gas.
In the process of analyzing the possibility of the contamination of the fermentation product, the contamination caused by gas causes occupies the first place, so that the integrity of the filter element is the important factor for ensuring the normal fermentation of the product. In the existing filter element integrity test method, the sterile environment of the filter element is mostly needed to be destroyed, namely, the filter element is taken down to be detected by an integrity detector, and online detection cannot be carried out, so that the detection cost is high.
CN201110350245.3 discloses a filter online integrity test method, which is used for integrity test of a filter element through a conventional bubble point test, a diffusion flow test or a pressure maintenance test, wherein the three test methods all need to wet the filter element with liquid for detection, and are more suitable for testing the liquid filter element; although the diffusion flow test is suitable for the integrity test of a filter element with a larger membrane area, the diffusion is in direct proportion to the membrane area and is irrelevant to the membrane aperture, and the increase of the accumulation of the diffusion flow can reduce the actual effectiveness of the integrity test, so that the test result is inaccurate; the pressure holding test measures the pressure decay at each increment by providing the upstream pressure and increasing it by a predetermined pressure increment, and this test method is only suitable for some rough tests and has a low accuracy.
Disclosure of Invention
The invention aims to provide an online integrity testing method for a filter element of a fine filter, which has the advantages of low cost, high detection sensitivity, no need of disassembling the filter element and simple and convenient operation, and aims to solve the problems in the background technology.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
an online integrity test method for a fine filter element comprises the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle and a bottle cap in threaded connection with the testing bottle, a liquid culture medium is arranged in the testing bottle, an air inlet pipe and an air outlet pipe are arranged on the bottle cap, one end of the air inlet pipe extends into the liquid culture medium, a first sealing film is arranged at the other end of the air inlet pipe, one end of the air outlet pipe is located above the liquid culture medium, an air filter is arranged at the other end of the air outlet pipe, a second sealing film is coated outside the air filter, the bottle cap is unscrewed for a half circle, the testing device is sterilized for 20min at the temperature of 121 ℃ and under the pressure of 0.1MPa, and the bottle cap is screwed for standby after sterilization is completed;
(2) And (3) sterilizing the filter element: sterilizing a filter element in a fine filter for 20min at the temperature of 123 ℃ under 0.12MPa, introducing air into the fine filter after the sterilization is finished and before the pressure in the fine filter is reduced to 0MPa, drying the filter element, and waiting for testing;
(3) Test group: opening a first sealing film, communicating an air inlet pipe of the testing device with the fine filter, opening a second sealing film, introducing air into the fine filter for 1h, introducing the air into the testing bottle, sealing the first sealing film and the second sealing film after the air introduction is finished, and waiting for flat plate coating detection;
(4) Blank control group: taking a blank testing device, wherein the blank testing device has the same structure as the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening a first sealing film of the blank testing device, communicating an air inlet pipe of the blank testing device with the fine filter, opening a second sealing film of the blank testing device, sealing the first sealing film and the second sealing film of the blank testing device after the blank testing device is placed for 1h, and waiting for flat coating detection;
(5) Plate coating detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 mu l of liquid culture medium from the testing device in the step (3) and the blank testing device in the step (4), coating the liquid culture medium on a detection flat plate, putting the detection flat plate in an incubator at 37 ℃ for culturing for 24h, and observing whether sterile colonies exist;
(6) And (4) analyzing results: and comparing the detection result of the test group with the detection result of the blank control group, and judging whether the filter element is complete.
As an improvement, in the step (1), the first sealing film and the second sealing film are kraft paper, plastic film or tin foil paper.
As an improvement, in the step (1), the air filter is a 0.22 mu m air filter membrane or absorbent cotton coated with double layers of gauze.
As an improvement, in step (2), the bottom of smart filter is equipped with first needle valve, the lower part of smart filter is equipped with the second needle valve, first needle valve is connected with first silicone tube, the second needle valve is connected with the second silicone tube, in first silicone tube and the second silicone tube all stretched into the cask, fill cooling water in the cask, right when filter core among the smart filter carries out the sterilization, open first needle valve and second needle valve, to let in steam among the smart filter, after the sterilization, close first needle valve and second needle valve, will first silicone tube and second silicone tube press from both sides tightly with the stagnant water respectively.
As a further improvement, the joint of the first needle valve and the first silicone tube and the joint of the second needle valve and the second silicone tube are fixed by a binding tape.
As a modification, in step (5), the liquid culture medium left in the test device and the blank test device is continuously cultured in an incubator at 37 ℃ overnight, and then the detection plate is coated again to observe whether the colony exists or not.
As a further improvement, in the step (5), the detection plate is an LB agar plate or a PDA agar plate.
As a modification, in the step (1), the liquid medium is added in an amount of 1/3 of the volume of the test bottle.
As a modification, in the step (1), the liquid medium is LB liquid medium or PDA liquid medium.
Due to the adoption of the technical scheme, the invention has the beneficial effects that:
according to the test method provided by the invention, the simple test device is matched with bacterial colony detection, the on-line integrity test of the filter element in the fine filter can be realized without taking down the filter element, the sterile environment of the filter element in the fine filter cannot be damaged in the test process, the cost of the test device and materials used in the whole test process is low, the test result is relatively intuitive, the integrity of the filter element can be judged by checking whether the bacteria exist on the detection flat plate, if the bacteria exist on the detection flat plate, the integrity of the filter element is shown, and if the bacteria exist on the detection flat plate, the damage of the filter element is shown. The first sealing film and the second sealing film in the testing device can prevent external air from entering the testing device, and the air filter at the tail end of the exhaust pipe can prevent the external air from entering the testing device when the second sealing film is opened so as to interfere with a testing result.
Drawings
FIG. 1 is a schematic diagram of a fine filter and a testing device according to the present invention;
FIG. 2 is a schematic diagram of a fine filter sterilization process according to the present invention;
FIG. 3 is a schematic structural diagram of a testing apparatus provided in the present invention;
wherein: 1-test bottle, 2-bottle cap, 3-air inlet pipe, 4-exhaust pipe, 5-first sealing film, 6-third silicone tube, 7-second sealing film, 8-fourth silicone tube, 9-air filter, 10-fine filter, 11-first needle valve, 12-second needle valve, 13-first silicone tube, 14-second silicone tube, 15-steam valve, 16-filter element, 17-pressure gauge, 18-air valve, 19-water bucket, 91-absorbent cotton, and 92-double-layer gauze.
Detailed Description
The present invention will be further described with reference to the following detailed description and accompanying drawings. Wherein the showings are for the purpose of illustration only and are shown by way of illustration only and not in actual form, and are not to be construed as limiting the present patent; to better illustrate the embodiments of the present invention, some parts of the drawings may be omitted, enlarged or reduced, and do not represent the size of an actual product; it will be understood by those skilled in the art that certain well-known structures in the drawings and descriptions thereof may be omitted.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", etc. based on the orientation or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not intended to indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present patent, and the specific meaning of the terms may be understood by those skilled in the art according to specific circumstances.
The test apparatus and the blank test apparatus used in this example are structured as shown in fig. 1 to 3. Example 1
An online integrity test method for a fine filter element comprises the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle 1, wherein a 1/3 volume LB liquid culture medium is arranged in the testing bottle 1, the top end of the testing bottle 1 is in threaded connection with a bottle cap 2, an air inlet pipe 3 and an exhaust pipe 4 are arranged on the bottle cap 2, one end of the air inlet pipe 3 extends into the LB liquid culture medium, the other end of the air inlet pipe 3 is connected with a third silicone tube 6, the tail end of the third silicone tube 6 is coated with a first sealing film 5, the first sealing film 5 is kraft paper, one end of the exhaust pipe 4 is positioned above the LB liquid culture medium, the other end of the exhaust pipe 4 is connected with a fourth silicone tube 8, the tail end of the fourth silicone tube 8 is provided with an air filter 9, the air filter 9 is absorbent cotton 91 coated with double-layer gauze 92, the air filter 9 is coated with a second sealing film 7, the second sealing film 7 is kraft paper, water stopping clamps are arranged on the third silicone tube 6 and the fourth silicone tube 8, the bottle cap 2 is unscrewed by a half circle, the testing device is sterilized at 0.1MPa and 121 ℃, and the bottle cap 2 is screwed tightly for standby;
(2) And (3) sterilizing the filter element: introducing steam into the fine filter 10, opening a first needle valve 11 at the bottom of the fine filter 10 and a second needle valve 12 at the lower part of the fine filter 10, connecting the first needle valve 11 with a first silicone tube 13, connecting the second needle valve 12 with a second silicone tube 14, wherein the first silicone tube 13 and the second silicone tube 14 are only required to be subjected to steam emission, extending the first silicone tube 13 and the second silicone tube 14 into a water barrel 19 for steam condensation, adjusting a steam valve 15, sterilizing a filter element 16 in the fine filter 10 at 0.12MPa and 123 ℃ for 20min, closing the steam valve 15 after the sterilization is finished, arranging a pressure gauge 17 on the fine filter 10, opening the air valve 18 before the pointer of the pressure gauge 17 is reduced to 0MPa, introducing air into the fine filter 10, drying the filter element 16, closing the first needle valve 11 and the second needle valve 12, clamping the first silicone tube 13 and the second silicone tube 14 with water stop clamps respectively, and waiting for testing;
(3) Test group: opening the first sealing film 5 at the tail end of the third silicone tube 6, quickly removing the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 with the second needle valve 12, fixing by using a binding belt, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize by using 75% alcohol, remove the second sealing film 7 at the tail end of the fourth silicone tube 8, remove the water stop clamps on the third silicone tube 6 and the fourth silicone tube 8, open the second needle valve 12, introduce air into the test bottle 1 for 1h, close the second needle valve 12, clamp the third silicone tube 6 and the fourth silicone tube 8 by using the water stop clamps, seal the first sealing film 5 and the second sealing film 7, and wait for flat plate detection;
(4) Blank control group: taking a blank testing device, wherein the structure of the blank testing device is the same as that of the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening the first sealing film 5 of the blank testing device, quickly taking off the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 of the blank testing device with the second needle valve 12, fixing the blank testing device by using a binding tape, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize the mask by using 75% alcohol, take off the second sealing film 7 of the blank testing device, take off the third silicone tube 6 of the blank testing device and a water stop clamp on the fourth silicone tube 8, after placing for 1h, tightly clamping the third silicone tube 6 and the fourth silicone tube 8 of the blank testing device by using the water stop clamp, sealing the first sealing film 5 and the second sealing film 7 of the blank testing device, and waiting for flat plate coating detection;
(5) Coating a flat plate for detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 mul of LB liquid culture medium from the test device in the step (3) and the blank test device in the step (4), coating the LB liquid culture medium on an LB detection flat plate, putting the LB detection flat plate in an incubator at 37 ℃ for culturing for 24h, and observing whether sterile colonies exist;
(6) And (4) analyzing results: comparing the detection result of the test group with the detection result of the blank control group to judge whether the filter element is complete; if the control group and the test group are free from contamination, the operation is reliable and the filter element is complete; if the control group has bacteria, the test group is sterile, which indicates that the operation is not reliable and needs to be redone; if the control group is sterile, the test group is sterile, which indicates that the operation is reliable, the filter element is incomplete and needs to be replaced; if the control group and the test group have bacteria, the operation is not reliable and needs to be redone. Example 2
An online integrity test method for a fine filter element comprises the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle 1, a 1/3 volume of PDA liquid culture medium is arranged in the testing bottle 1, the top end of the testing bottle 1 is in threaded connection with a bottle cap 2, an air inlet pipe 3 and an exhaust pipe 4 are arranged on the bottle cap 2, one end of the air inlet pipe 3 extends into the PDA liquid culture medium, the other end of the air inlet pipe 3 is connected with a third silicone tube 6, the tail end of the third silicone tube 6 is coated with a first sealing film 5, the first sealing film 5 is a plastic film, one end of the exhaust pipe 4 is located above the PDA liquid culture medium, the other end of the exhaust pipe 4 is connected with a fourth silicone tube 8, the tail end of the fourth silicone tube 8 is provided with an air filter 9, the air filter 9 is absorbent cotton 91 coated with double-layer gauze 92, the air filter 9 is coated with a second sealing film 7, the second sealing film 7 is a plastic film, water stopping clamps are arranged on the third silicone tube 6 and the fourth silicone tube 8, the bottle cap 2 is unscrewed by a half-turn, the testing device is sterilized at 0.1MPa and 121 ℃, and the bottle cap 2 is screwed tightly for standby after the testing device is sterilized;
(2) And (3) sterilizing the filter element: introducing steam into the fine filter 10, opening a first needle valve 11 at the bottom of the fine filter 10 and a second needle valve 12 at the lower part of the fine filter 10, wherein the first needle valve 11 is connected with a first silicone tube 13, the second needle valve 12 is connected with a second silicone tube 14, the first silicone tube 13 and the second silicone tube 14 are only required to be properly provided with steam, extending the first silicone tube 13 and the second silicone tube 14 into a water barrel 19 for steam condensation, adjusting a steam valve 15, sterilizing a filter element 16 in the fine filter 10 at 0.12MPa and 123 ℃ for 20min, closing the steam valve 15 after the sterilization is finished, arranging a pressure gauge 17 on the fine filter 10, opening an air valve 18 before the pointer of the pressure gauge 17 is reduced to 0MPa, introducing air into the fine filter 10, drying the filter element 16, closing the first needle valve 11 and the second needle valve 12, respectively clamping the first silicone tube 13 and the second silicone tube 14 by water stop clamps, and waiting for testing;
(3) Test group: opening the first sealing film 5 at the tail end of the third silicone tube 6, quickly removing the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 with the second needle valve 12, fixing the third silicone tube 6 by using a binding belt, quickly operating the step, keeping the environment as static as possible, wearing a mask, wearing gloves, sterilizing the mask by using 75% alcohol, removing the second sealing film 7 at the tail end of the fourth silicone tube 8, removing the water-stop clamps on the third silicone tube 6 and the fourth silicone tube 8, opening the second needle valve 12, introducing air into the test bottle 1 for 1h, closing the second needle valve 12, clamping the third silicone tube 6 and the fourth silicone tube 8 by using the water-stop clamps, sealing the first sealing film 5 and the second sealing film 7, and waiting for flat plate detection;
(4) Blank control group: taking a blank testing device, wherein the structure of the blank testing device is the same as that of the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening the first sealing film 5 of the blank testing device, quickly taking off the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 of the blank testing device with the second needle valve 12, fixing the blank testing device by using a binding tape, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize the mask by using 75% alcohol, take off the second sealing film 7 of the blank testing device, take off the third silicone tube 6 of the blank testing device and a water stop clamp on the fourth silicone tube 8, after placing for 1h, tightly clamping the third silicone tube 6 and the fourth silicone tube 8 of the blank testing device by using the water stop clamp, sealing the first sealing film 5 and the second sealing film 7 of the blank testing device, and waiting for flat plate coating detection;
(5) Coating a flat plate for detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 mu l of PDA liquid culture medium from the test device in the step (3) and the blank test device in the step (4), coating the PDA liquid culture medium on an LB agar plate, putting the LB agar plate in an incubator at 37 ℃ for culturing for 24h, and observing the sterile colony; continuously placing the remaining PDA liquid culture medium in the test device and the blank test device in an incubator at 37 ℃ for overnight culture, coating an LB agar plate again, and observing whether the bacterial colony exists;
(6) And (4) analyzing results: comparing the detection result of the test group with the detection result of the blank control group to judge whether the filter element is complete; if the control group and the test group are free from contamination, the operation is reliable and the filter element is complete; if the control group has bacteria, the test group is sterile, which indicates that the operation is not reliable and needs to be redone; if the control group is sterile, the test group is sterile, which indicates that the operation is reliable, the filter element is incomplete and needs to be replaced; if the control group and the test group have bacteria, the operation is not reliable and needs to be redone. Example 3
An online integrity test method for a fine filter element comprises the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle 1, a LB liquid culture medium with the volume of 1/3 is arranged in the testing bottle 1, the top end of the testing bottle 1 is in threaded connection with a bottle cap 2, an air inlet pipe 3 and an air outlet pipe 4 are arranged on the bottle cap 2, one end of the air inlet pipe 3 extends into the LB liquid culture medium, the other end of the air inlet pipe 3 is connected with a third silicone tube 6, the tail end of the third silicone tube 6 is coated with a first sealing film 5, the first sealing film 5 is tin foil paper, one end of the air outlet pipe 4 is located above the LB liquid culture medium, the other end of the air outlet pipe 4 is connected with a fourth silicone tube 8, the tail end of the fourth silicone tube 8 is provided with an air filter 9, the air filter 9 is an air filter membrane with the size of 0.22 mu m, the air filter 9 is coated with a second sealing film 7, the second sealing film 7 is tin foil paper, water stop clamps are arranged on the third silicone tube 6 and the fourth silicone tube 8, the bottle cap 2 is unscrewed by a half-turn, the testing device is sterilized at the temperature of 0.1 and 121 ℃, the testing device is screwed down for 20min after sterilization, the bottle cap 2 is screwed for standby;
(2) And (3) sterilizing the filter element: introducing steam into the fine filter 10, opening a first needle valve 11 at the bottom of the fine filter 10 and a second needle valve 12 at the lower part of the fine filter 10, wherein the first needle valve 11 is communicated with a first silicone tube 13, the second needle valve 12 is connected with a second silicone tube 14, the first silicone tube 13 and the second silicone tube 14 are only required to be properly sprayed with the steam, extending the first silicone tube 13 and the second silicone tube 14 into a water barrel 19 for steam condensation, adjusting a steam valve 15, sterilizing a filter element 16 in the fine filter 10 at 0.12MPa and 123 ℃ for 20min, closing the steam valve 15 after the sterilization is finished, arranging a pressure gauge 17 on the fine filter 10, opening an air valve 18 before the pointer of the pressure gauge 17 is reduced to 0MPa, introducing air into the fine filter 10, drying the filter element 16, closing the first needle valve 11 and the second needle valve 12, clamping the first silicone tube 13 and the second silicone tube 14 with water stop clamps respectively, and waiting for testing;
(3) Test group: opening the first sealing film 5 at the tail end of the third silicone tube 6, quickly removing the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 with the second needle valve 12, fixing by using a binding belt, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize by using 75% alcohol, remove the second sealing film 7 at the tail end of the fourth silicone tube 8, remove the water stop clamps on the third silicone tube 6 and the fourth silicone tube 8, open the second needle valve 12, introduce air into the test bottle 1 for 1h, close the second needle valve 12, clamp the third silicone tube 6 and the fourth silicone tube 8 by using the water stop clamps, seal the first sealing film 5 and the second sealing film 7, and wait for flat plate detection;
(4) Blank control group: taking a blank testing device, wherein the structure of the blank testing device is the same as that of the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening the first sealing film 5 of the blank testing device, quickly taking off the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 of the blank testing device with the second needle valve 12, fixing the blank testing device by using a binding tape, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize the mask by using 75% alcohol, take off the second sealing film 7 of the blank testing device, take off the third silicone tube 6 of the blank testing device and a water stop clamp on the fourth silicone tube 8, after placing for 1h, tightly clamping the third silicone tube 6 and the fourth silicone tube 8 of the blank testing device by using the water stop clamp, sealing the first sealing film 5 and the second sealing film 7 of the blank testing device, and waiting for flat plate coating detection;
(5) Coating a flat plate for detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 mul of LB liquid culture medium from the test device in the step (3) and the blank test device in the step (4), coating the LB liquid culture medium on a PDA agar plate, putting the PDA agar plate in an incubator at 37 ℃ for culturing for 24h, and observing whether sterile colonies exist; continuously placing the residual LB liquid culture medium in the test device and the blank test device in an incubator at 37 ℃ for overnight culture, then coating a PDA agar plate once, and observing whether the bacterial colony exists;
(6) And (4) analyzing results: comparing the detection result of the test group with the detection result of the blank control group to judge whether the filter element is complete; if the control group and the test group are free from contamination, the operation is reliable and the filter element is complete; if the control group has bacteria, the test group is sterile, which indicates that the operation is not reliable and needs to be redone; if the control group is sterile, the test group is sterile, which indicates that the operation is reliable, the filter element is incomplete and needs to be replaced; if the control group and the test group have bacteria, the operation is not reliable and needs to be redone. Example 4
An online integrity test method for a fine filter element comprises the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle 1, a 1/3 volume of PDA liquid culture medium is arranged in the testing bottle 1, the top end of the testing bottle 1 is in threaded connection with a bottle cap 2, an air inlet pipe 3 and an exhaust pipe 4 are arranged on the bottle cap 2, one end of the air inlet pipe 3 extends into the PDA liquid culture medium, the other end of the air inlet pipe 3 is connected with a third silicone tube 6, the tail end of the third silicone tube 6 is coated with a first sealing film 5, the first sealing film 5 is kraft paper, one end of the exhaust pipe 4 is located above the PDA liquid culture medium, the other end of the exhaust pipe 4 is connected with a fourth silicone tube 8, the tail end of the fourth silicone tube 8 is provided with an air filter 9, the air filter 9 is an air filter membrane of 0.22 mu m, the air filter 9 is coated with a second sealing film 7, the second sealing film 7 is kraft paper, water stopping clamps are arranged on the third silicone tube 6 and the fourth silicone tube 8, the bottle cap 2 is unscrewed by a half-turn, the testing device is sterilized at 0.1MPa and 121 ℃, the bottle cap 2 is screwed tightly for standby after sterilization;
(2) And (3) sterilizing the filter element: introducing steam into the fine filter 10, opening a first needle valve 11 at the bottom of the fine filter 10 and a second needle valve 12 at the lower part of the fine filter 10, wherein the first needle valve 11 is communicated with a first silicone tube 13, the second needle valve 12 is connected with a second silicone tube 14, the first silicone tube 13 and the second silicone tube 14 are only required to be properly sprayed with the steam, extending the first silicone tube 13 and the second silicone tube 14 into a water barrel 19 for steam condensation, adjusting a steam valve 15, sterilizing a filter element 16 in the fine filter 10 at 0.12MPa and 123 ℃ for 20min, closing the steam valve 15 after the sterilization is finished, arranging a pressure gauge 17 on the fine filter 10, opening an air valve 18 before the pointer of the pressure gauge 17 is reduced to 0MPa, introducing air into the fine filter 10, drying the filter element 16, closing the first needle valve 11 and the second needle valve 12, clamping the first silicone tube 13 and the second silicone tube 14 with water stop clamps respectively, and waiting for testing;
(3) Test group: opening the first sealing film 5 at the tail end of the third silicone tube 6, quickly removing the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 with the second needle valve 12, fixing by using a binding belt, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize by using 75% alcohol, remove the second sealing film 7 at the tail end of the fourth silicone tube 8, remove the water stop clamps on the third silicone tube 6 and the fourth silicone tube 8, open the second needle valve 12, introduce air into the test bottle 1 for 1h, close the second needle valve 12, clamp the third silicone tube 6 and the fourth silicone tube 8 by using the water stop clamps, seal the first sealing film 5 and the second sealing film 7, and wait for flat plate detection;
(4) Blank control group: taking a blank testing device, wherein the structure of the blank testing device is the same as that of the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening the first sealing film 5 of the blank testing device, quickly taking off the second silicone tube 14 on the second needle valve 12, connecting the third silicone tube 6 of the blank testing device with the second needle valve 12, fixing the blank testing device by using a binding tape, wherein the operation of the step is quick, the environment is kept static as much as possible, an operator needs to wear a mask, wear gloves and sterilize the mask by using 75% alcohol, take off the second sealing film 7 of the blank testing device, take off the third silicone tube 6 of the blank testing device and a water stop clamp on the fourth silicone tube 8, after placing for 1h, tightly clamping the third silicone tube 6 and the fourth silicone tube 8 of the blank testing device by using the water stop clamp, sealing the first sealing film 5 and the second sealing film 7 of the blank testing device, and waiting for flat plate coating detection;
(5) Plate coating detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 microliter of PDA liquid culture medium from the test device in the step (3) and the blank test device in the step (4), coating the PDA liquid culture medium on a PDA agar plate, putting the PDA agar plate in an incubator at 37 ℃ for culturing for 24 hours, and observing the existence of sterile colonies; continuously placing the remaining PDA liquid culture medium in the test device and the blank test device in an incubator at 37 ℃ for overnight culture, then coating a PDA agar plate once, and observing whether the bacterial colony exists;
(6) And (4) analyzing results: the detection result of the test group is compared with the detection result of the blank control group, so that whether the filter element is complete or not can be judged; if the control group and the test group are free from contamination, the operation is reliable and the filter element is complete; if the control group has bacteria, the test group is sterile, which indicates that the operation is not reliable and needs to be redone; if the control group is sterile, the test group is sterile, which indicates that the operation is reliable, the filter element is incomplete and needs to be replaced; if the control group and the test group have bacteria, the operation is not reliable and needs to be redone.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. An online integrity test method for a filter element of a fine filter is characterized by comprising the following steps:
(1) Sterilizing a testing device: the testing device comprises a testing bottle and a bottle cap in threaded connection with the testing bottle, a liquid culture medium is arranged in the testing bottle, an air inlet pipe and an air outlet pipe are arranged on the bottle cap, one end of the air inlet pipe extends into the liquid culture medium, a first sealing film is arranged at the other end of the air inlet pipe, one end of the air outlet pipe is located above the liquid culture medium, an air filter is arranged at the other end of the air outlet pipe, a second sealing film is coated outside the air filter, the bottle cap is unscrewed for a half circle, the testing device is sterilized for 20min at 121 ℃ and 0.1MPa, and the bottle cap is screwed for standby after sterilization is completed;
(2) And (3) sterilizing the filter element: sterilizing a filter element in a fine filter for 20min at the temperature of 123 ℃ under 0.12MPa, introducing air into the fine filter after the sterilization is finished and before the pressure in the fine filter is reduced to 0MPa, drying the filter element, and waiting for testing;
(3) Test group: opening a first sealing film, communicating an air inlet pipe of the testing device with the fine filter, opening a second sealing film, introducing air into the fine filter for 1h, introducing the air into the testing bottle, sealing the first sealing film and the second sealing film after the air introduction is finished, and waiting for flat plate coating detection;
(4) Blank control group: taking a blank testing device, wherein the blank testing device has the same structure as the testing device in the step (1), and sterilizing the blank testing device for later use according to the operation in the step (1); opening a first sealing film of the blank testing device, communicating an air inlet pipe of the blank testing device with the fine filter, opening a second sealing film of the blank testing device, sealing the first sealing film and the second sealing film of the blank testing device after the blank testing device is placed for 1h, and waiting for flat coating detection;
(5) Coating a flat plate for detection: in the environment of a biological safety cabinet or an ultra-clean workbench, respectively taking 500 mu l of liquid culture medium from the testing device in the step (3) and the blank testing device in the step (4), coating the liquid culture medium on a detection flat plate, putting the detection flat plate in an incubator at 37 ℃ for culturing for 24h, and observing whether sterile colonies exist;
(6) And (4) analyzing results: and comparing the detection result of the test group with the detection result of the blank control group, and judging whether the filter element is complete.
2. The fine filter cartridge on-line integrity test method as recited in claim 1, wherein in step (1), the first and second sealing films are kraft paper, plastic film, or tinfoil paper.
3. The online integrity test method for the filter element of the fine filter according to claim 1, wherein in the step (1), the air filter is a 0.22 μm air filter membrane or absorbent cotton coated with double-layer gauze.
4. The online integrity testing method for the filter element of the fine filter according to claim 1, wherein in step (2), the bottom of the fine filter is provided with a first needle valve, the lower part of the fine filter is provided with a second needle valve, the first needle valve is connected with a first silicone tube, the second needle valve is connected with a second silicone tube, the first silicone tube and the second silicone tube both extend into a bucket, the bucket is filled with cooling water, and when the filter element in the fine filter is sterilized, the first needle valve and the second needle valve are opened, steam is introduced into the fine filter, and after the sterilization is finished, the first needle valve and the second needle valve are closed, and the first silicone tube and the second silicone tube are respectively clamped by a water stop clamp.
5. The method for testing the online integrity of a fine filter cartridge according to claim 4, wherein the joint of the first needle valve and the first silicone tube and the joint of the second needle valve and the second silicone tube are both fixed by ties.
6. The fine filter cartridge on-line integrity test method as recited in claim 1, wherein in step (5), the remaining liquid culture medium in both the test unit and the blank test unit is further incubated in an incubator at 37 ℃ overnight, and the test plate is coated again to observe the presence or absence of colonies.
7. The fine filter cartridge in-line integrity test method as claimed in claim 6, wherein in step (5), the test plate is LB agar plate or PDA agar plate.
8. The fine filter cartridge in-line integrity test method of claim 1, wherein in step (1), the liquid culture medium is added in an amount of 1/3 of the volume of the test bottle.
9. The fine filter cartridge online integrity test method of claim 1, wherein in step (1), the liquid medium is LB liquid medium or PDA liquid medium.
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| CN115824616B (en) | 2023-04-14 |
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