CN112957540B - Needle tube for safety insulin pen needle - Google Patents
Needle tube for safety insulin pen needle Download PDFInfo
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- CN112957540B CN112957540B CN202110160741.6A CN202110160741A CN112957540B CN 112957540 B CN112957540 B CN 112957540B CN 202110160741 A CN202110160741 A CN 202110160741A CN 112957540 B CN112957540 B CN 112957540B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/08—Materials for coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/16—Biologically active materials, e.g. therapeutic substances
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M5/00—Devices for bringing media into the body in a subcutaneous, intra-vascular or intramuscular way; Accessories therefor, e.g. filling or cleaning devices, arm-rests
- A61M5/178—Syringes
- A61M5/31—Details
- A61M5/32—Needles; Details of needles pertaining to their connection with syringe or hub; Accessories for bringing the needle into, or holding the needle on, the body; Devices for protection of needles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/216—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with other specific functional groups, e.g. aldehydes, ketones, phenols, quaternary phosphonium groups
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
- A61L2300/606—Coatings
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
- A61M2205/00—General characteristics of the apparatus
- A61M2205/02—General characteristics of the apparatus characterised by a particular materials
- A61M2205/0238—General characteristics of the apparatus characterised by a particular materials the material being a coating or protective layer
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Abstract
The invention discloses a needle tube for a safe insulin pen needle; the preparation method comprises the following steps: pretreating a stainless steel needle tube; forming composite sol by using 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone, a mixture of the cohnolidol diol, KH560 and tetraethyl orthosilicate; coating by adopting a dipping-pulling method to form a coating, then carrying out heat treatment and cooling to obtain a first hybrid layer; and repeating the steps to form a second coating until 3-5 modification layers are obtained, forming a hybrid composite layer coated on the surface of the needle tube, and thus obtaining the needle tube. The needle tube has excellent biological corrosion resistance and antibacterial property, the puncture force for puncturing the skin is as low as less than half of the national standard, so that the human body hardly generates pain, and the needle tube is safe and nontoxic; the needle tube has wide application in a safe insulin pen needle.
Description
Technical Field
The invention belongs to the technical field of medical instruments, and particularly relates to a needle tube for a safe insulin pen needle.
Background
Insulin injection devices such as insulin pens and injection needles have been widely used as a method for treating diabetes. The main function of the device is to accurately infuse insulin into the body of a diabetic patient through an injection device so as to achieve the purpose of controlling the blood sugar of the patient. The injection needle used in the insulin injection device is generally made of stainless steel. However, the corrosion problem of stainless steel materials has been concerned because the corrosion problem has greatly limited the range and age of its use and caused serious loss to national economy. The preparation of protective coatings on stainless steel surfaces is one of the most important and commonly used methods to prevent or control metal corrosion.
At present, stainless steel in metal medical materials is widely applied in clinical medicine, such as a needle tube of a safe insulin pen needle; however, stainless steel has a series of inevitable problems in practical use, such as high temperature oxidation, acid corrosion, etc., which results in serious waste and significant loss of the stainless steel material; therefore, the metal surface corrosion prevention technology has been widely focused and researched, and among them, the technology is most widely used, namely, a metal or non-metal coating is prepared on the metal surface by various methods to promote the metal corrosion resistance; with the development of modern industry, the performance requirements of metal surfaces are higher, including corrosion resistance, wear resistance and high temperature resistance, so that the coating technology of the metal surfaces is rapidly developed and applied under the background, and the coating technology is widely applied in the medical field. In addition, the needle tube penetrating into the skin to cause no pain to the human body and the preparation of safe and nontoxic needle tubes are also subject studies conducted by many researchers to make the needle tubes be better applied to the medical field.
Disclosure of Invention
The invention aims to provide a composite sol with better stability, which is coated on the surface of a stainless steel needle tube to form a hybrid layer, so that the needle tube has excellent biological corrosion resistance and antibacterial property, the puncture force for puncturing the skin is as low as less than half of the national standard, the human body hardly generates pain, and the composite sol is safe and nontoxic; the needle tube has wide application in a safe insulin pen needle.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a needle cannula for a safety insulin pen needle comprising: a stainless steel needle tube;
the surface of the stainless steel needle tube is coated with a hybrid layer obtained by processing a composite sol prepared from a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol, KH560 and tetraethyl orthosilicate.
The composite sol is prepared from a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol, KH560 and tetraethyl orthosilicate, and has excellent stability; the hybrid coating is coated on the surface of the needle tube to form a hybrid coating, so that the needle tube has excellent biological corrosion resistance and antibacterial property; the reason may be that tetraethyl orthosilicate is hydrolyzed and is subjected to condensation polymerization with KH560 to form a certain network structure through crosslinking, a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol enters the network structure to form a firm covalent bond, and the prepared composite sol is uniformly coated on the surface of the needle tube, so that the needle tube has excellent biological corrosion resistance and antibacterial property; meanwhile, the needle tube penetrates into the skin by using the puncture force which is less than half of the national standard, so that the human body hardly generates pain, and the needle tube is safe and nontoxic.
Preferably, in the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the colelactone diol, the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the colelactone is 0.5-1.2: 1.
Preferably, the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the mixture of the colactone diol, KH560 and tetraethyl orthosilicate is 0.3-0.8: 0.25-0.6: 3.5-4.5.
Preferably, the number of layers of the hybrid coating is 3-5.
The invention also discloses application of the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the coriolide diol in improving the stability of the composite sol.
The invention also discloses application of the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol in improving the antibacterial property of a needle tube of a safety insulin pen needle.
The invention also discloses application of the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol in improving the antibacterial property of a needle tube of a safety insulin pen needle.
The invention also discloses a preparation method of the needle tube for the safe insulin pen needle.
A preparation method of a needle tube for a safe insulin pen needle comprises the following steps:
(1) pretreatment of a stainless steel needle tube: polishing a stainless steel needle tube, washing with water, drying, then placing in an ethanol solution for ultrasonic cleaning, then performing alkali cleaning, acid cleaning and water cleaning, finally performing ultrasonic cleaning in the ethanol solution, and drying for later use;
(2) preparing composite sol: forming a composite sol by using a sol-gel method to mix 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone with a mixture of colactone diol, KH560 and tetraethyl orthosilicate;
(3) preparing a coating: coating by adopting a dipping-pulling method, immersing the needle tube pretreated in the step (1) into the composite sol in the step (2), pulling the pretreated needle tube to form a coating, then carrying out heat treatment, and cooling to obtain a first hybrid layer;
(4) preparing a needle tube finished product: and (4) repeating the step (3) to form a second coating until 3-5 modification layers are obtained, forming a hybrid composite layer coated on the surface of the needle tube, and preparing the needle tube for the safe insulin pen needle.
Preferably, the preparation method of the composite sol is as follows:
placing tetraethyl orthosilicate and deionized water into a three-neck flask provided with a stirrer, a thermometer and a condenser, adding acetic acid serving as a catalyst and a small amount of absolute ethyl alcohol, magnetically stirring for 1-3 hours at 25-45 ℃, adding a mixture of KH560, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol, wherein the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolis lactone diol is 0.3-0.8: 0.25-0.6: 3.5-4.5, and continuously stirring for 12-18 hours to obtain the composite sol, wherein the weight ratio of the tetraethyl orthosilicate to the acetic acid to the deionized water is 3-5: 1.5-2.5: 45-60.
Preferably, the pH value of the composite sol is 5.5-6.5.
Preferably, the pulling rate of the needle tube in the step (3) is 1.2-3.2 cm/min.
Preferably, in the step (3), the heat treatment temperature of the needle tube coating is 80-170 ℃, and the treatment time is 4-8 min.
Preferably, the diameter of the needle tube is 0.2-0.35 mm, and the length is 3-15 mm.
The invention adopts the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the collylidene diol, KH560 and tetraethyl orthosilicate to prepare the composite sol, and the composite sol is coated on the surface of the needle tube to form the hybrid coating, thereby having the following beneficial effects: the prepared composite sol has excellent stability; the surface of the needle tube is coated with the coating to form a hybrid layer, so that the needle tube has excellent biological corrosion resistance and antibacterial property; the reason may be that tetraethyl orthosilicate is hydrolyzed and is subjected to condensation polymerization with KH560 to form a certain net structure through crosslinking, and a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol enters the net structure to form a firm covalent bond which is uniformly coated on the surface of the needle tube, so that the needle tube has excellent biological corrosion resistance and antibacterial property; meanwhile, the needle tube penetrates into the skin by using the puncture force which is less than half of the national standard, so that the human body hardly generates pain, and the needle tube is safe and nontoxic; the needle tube has wide application in a safe insulin pen needle. Therefore, the invention prepares a compound sol with better stability, and the compound sol is coated on the surface of a stainless steel needle tube to form a hybrid layer, so that the needle tube has excellent biological corrosion resistance and antibacterial property, the puncture force for puncturing the skin is as low as less than half of the national standard, the human body can hardly generate pain, and the compound sol is safe and nontoxic; the needle tube has wide application in a safe insulin pen needle.
Drawings
FIG. 1 shows the time at which gelation of the composite sol occurs;
FIG. 2 is a graph showing the self-corrosion potential of the syringe;
FIG. 3 shows the penetration force of the needle cannula.
Detailed Description
In order to further improve the stability of the composite sol and enable the needle tube to have better biological corrosion resistance, the invention adopts the following preferable measures:
adding a mixture of cyanidin 3-xyloside and citric acid fatty acid glyceride in the preparation process of the composite sol, wherein the weight ratio of the cyanidin 3-xyloside to the citric acid fatty acid glyceride is 1: 0.2-0.5, and the addition amount of the mixture of the cyanidin 3-xyloside and the citric acid fatty acid glyceride is 0.5-0.8% of the weight percentage of the composite sol; the addition of the mixture of cyanidin 3-xyloside and citric acid fatty glyceride further improves the biological corrosion resistance and the antibacterial property of the needle tube; the reason may be that the cyanidin 3-xyloside and citric acid fatty glyceride mixture and other components in the sol generate synergistic effect, so that the stability of the composite sol is improved, the physical and chemical properties of the composite sol are improved, and the composite sol is coated on the surface of the needle tube to form a hybrid layer, so that the biological corrosivity and the antibacterial property of the needle tube are improved.
The technical solution of the present invention is further described in detail below with reference to the following detailed description and the accompanying drawings:
example 1
A needle tube for a safe insulin pen needle is prepared by the following steps:
(1) pretreatment of a stainless steel needle tube: polishing a stainless steel needle tube, cleaning with distilled water, blow-drying, then placing in an ethanol solution for ultrasonic cleaning for 5min, then cleaning with a 5% sodium hydroxide solution for 3min, then cleaning with a 5% nitric acid solution for 3min, cleaning with distilled water, blow-drying, finally ultrasonic cleaning in the ethanol solution for 10min, and drying for later use;
(2) preparing composite sol: tetraethyl orthosilicate and deionized water are placed in a three-neck flask provided with a stirrer, a thermometer and a condenser tube, catalyst acetic acid and a small amount of absolute ethyl alcohol are added, magnetic stirring is carried out for 3 hours at the temperature of 35 ℃, wherein the weight ratio of tetraethyl orthosilicate, acetic acid and deionized water is 3.5:2:50, then a mixture of KH560, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and colactone diol is added, wherein the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolide is 0.7:1, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolide diol mixture, KH560 and tetraethyl orthosilicate are 0.6:0.45:4, the mixture is continuously stirred for 16H and aged to obtain composite sol, and the pH value of the composite sol is 6.3;
(3) preparing a coating: coating by adopting a dipping-pulling method, immersing the needle tube pretreated in the step (1) into the composite sol in the step (2), pulling the pretreated needle tube at a pulling rate of 2.5cm/min to form a coating, then placing the coating in a heating furnace, carrying out heat treatment at 110 ℃ for 6min, and cooling to obtain a first hybrid layer;
(4) preparing a needle tube finished product: and (4) repeating the step (3) to form a second coating until 3 modification layers are obtained, forming a hybrid composite layer coated on the surface of the needle tube, and preparing the needle tube for the safe insulin pen needle.
Example 2
A needle tube for a safe insulin pen needle is prepared by the following steps:
step (1) same as example 1;
(2) preparing composite sol: tetraethyl orthosilicate and deionized water are placed in a three-neck flask provided with a stirrer, a thermometer and a condenser tube, catalyst acetic acid and a small amount of absolute ethyl alcohol are added, magnetic stirring is carried out for 3 hours at the temperature of 35 ℃, wherein the weight ratio of tetraethyl orthosilicate, acetic acid and deionized water is 5:2:60, then a mixture of KH560, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and collylidene diol is added, wherein the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolide is 1:1, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolide diol mixture, KH560 and tetraethyl orthosilicate is 0.8:0.6:4.5, the mixture is continuously stirred for 14H and is aged to obtain composite sol, and the pH value of the composite sol is 6.5;
(3) preparing a coating: coating by adopting a dipping-pulling method, immersing the needle tube pretreated in the step (1) into the composite sol in the step (2), pulling the pretreated needle tube at a pulling rate of 1.5cm/min to form a coating, then placing the coating in a heating furnace, carrying out heat treatment at 150 ℃, wherein the treatment time is 4min, and cooling to obtain a first hybrid layer;
(4) preparing a needle tube finished product: and (4) repeating the step (3) to form a second coating until 3 modification layers are obtained, forming a hybrid composite layer coated on the surface of the needle tube, and preparing the needle tube for the safe insulin pen needle.
Example 3
The needle tube for the safe insulin pen needle has the same preparation steps as those of the embodiment 1, except that the preparation steps are as follows: in the step (2), the composite sol is prepared by placing tetraethyl orthosilicate and deionized water into a three-neck flask provided with a stirrer, a thermometer and a condenser, adding acetic acid serving as a catalyst and a small amount of absolute ethyl alcohol, magnetically stirring for 3 hours at 35 ℃ with the weight ratio of the tetraethyl orthosilicate to the acetic acid to the deionized water being 3.5:2:50, then adding KH560 and 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone with the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the KH560 and the tetraethyl orthosilicate being 0.6:0.45:4, continuously stirring for 12 hours, aging to obtain the composite sol, and measuring the pH value to be 6.2.
Example 4
The needle tube for the safe insulin pen needle has the same preparation steps as those of the embodiment 1, except that the preparation steps are as follows: in the step (2), the composite sol is prepared by placing tetraethyl orthosilicate and deionized water into a three-neck flask provided with a stirrer, a thermometer and a condenser tube, adding acetic acid serving as a catalyst and a small amount of absolute ethyl alcohol, magnetically stirring for 3 hours at 35 ℃, wherein the weight ratio of the tetraethyl orthosilicate to the acetic acid to the deionized water is 3.5:2:50, then adding KH560 and Coriolis lactone diol, wherein the weight ratio of the Coriolis lactone diol to the KH560 to the tetraethyl orthosilicate is 0.6:0.45:4, continuously stirring for 12 hours, aging to obtain the composite sol, and measuring the pH value of the composite sol to be 6.3.
Example 5
The needle tube for the safe insulin pen needle has the same preparation steps as those of the embodiment 1, except that the preparation steps are as follows: in the step (2), tetraethyl orthosilicate and deionized water are placed in a three-neck flask provided with a stirrer, a thermometer and a condenser, catalyst acetic acid and a small amount of absolute ethyl alcohol are added, magnetic stirring is carried out for 3 hours at 35 ℃, the weight ratio of tetraethyl orthosilicate, acetic acid and deionized water is 3.5:2:50, then KH560, a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol is added, the weight ratio of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to coriolis lactone is 0.7:1, 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to coriolis lactone, the weight ratio of KH560 and tetraethyl orthosilicate is 0.6:0.45:4, a mixture of cyanidin 3-xyloside and citric acid fatty glyceride is added, wherein the weight ratio of cyanidin 3-xyloside to citric acid fatty glyceride is 1:0.3, the addition amount of the mixture of cyanidin 3-xyloside and citric acid fatty glyceride is 0.7 percent of the weight percentage of the composite sol, the mixture is continuously stirred for 16 hours and aged to obtain the composite sol, and the pH value of the composite sol is measured to be 6.2.
Example 6
The needle tube for the safe insulin pen needle has the same preparation steps as those of the embodiment 1, except that the preparation steps are as follows: in the step (3), the coating is prepared by adopting a dipping-pulling method, the needle tube pretreated in the step (1) is immersed in the composite sol in the step (2), the pretreated needle tube is pulled at a pulling rate of 3cm/min to form a coating, then the coating is placed in a heating furnace for heat treatment at 150 ℃ for 5min, and the coating is cooled to obtain a first hybrid layer.
Comparative example 1
The needle tube for the safe insulin pen needle has the same preparation steps as those of the embodiment 1, except that the preparation steps are as follows: in the step (2), the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the colactone diol is not added in the preparation of the composite sol.
Comparative example 2
A needle tube for a safety insulin pen needle was made of a stainless steel needle tube without a hybrid layer as comparative example 2.
Test example 1
1. Determination of stability of composite Sol
The stability of the sol was judged by the time required for the sol sample to gel.
FIG. 1 shows the time at which gelation of the composite sol occurs. As can be seen from FIG. 1, the gelation time of the composite sol in examples 1 and 2 is higher than 30 days, the stability of the composite sol in example 1 is higher than that in examples 3-4 by comparing examples 1 and 3-4, which shows that the stability of the composite sol is improved by simultaneously adding a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and Coryliden diol to the composite sol; the gelation time of the composite sol in example 5 is not less than 40 days, and compared with examples 1 and 5, the gelation time of the composite sol in example 5 is higher than that in example 1, which shows that the stability of the composite sol is further improved by adding the mixture of cyanidin 3-xyloside and citric acid fatty glyceride in the composite sol.
Test example 2
1. Measurement of antibacterial Properties of needle tubes
This test prepared a suspension of bacteria (Staphylococcus aureus 3X 10) at a certain concentration7CFU/mL, E.coli 1.5X 107CFU/mL, Candida albicans 107CFU/mL, PBS suspension, pH 7.2), uniformly spraying a layer of bacteria liquid on the surface of the needle tube sample by using a spray can, repeating for three times, standing the sample for 1h, washing the bacteria on the surface of the needle tube by using PBS buffer solution, diluting to a proper time, and coating on a plate for counting. The removal rate of bacteria was calculated.
TABLE 1 antibacterial Rate (%) of needle tubing
As can be seen from table 1, the inhibition rates of the needle tubes in examples 1, 2 and 6 on staphylococcus aureus are higher than 90%, the inhibition rate of escherichia coli is higher than 87.5%, the inhibition rate of candida albicans is higher than 86%, and the inhibition rates of the needle tubes in comparative examples 1, 3-4 and 1 are higher than that of examples 3-4 and 1-2, which indicates that the inhibition rates of the needle tubes are improved by adding the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the collylactone diol into the composite sol, so that the needle tubes have better antibacterial property; comparing example 1 with example 5, the inhibition rate of example 5 on staphylococcus aureus is not obviously different from that of example 1, and the inhibition rate on escherichia coli and candida albicans is higher than that of example 1-2, which shows that the addition of the mixture of cyanidin 3-xyloside and citric acid fatty glyceride in the composite sol further improves the inhibition rate of the needle tube on escherichia coli and candida albicans, and has no obvious influence on the inhibition rate of staphylococcus aureus.
2. Determination of the resistance of a needle tube to biological corrosion
The self-corrosion potential is characteristic of electrochemical corrosion of metal materialFor the fundamental parameters of corrosion thermodynamics, in most cases, materials with lower values of the self-corrosion potential are more susceptible to electrochemical corrosion behavior. The electrochemical corrosion solution for the test adopts Hank's simulated body fluid (HBSS), the pH value is adjusted to 7.1-7.5 by 5.5 percent sodium bicarbonate before use, and the test temperature (37 +/-0.5) DEG C is maintained by using an HH-601A super constant temperature water bath. Before the electrochemical corrosion test, the sample is firstly immersed in a corrosion medium for stabilization for 30 min. Constant potential open circuit potential time curve parameters: the sensitivity is 1mA, the filtering parameter is 10Hz, the amplification factor is 1, the initial potential is-2.5V, the sampling interval time is 0.1s, and the measurement time is 1800 s. The potential adopts self-corrosion potential, the excitation signal is sine wave, the AC disturbance amplitude is 1mA, the amplification factor is 10mV, and the maximum frequency is 105Hz, minimum frequency of 10-2Hz, the current range is 1mA, and the amplification factor is 1. Linear scanning tafel curve test parameters: the sensitivity is 1mA current range, the filter parameter is 10Hz, the amplification factor is 1, the initial potential is-2.5V, the termination potential is 4.0V, and the scanning speed is 0.005V/s.
FIG. 2 shows the self-corrosion potential of the syringe. As can be seen from FIG. 2, the values of the self-corrosion potential of the composite sol are higher than-0.3V in the examples 1, 2 and 6, and higher than-0.3V in the comparative examples 1, 3-4 and 1-2 and higher than that of the examples 3-4 and 1-2, which shows that the mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the coriolide diol is added into the composite sol simultaneously, so that the self-corrosion potential of the needle tube is improved and is shifted to the positive potential value, namely, the needle tube has better biological corrosion resistance; the self-corrosion potential value of example 5 is higher than-0.2V, and compared with example 1 and example 5, the self-corrosion potential value of example 5 is higher than that of example 1, which shows that the addition of the mixture of cyanidin 3-xyloside and citric acid fatty acid glyceride in the composite sol further improves the biological corrosion resistance of the needle tube.
3. Determination of puncture force of needle tube
The puncture force of the needle tube is measured according to YBB 0009-: the prepared needle tube sample (specification: 0.3mm) and the simulated skin (polyurethane film, thickness: 0.35 + -0.05 mm) were left at (22 + -2) ° C for at least 24 hours and tested at the same temperature. The test specimens were mounted on a test machine with the axis perpendicular to the surface of the simulated skin and the tip pointing towards the center of the circular puncture area, with the simulated skin vertically punctured at a speed of (100 ± 10) mm/min, and the puncture test was performed while recording the maximum peak force.
TABLE 2 puncture force criteria
| Specification (mm) | Puncture force |
| 0.3～0.6 | ≤0.7 |
| 0.7～0.9 | ≤0.85 |
FIG. 3 shows the penetration force of the needle cannula. As can be seen from fig. 3, the piercing force of examples 1, 2 and 6 is less than 0.25N, i.e., less than half of the national standard, and the piercing into the skin hardly causes pain; comparing the example 1 with the examples 3-4 and the comparative examples 1-2, the puncture force of the example 1 is lower than that of the examples 3-4 and the comparative examples 1-2, which shows that the puncture force of the needle tube is reduced by simultaneously adding the mixture of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the coriolis lactone diol into the composite sol, probably because the hybrid layer formed on the surface of the needle tube plays a certain lubricating role and the pain feeling to the human body can be reduced when the needle tube is used; comparing example 1 with example 5, the puncture force of example 5 is almost the same as that of example 1, which shows that the mixture of cyanidin 3-xyloside and citric acid fatty glyceride is added into the composite sol, and a coating is formed on the surface of the needle tube, and the coating has no influence on the puncture force of the needle tube.
4. Determination of acute systemic toxicity of needle tubes
The test measures the acute systemic toxicity of the needle tube according to YBB 0009-; preparation of a test solution: and (3) immersing 20 needle tube samples into 250mL of sterile pyrogen-free 0.9% sodium chloride solution, keeping the temperature at 37 +/-0.3 ℃ for 1h, and taking out the needle tubes to obtain a test solution, wherein the storage time of the test solution cannot exceed 2 h. The test solution is taken and tested according to an acute systemic toxicity test method (YBB 00042003).
TABLE 3 acute systemic toxicity test results for needle cannula
| Test group | Phenomenon(s) |
| Example 1 | No toxic symptoms |
| Example 2 | No toxic symptoms |
| Example 3 | No toxic symptoms |
| Example 4 | No toxic symptoms |
| Example 5 | No toxic symptoms |
| Example 6 | No toxic symptoms |
As can be seen from Table 3, the needle cannulas in examples 1-6 have no acute systemic toxicity to human body, i.e. the needle cannulas have better safety to human body by coating the surface of the needle cannula with a composite sol layer containing a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and collylactone diol; and the mixture of cyanidin 3-xyloside and citric acid fatty glyceride is added into the composite sol, so that the non-toxic performance of the needle tube is not negatively influenced.
Conventional operations in the operation steps of the present invention are well known to those skilled in the art and will not be described herein.
The above embodiments are merely illustrative, and not restrictive, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention, and the protection scope of the present invention should be defined by the claims.
Claims (10)
1. A needle cannula for a safety insulin pen needle comprising: a stainless steel needle tube;
the surface of the stainless steel needle tube is coated with a hybrid layer obtained by treating a composite sol prepared from a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol, KH560 and tetraethyl orthosilicate.
2. The needle cannula of claim 1, wherein said safety insulin pen needle comprises: in the mixture of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and the coriolide diol, the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the coriolide is 0.5-1.2: 1.
3. The needle cannula of claim 1, wherein said safety insulin pen needle comprises: the weight ratio of the 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone to the mixture of the colactone diol, KH560 and tetraethyl orthosilicate is 0.3-0.8: 0.25-0.6: 3.5-4.5.
4. The needle cannula of claim 1, wherein said safety insulin pen needle comprises: the number of the hybrid layers is 3-5.
Use of a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis diol to increase the stability of a composite sol as claimed in claim 1.
Use of a mixture of 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone and coriolis lactone diol to increase the antimicrobial properties of the needle cannula of a safety insulin pen needle as claimed in claim 1.
7. The method for preparing a needle tube for a safety insulin pen needle as claimed in claim 1, comprising the steps of:
(1) pretreatment of a stainless steel needle tube: polishing a stainless steel needle tube, washing with water, drying, then placing in an ethanol solution for ultrasonic cleaning, then performing alkali cleaning, acid cleaning and water cleaning, finally performing ultrasonic cleaning in the ethanol solution, and drying for later use;
(2) preparing composite sol: forming a composite sol by using a sol-gel method to mix 3,4, 6-trimethoxy-1 (3H) -isobenzofuranone with a mixture of colactone diol, KH560 and tetraethyl orthosilicate;
(3) preparing a coating: coating by adopting a dipping-pulling method, immersing the needle tube pretreated in the step (1) into the composite sol in the step (2), pulling the pretreated needle tube to form a coating, then carrying out heat treatment, and cooling to obtain a first hybrid layer;
(4) preparing a needle tube finished product: and (4) repeating the step (3) to form a second coating until 3-5 modification layers are obtained, forming a hybrid composite layer coated on the surface of the needle tube, and preparing the needle tube for the safe insulin pen needle.
8. The method for preparing the needle tube of the safety insulin pen needle as claimed in claim 7, wherein the method comprises the following steps: the pulling rate of the needle tube in the step (3) is 1.2-3.2 cm/min.
9. The method for preparing the needle tube of the safety insulin pen needle as claimed in claim 7, wherein the method comprises the following steps: in the step (3), the heat treatment temperature of the needle tube coating is 80-170 ℃, and the treatment time is 4-8 min.
10. A needle tube for a safety insulin pen needle prepared by the preparation method of any one of claims 7 to 9.
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