A device and method for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products.

Abstract

This invention relates to the field of medical device testing technology, and discloses a device and method for measuring the amount of debris falling off rubber stoppers used in the outer packaging of human medical infusion liquid products. A fixed cylinder is mounted on a base, with an outer insulating pad between the fixed cylinder and the base. A shielding shell surrounds the fixed cylinder, and a matching shielding cover is located on the top of the shielding shell. The shielding cover has an upward-protruding sample mounting port in the center. An inner insulating pad is located at the bottom of the fixed cylinder, and a metal guide block is located above the inner insulating pad. A friction cylinder is encircled above the metal guide block, and a retractable friction rod is located in the center of the friction cylinder above the metal guide block. The lower part of the metal guide block is connected to an electrometer and an oscilloscope. This invention is applicable to the measurement of debris volume that cannot be observed with normal human vision, providing a novel solution that can observe small-diameter debris that is unobservable by existing methods.

Description

Technical Field

[0001] This invention relates to the field of medical device testing technology, specifically to a device and method for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products. Background Technology

[0002] With the continuous development of medical technology, a plethora of liquid health products and pharmaceuticals for oral, injection, and infusion administration have emerged. Among these are products intended for direct intravenous injection or infusion, whose safety is of paramount concern due to their direct entry into the bloodstream and participation in blood circulation. These liquid products are all sterilely sealed in containers, some classified as medical devices and others as pharmaceutical packaging materials. In clinical use, syringes, infusion sets, or puncture devices are used to penetrate the container and extract the liquid medication. To facilitate extraction, liquid containers are typically designed... An opening made of rubber stopper facilitates puncture and extraction; however, the process of the puncture object (injection needle, puncture device) from contacting the rubber stopper to penetrating it generates puncture debris. This debris is a contaminant that becomes a solid in the liquid after entering the liquid drug, and its mixing with the drug composition may also affect the drug's composition. The harm to the human body is obvious, such as causing allergic reactions, pyrogenic reactions, phlebitis, pulmonary hypertension, granulomas, etc. Studies have shown that debris with a particle size ≤2.0μm dissolves directly in the drug solution, while those with a particle size >2.0μm are suspended in the drug solution, and only debris larger than 50μm can be observed under a microscope.

[0003] Existing puncture openings mostly use halogenated butyl rubber stoppers, which are widely used in pharmaceutical packaging materials due to their advantages of acid and alkali resistance, good airtightness, high cleanliness, and no reaction with drugs or other chemical reagents, exhibiting excellent chemical stability. However, puncture debris has become a major problem for pharmaceutical manufacturers. In recent years, Zhou Quan published "Analysis of Factors Affecting Rubber Puncture Debris" in the *Northwest Pharmaceutical Journal*, studying the standard causes of puncture debris and complaint handling methods; Xu Ya et al. published "Investigation and Analysis of Puncture Debris Situation of Pharmaceutical Butyl Rubber Stoppers" in *Straits Pharmaceutical Journal*, studying and comparing the puncture debris situation of different brands of products.

[0004] Currently, the 2020 edition of the Pharmacopoeia of the People's Republic of China, Volume IV, specifies three testing methods for Chinese medicine packaging materials, all of which involve visual observation or counting under a microscope. The existing standard YBB00332004-2015, "Determination of Peel Shedding Material from Rubber Stoppers for Injection," is almost identical to the pharmacopoeia. In actual testing, small-diameter peeling material is difficult to record by visual observation or counting under a microscope. The recorded quantity is greatly influenced by the observer, resulting in inaccurate values ​​and unclear or incomplete standards, especially in areas involving arbitration testing and microscopic material research, where there are no accurate reference standards. Summary of the Invention

[0005] This invention addresses the obvious harm to human health posed by puncture debris from rubber stoppers used in the outer packaging of liquid products for human medical infusion. Current testing standards rely on relatively crude methods such as visual inspection or microscopic examination, lacking more precise approaches. Furthermore, the amount of debris, which is not normally observable by human eyes, remains unmeasurable. This is particularly true in areas such as arbitration testing and microscopic material research, where more accurate measurement methods are lacking. The impact of puncture debris on the purity of the medication and its potential harm to the human body is also evident. Therefore, this invention provides a device and method for measuring puncture debris from rubber stoppers used in the outer packaging of liquid products for human medical infusion.

[0006] This invention is achieved using the following techniques:

[0007] This invention provides a device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion. A fixed cylinder is mounted on a base, with an outer insulating pad between the fixed cylinder and the base. A shielding shell surrounds the fixed cylinder, and a matching shielding cover is located on the top of the shielding shell. An upward-protruding sample mounting port is located in the center of the shielding cover. An inner insulating pad is located at the bottom of the fixed cylinder, and a metal guide block is located above the inner insulating pad. A friction cylinder is encircled above the metal guide block, and a retractable friction rod is located in the center of the friction cylinder above the metal guide block. The lower part of the metal guide block is connected to an electrometer and an oscilloscope.

[0008] In practice, this invention provides a device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products. The fixing cylinder is made of metal and is set on a base with an outer insulating pad between the fixing cylinder and the base. The fixing cylinder is covered by a shielding shell, and the top of the shielding shell is equipped with a matching shielding cover. Both the shielding shell and the shielding cover can shield external interference electric fields to avoid changes in the surrounding environment from interfering with the accuracy of the test. The shielding cover has an upward-protruding sample mounting port in the middle, which can stably mount the sample on the shielding cover and ensure that the sample being tested does not fall off during the puncture process.

[0009] An inner insulating pad is provided at the bottom of the fixed cylinder to prevent static charge from escaping through the inner sleeve. A metal conductor block is provided above the inner insulating pad, and a friction cylinder made of rubber is fitted around the upper part of the metal conductor block. A support ring is fixed to the lower inner wall of the fixed cylinder, located in the middle of the metal conductor block, with a gap between the support ring and the metal conductor block. The friction cylinder is placed on the support ring and is tightly installed inside the fixed cylinder to prevent movement during friction. A retractable friction rod is provided in the center of the friction cylinder above the metal conductor block. The friction rod includes a friction part and a handle part. The surface of the friction part is covered with fur. The handle part is connected to the friction part by a limiting ring protrusion. The limiting ring protrusion is made of insulating material. Made of insulating material, when the friction rod is pulled up and down, the friction between the friction rod and the friction cylinder generates charge and forms a potential difference. When the limiting ring of the friction rod abuts against the top of the friction cylinder, that is, when the friction rod is in the lower stroke, there is a gap between the free end of the friction part and the top surface of the metal conductor block. The lower part of the metal conductor block is connected to an electrometer and an oscilloscope. The electrometer is used to verify whether static charge is generated, and the oscilloscope is used to monitor the instantaneous amplitude peak during electrostatic discharge. Both the electrometer and the oscilloscope are connected to the metal conductor block through wires that pass through the lower part of the fixed cylinder and the shielding shell. Both the electrometer and the oscilloscope are grounded, that is, the electrometer and the oscilloscope are connected in parallel, with one end connected to the metal conductor block and the other end grounded.

[0010] In use, this invention provides a method for determining the puncture and shedding debris of rubber stoppers used in the outer packaging of human medical infusion liquid products, comprising the following steps:

[0011] a. Preparation of the sample to be tested

[0012] Take the sample to be tested and place it in 75% alcohol, shake it gently and soak for 5 minutes. Use clean metal tweezers to remove the sample and place it on a perforated wire mesh frame, ensuring that the sample is in contact with other objects. Use a constant temperature oven to air dry at 30℃ for 5 minutes for later use.

[0013] b. Preparation of measuring apparatus

[0014] Open the shielding cover and place it upside down on a clean workbench for later use. Take out the friction cylinder and wipe its surface with 75% alcohol until no lint falls off. Place the friction cylinder on a perforated wire mesh frame and air dry it in a constant temperature chamber at 30°C for 5 minutes. Install the air-dried friction cylinder into the fixed cylinder, placing it on the support ring. Ensure the lower part of the friction cylinder is interference-fitted with the metal guide block to prevent it from being pulled out of the fixed cylinder by the friction rod during friction. Fully insert the friction rod into the friction cylinder and use an antistatic fan to blow air onto the surfaces of all connecting parts of the device for 3 minutes. Then, zero the electrometer.

[0015] c. Rub and record the initial electrostatic value.

[0016] Hold the handle of the friction bar and pull it up and down in a vertical direction to make the friction bar rub against the friction cylinder. Remove the friction bar, cover it with the shielding cover, and record the value of the electrometer after it stabilizes.

[0017] d. Puncture test

[0018] Install the test sample prepared in step a into the sample mounting port, hold the puncture device and puncture the test sample once, record the waveform displayed on the oscilloscope for future reference; remove the punctured test sample, replace it with a new test sample, and similarly perform one puncture, record the waveform displayed on the oscilloscope for future reference.

[0019] e. Calculation and Judgment

[0020] Retrieve the waveform record from the oscilloscope during the puncture and observe the number of peaks that appear on the oscilloscope. The number of waveforms that appear during the puncture is the number of falling debris particles. If the number of waveforms that appear during the puncture exceeds the maximum allowable number of particles per sample specified in the standard, it does not meet the requirements; otherwise, it meets the requirements.

[0021] This invention also provides a device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion. A fixed cylinder is mounted on a base, with an outer insulating pad between the fixed cylinder and the base. The fixed cylinder is covered by a shielding shell, and a matching shielding cover is provided on the top of the shielding shell. The shielding cover has an upwardly protruding sample mounting port in the middle. An inner insulating pad is provided at the bottom of the fixed cylinder, and a friction cylinder is provided above the inner insulating pad. A photosensitive film is provided at intervals in the center of the friction cylinder, and the photosensitive film is placed vertically on the inner insulating pad. The friction cylinder is equipped with a retractable friction rod inside it.

[0022] In practice, this invention provides a device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products. The fixing cylinder is made of metal and is set on a base with an outer insulating pad between the fixing cylinder and the base. The fixing cylinder is covered by a shielding shell, and the top of the shielding shell is equipped with a matching shielding cover. Both the shielding shell and the shielding cover can shield external interference electric fields to avoid changes in the surrounding environment from interfering with the accuracy of the test. The shielding cover has an upward-protruding sample mounting port in the middle, which can stably mount the sample on the shielding cover and ensure that the sample being tested does not fall off during the puncture process.

[0023] An inner insulating pad is located at the bottom of the fixed cylinder to prevent electrostatic charge from escaping through the inner sleeve. A friction cylinder, made of rubber, is placed on top of the inner insulating pad and rests on it. A photosensitive film is spaced at the center of the friction cylinder, meaning the film is located in the center and does not contact the friction cylinder at any point. Falling debris enters the electrostatic field, and the photosensitive film records the sparks generated during electrostatic discharge. The photosensitive film is cross-shaped and is placed vertically on the inner insulating pad via a photosensitive film base. Specifically, the photosensitive film is vertically inserted... The photosensitive film is attached to the base of the photosensitive film, which is placed on the inner insulating pad. The photosensitive film is not in contact with the friction cylinder at all sides. The height of the photosensitive film and the base is the same as that of the friction cylinder. The friction cylinder is equipped with a retractable friction rod inside it. The friction rod includes a friction part and a handle part. The surface of the friction part is covered with fur. The handle part is connected to the friction part by a limiting ring protrusion. The limiting ring protrusion is made of insulating material. When the friction rod is pulled up and down, the friction between the friction rod and the friction cylinder generates charges and forms a potential difference, creating an electrostatic field inside the friction cylinder.

[0024] In use, this invention provides a method for determining the puncture and shedding debris of rubber stoppers used in the outer packaging of human medical infusion liquid products, comprising the following steps:

[0025] a. Preparation of the sample to be tested

[0026] Take the sample to be tested and gently shake it in 75% alcohol. Use clean metal tweezers to remove the sample and place it on a perforated wire mesh frame. Air dry it at a constant temperature of 30℃ for later use.

[0027] b. Preparation of measuring apparatus

[0028] Wipe the surface of the friction cylinder with 75% alcohol and place it on a perforated wire mesh frame to air dry at a constant temperature of 30°C. Insert the photosensitive film into the photosensitive film base and turn on the anti-static fan in the darkroom to blow air onto the surface of the photosensitive film and the photosensitive film base for 1 minute. Use the anti-static fan to blow air onto the surfaces of each connecting part of the device for 3 minutes. Place the photosensitive film and the photosensitive film base in the center of the inner insulating pad, i.e., the center position of the device, in the darkroom.

[0029] c, friction

[0030] Insert the friction rod into the friction cylinder, hold the handle of the friction rod and pull the friction rod up and down in the vertical direction to make the friction rod rub against the friction cylinder. Remove the friction rod, put the friction cylinder into the fixed cylinder after friction, and cover it with the shielding cover.

[0031] d. Puncture test

[0032] Install the test sample prepared in step a into the sample mounting port, and remove the entire device from the dark chamber; hold the puncture device and perform a puncture on the test sample once.

[0033] e. Calculation and Judgment

[0034] After the test, place the device back in the darkroom, remove the photosensitive film, illuminate the film with a UV lamp, observe and record the number of exposure points, or observe after developing the film with developer; the number of exposure points appearing on the photosensitive film is the number of debris particles; if the sum of the number of exposure points on the surface of the photosensitive film is more than the maximum allowable number of particles per sample specified in the standard, it does not meet the requirements; otherwise, it meets the requirements.

[0035] Compared with the prior art, the present invention has the following beneficial effects:

[0036] This invention utilizes the phenomenon that falling debris alters the local electrostatic charge value. Through theoretical analysis, practical operation, and data statistics, it discloses a more suitable method for measuring puncture debris compared to existing methods. By observing the magnitude of the change in value, the amount of debris is reflected, establishing a corresponding relationship to achieve the expected function. This invention fundamentally solves many drawbacks of existing methods for measuring puncture debris using visual observation, such as inaccurate results and the lack of complete and standardized reference criteria. Furthermore, this invention can also be applied to the measurement of debris volume that cannot be observed with normal human vision, especially in arbitration testing and microscopic material research, providing a completely new solution that can observe small-diameter debris that cannot be observed by existing methods.

[0037] The device and method for measuring the puncture debris of rubber stoppers used in the outer packaging of liquid products for human medical infusion disclosed in this invention can effectively observe small-diameter debris by establishing a correspondence between the number of signal occurrences and the number of adsorbed debris, accurately measure the number of debris, facilitate the establishment of a unified standard for puncture debris, and is suitable for the introduction of a unified standard. Attached Figure Description

[0038] Figure 1 This is a schematic diagram of the device in Embodiment 1 of the present invention.

[0039] Figure 2 This is a cross-sectional view of the partial structure in Embodiment 1 of the present invention in which the friction rod is installed.

[0040] Figure 3 This is a cross-sectional view of the part of the structure in Embodiment 1 of the present invention without the friction rod installed.

[0041] Figure 4 The number of times debris occurred in Example 1.

[0042] Figure 5 This refers to a single chip peak in Example 1.

[0043] Figure 6 This is a schematic diagram of the device in Embodiment 2 of the present invention.

[0044] Figure 7This is an exposure effect diagram of Example 2.

[0045] In the figure: 1-fixed cylinder, 2-base, 3-outer insulating pad, 4-shielding shell, 5-shielding cover, 6-sample mounting port, 7-inner insulating pad, 8-metal guide block, 9-friction cylinder, 10-friction rod, 1001-friction part, 1002-handle part, 1003-limiting ring protrusion, 11-wire, 12-electrometer, 13-oscilloscope, 14-support ring, 15-sample under test, 16-photosensitive film, 17-photosensitive film base. Implementation

[0046] The specific embodiments of the present invention will now be described in detail with reference to the accompanying drawings. Example 1

[0047] A device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion, such as... Figures 1-3 As shown: The fixing cylinder 1 is made of metal and is set on the base 2. An outer insulating pad 3 is placed between the fixing cylinder 1 and the base 2. The fixing cylinder 1 is covered by a shielding shell 4. The top of the shielding shell 4 is equipped with a matching shielding cover 5. Both the shielding shell 4 and the shielding cover 5 can shield the external interference electric field and avoid the surrounding environment from interfering with the accuracy of the test. The shielding cover 5 has an upward-protruding sample mounting port 6 in the middle. The sample mounting port 6 can stably install the sample on the shielding cover 5 and ensure that the sample being tested does not fall off during the puncture process.

[0048] An inner insulating pad 7 is provided at the bottom of the fixed cylinder 1 to prevent static charge from escaping through the inner sleeve. A metal conductor block 8 is provided above the inner insulating pad 7. A friction cylinder 9 is ringed around the upper part of the metal conductor block 8. The friction cylinder 9 is made of rubber. A support ring 14 is fixed to the lower inner wall of the fixed cylinder 1. The support ring 14 is located in the middle of the metal conductor block 8, and there is a gap between the support ring 14 and the metal conductor block 8. The friction cylinder 9 is placed on the support ring 14 and is tightly installed in the fixed cylinder 1 to prevent movement during friction. A retractable friction rod 10 is provided in the center of the friction cylinder 9 above the metal conductor block 8. The friction rod 10 includes a friction part 1001 and a handle part 1002. The surface of the friction part 1001 is covered with fur. The handle part 1002 is connected to the friction part 1001 by a limiting ring protrusion 1003. 3. Made of insulating material, when the friction rod 10 is pulled up and down, the friction rod 10 and the friction cylinder 9 generate charge and form a potential difference. When the limiting ring protrusion 1003 of the friction rod 10 abuts against the top of the friction cylinder 9, that is, when the friction rod 10 is in the lower stroke, there is a gap between the free end of the friction part 1001 and the top surface of the metal guide block 8. The lower part of the metal guide block 8 is connected to the electrometer 12 and the oscilloscope 13. The electrometer 12 is used to verify whether static charge is generated, and the oscilloscope 13 is used to monitor the instantaneous amplitude peak during electrostatic discharge. The electrometer 12 and the oscilloscope 13 are both connected to the metal guide block 8 through the wires 11 that pass through the lower part of the fixed cylinder 1 and the shielding shell 4. The electrometer 12 and the oscilloscope 13 are both grounded, that is, the electrometer 12 and the oscilloscope 13 are connected in parallel, with one end connected to the metal guide block 8 and the other end grounded.

[0049] In use, this invention provides a method for determining the puncture and shedding debris of rubber stoppers used in the outer packaging of human medical infusion liquid products, comprising the following steps:

[0050] a. Preparation of the sample to be tested

[0051] Take the sample to be tested 15 and place it in 75% alcohol, shake it slightly and soak for 5 minutes. Use clean metal tweezers to remove the sample to be tested 15 and place it on a perforated wire mesh frame, ensuring that the sample to be tested 15 is in contact with other objects. Use a constant temperature oven to air dry at 30℃ for 5 minutes for later use.

[0052] b. Preparation of measuring apparatus

[0053] The measured ambient temperature was 23℃±2℃, temperature fluctuation was ≤2℃; relative humidity range was 35%~40%; atmospheric pressure range was 700hPa~1060hPa; illuminance was 300LX; laboratory floor was epoxy antistatic self-leveling compound (optional); laboratory cleanliness was Class 100,000 (optional); open the shielding cover 5 and place it upside down on the clean workbench for later use. Take out the friction cylinder 9 and wipe its surface with 75% alcohol. The surface of the wiped material should not shed lint. Place the friction cylinder 9 on the perforated wire mesh frame and air dry it in a constant temperature chamber at 30℃ for 5 minutes. Install the air-dried friction cylinder 9 into the fixed cylinder 1. Place the friction cylinder 9 on the support ring 14 and ensure that the lower part of the friction cylinder 9 is interference-fitted with the metal guide block 8 to prevent it from being pulled out of the fixed cylinder 1 by the friction rod 10 during friction. Insert the friction rod 10 completely into the friction cylinder 9 and use an antistatic fan to blow air onto the surfaces of each connection part of the device for 3 minutes. Then zero the electrometer 12.

[0054] c. Rub and record the initial electrostatic value.

[0055] Hold the handle 1002 of the friction rod 10 and pull the friction rod up and down 20 times in a vertical direction to make the friction rod 10 rub against the friction cylinder 9. Take out the friction rod 10, cover it with the shielding cover 5, and record the value of the electrometer 12 after it stabilizes.

[0056] d. Puncture test

[0057] Store the test waveform in the oscilloscope's memory for detailed study; select the current range for the vertical system and set the correct magnification; set the horizontal system to 20nS / div~50nS / div; set the trigger mode to single trigger and the trigger type to rising edge; install the test sample 15 prepared in step a into the sample mounting port 6, hold the puncture device (the puncture device specified in YBB00332004-2015 "Test Method for Puncture and Shedding of Rubber Stoppers and Gaskets for Injection"), puncture the test sample 15 once, and record the waveform displayed on the oscilloscope 13 for future reference; remove the punctured test sample 15, replace it with a new test sample, and similarly perform one puncture, recording the waveform displayed on the oscilloscope 13 for future reference;

[0058] e. Calculation and Judgment

[0059] like Figure 4 , 5 As shown: retrieve the waveform record of oscilloscope 13 during the puncture period and observe the number of peaks that appear on oscilloscope 13. The number of waveforms that appear during the puncture period is the number of falling debris particles. If the number of waveforms that appear during the puncture period is more than the maximum allowable number of particles per sample specified in the standard, it does not meet the requirements; otherwise, it meets the requirements. Example 2

[0060] A device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion, such as... Figure 6 As shown: The fixing cylinder 1 is made of metal and is set on the base 2. An outer insulating pad 3 is placed between the fixing cylinder 1 and the base 2. The fixing cylinder 1 is covered by a shielding shell 4. The top of the shielding shell 4 is equipped with a matching shielding cover 5. Both the shielding shell 4 and the shielding cover 5 can shield the external interference electric field and avoid the surrounding environment from interfering with the accuracy of the test. The shielding cover 5 has an upward-protruding sample mounting port 6 in the middle. The sample mounting port 6 can stably install the sample on the shielding cover 5 and ensure that the sample being tested does not fall off during the puncture process.

[0061] An inner insulating pad 7 is provided at the bottom of the fixed cylinder 1 to prevent static charge from escaping through the inner sleeve. A friction cylinder 9 is provided above the inner insulating pad 7 and is placed on the inner insulating pad 7. The friction cylinder 9 is made of rubber and has a photosensitive film 16 spaced in the center of the friction cylinder 9. That is, the photosensitive film 16 is located in the center of the friction cylinder and does not contact the friction cylinder 9 on all sides. When the debris enters the electrostatic field, the photosensitive film 16 records the sparks generated during electrostatic discharge. The photosensitive film 16 is cross-shaped and is placed vertically on the inner insulating pad 7 through the photosensitive film base 17. Specifically, the photosensitive film 16 is vertically inserted into the photosensitive pad 7. Inside the film base 17, the photosensitive film base 17 is placed on the inner insulating pad 7. The photosensitive film 16 is not in contact with the friction cylinder 9 around its perimeter. The height of the photosensitive film 16 and the photosensitive film base 17 is the same as that of the friction cylinder 9. The friction cylinder 9 is equipped with a retractable friction rod 10 inside it. The structure of the friction rod 10 is completely consistent with that in Embodiment 1, including a friction part and a handle part. The surface of the friction part is covered with fur. The handle part and the friction part are connected by a limiting ring protrusion. The limiting ring protrusion is made of insulating material. When the friction rod is pulled up and down, the friction between the friction rod and the friction cylinder generates charges and forms a potential difference, thus forming an electrostatic field inside the friction cylinder.

[0062] In use, this invention provides a method for determining the puncture and shedding debris of rubber stoppers used in the outer packaging of human medical infusion liquid products, comprising the following steps:

[0063] a. Preparation of the sample to be tested

[0064] Take the sample to be tested 15 and place it in 75% alcohol, shake it slightly and soak for 5 minutes. Use clean metal tweezers to remove the sample to be tested 15 and place it on a perforated wire mesh frame, ensuring that the sample to be tested 15 is in contact with other objects. Use a constant temperature oven to air dry at 30℃ for 5 minutes for later use.

[0065] b. Preparation of measuring apparatus

[0066] The measured ambient temperature was 23℃±2℃, with a temperature fluctuation of ≤2℃; relative humidity range was 35%~40%; atmospheric pressure range was 700hPa~1060hPa; illuminance was 300LX; laboratory floor was epoxy anti-static self-leveling compound (optional); laboratory cleanliness was Class 100,000 (optional); the surface of the friction cylinder 9 was wiped with 75% alcohol, and no lint was left on the surface of the wiped object. The friction cylinder 9 was then placed on a perforated wire mesh frame and air-dried at 30℃ for 5 minutes in a constant temperature chamber; the photosensitive film 16 was inserted into the photosensitive film base 17, and the anti-static fan was turned on in the darkroom to blow air onto the surface of the photosensitive film 16 and the photosensitive film base 17 for 1 minute; the anti-static fan was used to blow air onto the surface of each connecting part of the device for 3 minutes, and the photosensitive film 16 and the photosensitive film base 17 were placed in the center of the inner insulating pad 7, i.e., the center position of the device, in the darkroom;

[0067] c, friction

[0068] Insert the friction rod 10 into the friction cylinder 9, hold the handle 1002 of the friction rod 10, and pull the friction rod up and down 20 times in the vertical direction to make the friction rod 10 rub against the friction cylinder 9. Take out the friction rod 10 and put it into the fixed cylinder 1, and cover it with the shielding cover 5.

[0069] d. Puncture test

[0070] Install the test sample 15 prepared in step a into the sample installation port 6, and use the puncture device (the puncture device specified in YBB00332004-2015 "Test Method for Puncture and Shedding of Rubber Stoppers and Gaskets for Injection") to puncture the test sample 15 once.

[0071] e. Calculation and Judgment

[0072] like Figure 7 As shown: After the test, place the device back in the darkroom, take out the photosensitive film, irradiate the film with a UV lamp, observe and record the number of exposure points, or observe after developing the film with developer; the number of exposure points appearing on the photosensitive film is the number of debris particles; if the sum of the number of exposure points appearing on the surface of the photosensitive film is more than the maximum allowable number of particles for a single sample specified in the standard, it does not meet the requirements; otherwise, it meets the requirements.

[0073] The simulation test results are shown in the table below.

[0074]

[0075] Conclusion: All 10 samples met the requirements.

[0076] The scope of protection claimed by this invention is not limited to the specific embodiments described above. Moreover, for those skilled in the art, this invention can have various modifications and alterations. Any modifications, improvements, and equivalent substitutions made within the concept and principles of this invention should be included within the scope of protection of this invention.

Claims

1. A device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion, characterized in that: Includes a fixing cylinder (1), which is mounted on a base (2), and an outer insulating pad (3) is placed between the fixing cylinder (1) and the base (2); the fixing cylinder (1) is covered with a shielding shell (4), and the top of the shielding shell (4) is provided with a matching shielding cover (5), and the shielding cover (5) has an upwardly protruding sample mounting port (6) in the middle. The bottom of the fixed cylinder (1) is provided with an inner insulating pad (7), and a metal guide block (8) is provided above the inner insulating pad (7). A friction cylinder (9) is wrapped around the upper part of the metal guide block (8). A retractable friction rod (10) is provided in the center of the friction cylinder (9) above the metal guide block (8). The lower part of the metal guide block (8) is connected to an electrometer (12) and an oscilloscope (13).

2. The device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 1, characterized in that: A support ring (14) is fixed to the lower inner wall of the fixed cylinder (1), and the friction cylinder (9) is placed on the support ring (14).

3. The device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 2, characterized in that: The support ring (14) is located in the middle of the metal guide block (8).

4. The device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 1, characterized in that: The electrometer (12) and oscilloscope (13) are both connected to the metal conductor (8) through wires (11) passing through the bottom of the fixed cylinder (1) and the shielding shell (4), and both the electrometer (12) and oscilloscope (13) are grounded.

5. A device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of liquid products for human medical infusion, characterized in that: Includes a fixing cylinder (1), which is mounted on a base (2), and an outer insulating pad (3) is placed between the fixing cylinder (1) and the base (2); the fixing cylinder (1) is covered with a shielding shell (4), and the top of the shielding shell (4) is provided with a matching shielding cover (5), and the shielding cover (5) has an upwardly protruding sample mounting port (6) in the middle. The bottom of the fixed cylinder (1) is provided with an inner insulating pad (7), and a friction cylinder (9) is provided above the inner insulating pad (7). A photosensitive film (16) is provided in the center of the friction cylinder (9). The photosensitive film (16) is placed vertically on the inner insulating pad (7) through the photosensitive film base (17). The friction cylinder (9) is equipped with a friction rod (10) that can be pulled out inside it.

6. The device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 5, characterized in that: The photosensitive film (16) is cross-shaped and is vertically inserted into the photosensitive film base (17). The height of the photosensitive film (16) together with the photosensitive film base (17) is the same as that of the friction cylinder (9).

7. A device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 1 or 5, characterized in that: The friction rod (10) includes a friction part (1001) and a handle part (1002). The handle part (1002) and the friction part (1001) are connected by a limiting ring protrusion (1003). The surface of the friction part (1001) is covered with fur. The friction cylinder (9) is made of rubber.

8. The device for measuring the puncture and shedding of rubber stoppers used in the outer packaging of human medical infusion liquid products according to claim 7, characterized in that: When the limiting ring protrusion (1003) of the friction rod (10) abuts against the top of the friction cylinder (9), there is a gap between the free end of the friction part (1001) and the top surface of the metal guide block (8).

9. A method for determining the shedding material from puncture stoppers used in the outer packaging of liquid products for human medical infusion, characterized in that: Includes the following steps: a. Preparation of the sample to be tested Take the sample to be tested and gently shake it in 75% alcohol. Use clean metal tweezers to remove the sample and place it on a perforated wire mesh frame. Air dry it at a constant temperature of 30°C for later use. b. Preparation of measuring apparatus The shielding shell (4) is equipped with a matching shielding cover (5) at the top. The shielding cover (5) has an upward-protruding sample mounting port (6) in the middle. Open the shielding cover (5), take out the friction cylinder (9), wipe the surface of the friction cylinder (9) with 75% alcohol, and place the friction cylinder (9) on the hollow wire mesh frame and air dry it at a constant temperature of 30°C. Install the air-dried friction cylinder (9) into the fixed cylinder (1), place the friction cylinder (9) on the support ring (14), and the lower part of the friction cylinder (9) is press-fitted with the metal guide block (8). The lower part of the metal guide block (8) is connected to the electrometer (12) and the oscilloscope (13). Insert the friction rod (10) completely into the friction cylinder (9), use an anti-static fan to blow air onto the surface of each connecting part of the device for 3 minutes, and then zero the electrometer (12). c. Rub and record the initial electrostatic value. Hold the handle (1002) of the friction rod (10) and pull the friction rod (10) up and down in the vertical direction to make the friction rod (10) rub against the friction cylinder (9) fully. Take out the friction rod (10), cover it with the shielding cover (5), and record the value of the electrometer (12) after it stabilizes at this moment. d. Puncture test Install the test sample prepared in step a into the sample installation port (6), hold the puncture device and puncture the test sample once, record the waveform displayed on the oscilloscope (13) for future reference; remove the punctured test sample (15), replace it with a new test sample, and similarly perform one puncture, record the waveform displayed on the oscilloscope (13) for future reference. e. Calculation and Judgment Retrieve the waveform record of the oscilloscope (13) during the puncture period and observe the number of peaks that appear on the oscilloscope (13). The number of waveforms that appear during the puncture period is the number of falling debris particles. If the number of waveforms that appear during the puncture period is more than the maximum allowable number of particles per sample specified in the standard, it does not meet the requirements; otherwise, it meets the requirements.

10. A method for determining the shedding material from puncture of rubber stoppers used in the outer packaging of human medical infusion liquid products, characterized in that: Includes the following steps: a. Preparation of the sample to be tested Take the sample to be tested and gently shake it in 75% alcohol. Use clean metal tweezers to remove the sample and place it on a perforated wire mesh frame. Air dry it at a constant temperature of 30°C for later use. b. Preparation of measuring apparatus The shielding housing (4) is equipped with a matching shielding cover (5) at the top. The shielding cover (5) has an upward-protruding sample mounting port (6) in the middle. Wipe the surface of the friction cylinder (9) with 75% alcohol and place the friction cylinder (9) on the hollow wire mesh frame and air dry it at a constant temperature of 30°C. Insert the photosensitive film (16) into the photosensitive film base (17). Turn on the anti-static fan in the dark room and blow air onto the surface of the photosensitive film (16) and the photosensitive film base (17) for 1 minute. Use the anti-static fan to blow air onto the surface of each connecting part of the device for 3 minutes. Place the photosensitive film (16) and the photosensitive film base (17) in the center of the inner insulating pad (7) in the dark room, which is the center position of the device. c, friction Insert the friction rod (10) into the friction cylinder (9), hold the handle (1002) of the friction rod (10) and pull the friction rod (10) up and down in the vertical direction to make the friction rod (10) rub against the friction cylinder (9) fully. Take out the friction rod (10), put the friction cylinder (9) after friction into the fixed cylinder (1), and cover the shielding cover (5). d. Puncture test Install the sample to be tested prepared in step a into the sample mounting port (6), and remove the entire device from the dark chamber; hold the puncture device and perform a puncture on the sample to be tested; e. Calculation and Judgment After the experiment, place the device back in the darkroom, take out the photosensitive film, illuminate the film with a UV lamp, observe and record the number of exposure points, or observe after developing the film with developer; the number of exposure points appearing on the photosensitive film is the number of debris particles. If the total number of exposure spots on the surface of the photographic film exceeds the maximum allowable number of particles per sample specified in the standard, it does not meet the requirements; otherwise, it does meet the requirements.

Images