CN111621053A - Glass slide for medical detection and preparation method thereof - Google Patents

Glass slide for medical detection and preparation method thereof Download PDF

Info

Publication number
CN111621053A
CN111621053A CN202010494349.0A CN202010494349A CN111621053A CN 111621053 A CN111621053 A CN 111621053A CN 202010494349 A CN202010494349 A CN 202010494349A CN 111621053 A CN111621053 A CN 111621053A
Authority
CN
China
Prior art keywords
slide
glass slide
vinyl
polyether ketone
medical
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202010494349.0A
Other languages
Chinese (zh)
Inventor
王健
孟庆涛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN202010494349.0A priority Critical patent/CN111621053A/en
Publication of CN111621053A publication Critical patent/CN111621053A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12Chemical modification
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/06Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
    • C08F283/065Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18Manufacture of films or sheets
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/08Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/16Cyclodextrin; Derivatives thereof

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Physics & Mathematics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Materials For Medical Uses (AREA)

Abstract

The invention discloses a preparation method of a glass slide for medical detection, which is characterized by comprising the following steps: s1, preparing vinyl-terminated hyperbranched polyether ketone, S2, molding glass slide, and S3, and modifying the surface. The invention also provides a glass slide for medical detection prepared according to the preparation method of the glass slide for medical detection. The slide glass for medical detection disclosed by the invention is excellent in comprehensive performance, good in hydrophilicity, good in anti-falling effect and excellent in mechanical property.

Description

Glass slide for medical detection and preparation method thereof
Technical Field
The invention relates to the technical field of medical detection, in particular to a glass slide for medical detection and a preparation method thereof.
Background
In recent years, with the development of economy and the continuous improvement of living standard, people have more and more urgent desires to improve physical quality and medical treatment environment. Medical testing is a key technology for doctors to diagnose diseases, and the accuracy and precision of medical testing directly determine the effectiveness of treatment. The accurate medical detection can effectively improve the accuracy of disease diagnosis, thereby improving the success rate of treatment, improving the survival quality of patients and lightening the economic burden of the patients and family members thereof.
The glass slide is used in the medical detection process, the glass slide refers to a glass sheet or a quartz sheet for placing materials, when a sample is manufactured, a cell or tissue slice is placed on the glass slide, and then a cover glass is used for covering the glass slide, so that the function of the glass slide is realized.
The slide quality level of selling on the existing market is not uniform, some slides when carrying out experimental analysis, produce the piece easily, and the slide of producing among the prior art is difficult to wash, carry out many times experimental back, the partial material on slide surface can remain on the slide surface, consequently, can bring certain influence for the use of slide, the slide life-span of producing among the prior art is shorter, the number of times of use is limited, after repetitious usage and washing, can form on the slide surface and scrape violently, thereby influence the use of slide. The common glass slide glass on the market has thin and crisp performance and is easy to break, so care must be taken in the manufacturing and using processes, the glass slide glass can be broken by slight carelessness, specimens are damaged, and particularly some precious specimens are difficult to recover, so that the loss which is difficult to compensate is caused. On the other hand, for some specific precision instruments, ordinary hydrophobic slides cannot be used. Such as Roche full-automatic immunohistochemistry (Roche) instrument, because it contains a liquid cover film which is easy to adhere to a hydrophobic glass slide, the tissue staining is not uniform, and the test fails.
The Chinese patent application No. 201410849438.7 discloses a preparation method and a use method of a hydrophilic adhesive glass slide, wherein the glass slide is pretreated by 0.8-8% of aminosilane solution or 0.1-1% of polylysine solution, washed by water, dried, soaked in 0.5-5% of albumin solution, taken out, washed by water and dried to obtain the hydrophilic adhesive glass slide. The hydrophilic glass slide surface has hydrophilic groups, has good compatibility with biological macromolecules and strong adhesion performance, and makes the water-based reagent easily and uniformly spread on the glass slide surface, thereby overcoming the defect that the common adhesive glass slide is frequently dyed non-uniformly when used on an automatic immunohistochemical instrument. However, the glass slide does not improve the fragile performance, and the hydrophilic coating is easily peeled off from the surface of the glass slide, thereby affecting the detection accuracy.
Therefore, the development of the hydrophilic non-glass slide glass with excellent comprehensive performance, good anti-falling effect and excellent mechanical property meets the market demand, has wide market value and application prospect, and plays a very important role in promoting the development of the medical detection industry.
Disclosure of Invention
In view of this, the invention aims to provide a glass slide for medical detection and a preparation method thereof, wherein the preparation method is simple and easy to implement, high in preparation efficiency, low in preparation cost and suitable for industrial production. The slide glass for medical detection prepared by the preparation method has excellent comprehensive performance, good hydrophilicity, good anti-falling effect and excellent mechanical property.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, a basic catalyst and a polymerization inhibitor into a flask filled with a high-boiling-point solvent, heating to 210 ℃ at the speed of 2-5 ℃/min, purging with nitrogen or inert gas, carrying out heat preservation reaction for 4-6 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 3-6 times, and finally carrying out rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyether ketone;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and an initiator to form a mixed material, and then adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate;
step S3, surface modification: and (3) soaking the glass slide substrate prepared in the step (S2) in an aqueous solution of nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen-trimethyl ammonium chloride with the mass percentage concentration of 10-20% at 50-60 ℃ for 12-20 hours, taking out, washing with water for 3-7 times, drying in a vacuum drying oven at 90-100 ℃ to constant weight, and sterilizing at high temperature to obtain the glass slide for medical detection.
Preferably, the mass ratio of the hyperbranched polyetherketone containing reactive fluorine atoms, the 2- (allyloxy) phenol, the basic catalyst, the polymerization inhibitor and the high-boiling-point solvent in the step S1 is (2-3) to 1, (0.8-1.5) to (0.2-0.3) to (15-25).
Preferably, the basic catalyst is at least one of potassium carbonate, sodium carbonate and cesium carbonate; the polymerization inhibitor is at least one of chloranil and 1, 4-naphthoquinone; the inert gas is any one of helium, neon and argon; the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
Preferably, the preparation method of the hyperbranched polyetherketone containing reactive fluorine atoms is as follows: chinese invention patent example 3 with application number 00104981. X.
Preferably, the mass ratio of the vinyl-terminated hyperbranched polyetherketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the initiator in the step S2 is (3-5):1:1, (0.1-0.3):1, (0.05-0.08).
Preferably, the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
Preferably, the temperature of the high-temperature sterilization in the step S3 is 120-150 ℃.
Another object of the present invention is to provide a slide for medical examination prepared according to the method for preparing a slide for medical examination.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
(1) the preparation method of the glass slide for medical detection provided by the invention is simple and feasible, high in preparation efficiency, low in preparation cost and suitable for industrial production.
(2) The glass slide for medical detection provided by the invention overcomes the defects that the glass slide in the prior art is very thin and brittle in performance and easy to break, so that care must be taken in the manufacturing and using processes, the glass slide can be broken by careless attention, the specimens are damaged, and particularly, the precious specimens are difficult to recover, so that the loss which is difficult to compensate is caused. On the other hand, for some specific precision instruments, ordinary hydrophobic slides cannot be used. For example, the Roche full-automatic immunohistochemical instrument has the defects of uneven tissue staining and test failure due to the fact that the Roche full-automatic immunohistochemical instrument contains the liquid sealing cover film which is easy to adhere to the hydrophobic glass slide, and has the advantages of being excellent in comprehensive performance, good in hydrophilicity, good in anti-falling effect and excellent in mechanical property.
(3) According to the glass slide for medical detection, vinyl-terminated hyperbranched polyether ketone, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid and acrylonitrile which contain vinyl monomers are subjected to radical copolymerization reaction under the action of an initiator to form a three-dimensional network structure, so that the mechanical property, heat resistance and weather resistance of the glass slide are effectively improved, and the monomers have synergistic effect, so that the prepared glass slide is good in transparency, and the (4E) -2, 6-diamino-4-hexenoic acid contains hydrophilic amino and carboxyl, so that the wettability and adhesive force of the glass slide can be improved, and meanwhile, reaction sites are provided for subsequent surface modification.
(4) According to the glass slide for medical detection, the epoxy-beta-cyclodextrin is added, the epoxy group on the epoxy-beta-cyclodextrin reacts with the amino group on the (4E) -2, 6-diamino-4-hexenoic acid chemically, the hydrophilic hydroxyl group is introduced, so that all components are connected by chemical bonds, the performance stability of the glass slide is effectively improved, and the introduced cyclodextrin enables the glass slide to have good biocompatibility and is beneficial to improving the accuracy of medical detection.
(5) According to the glass slide for medical detection, the prepared glass slide substrate is subjected to surface modification by the nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen and nitrogen-trimethyl ammonium chloride, and the surface modification and the carboxyl on the (4E) -2, 6-diamino-4-hexenoic acid are subjected to ion exchange reaction, so that the glass slide substrate is modified on the surface of the glass slide in the form of ionic bonds, and the trimethoxysilylpropyl group is exposed on the surface of the glass slide, so that the anti-falling performance can be further improved, the accuracy of medical detection is improved, and meanwhile, the glass slide substrate can be recovered through hydrolysis reaction, and therefore, the glass slide can be recycled, and the economic value is higher.
Detailed Description
In order to make the technical solutions of the present invention better understood and make the above features, objects, and advantages of the present invention more comprehensible, the present invention is further described with reference to the following examples. The examples are intended to illustrate the invention only and are not intended to limit the scope of the invention.
In the embodiment of the invention, the raw materials are all purchased commercially; the preparation method of the hyperbranched polyetherketone containing reactive fluorine atoms is shown in the following: chinese invention patent example 3 with application number 00104981. X.
Example 1
A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyetherketone containing reactive fluorine atoms, 2- (allyloxy) phenol, potassium carbonate and tetrachlorobenzoquinone into a flask filled with dimethyl sulfoxide, heating to 170 ℃ at the speed of 2 ℃/min, purging with nitrogen, preserving heat for reaction for 4 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 3 times, and finally performing rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyetherketone; the mass ratio of the hyperbranched polyether ketone containing reactive fluorine atoms to the 2- (allyloxy) phenol to the potassium carbonate to the tetrachlorobenzoquinone to the dimethyl sulfoxide is 2:1:0.8:0.2: 15;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and azobisisobutyronitrile to form a mixed material, and adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate; the mass ratio of the vinyl-terminated hyperbranched polyether ketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the azobisisobutyronitrile is 3:1:1:0.1:1: 0.05;
step S3, surface modification: soaking the glass slide substrate prepared in the step S2 in an aqueous solution of nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen-trimethyl ammonium chloride with the mass percentage concentration of 10% at 50 ℃ for 12 hours, then taking out, washing with water for 3 times, then placing in a vacuum drying oven for drying at 90 ℃ to constant weight, and then sterilizing at high temperature to obtain a glass slide for medical detection; the temperature of the high-temperature sterilization is 120 ℃.
A slide for medical examination prepared according to the method for preparing a slide for medical examination.
Example 2
A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyetherketone containing reactive fluorine atoms, 2- (allyloxy) phenol, sodium carbonate and 1, 4-naphthoquinone into a flask filled with N, N-dimethylformamide, heating to 180 ℃ at the speed of 3 ℃/min, purging with helium, preserving heat, reacting for 4.5 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 4 times, and finally performing rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyetherketone; the mass ratio of the hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, sodium carbonate, 1, 4-naphthoquinone and N, N-dimethylformamide is 2.3:1:0.9:0.22: 17;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and azodiisoheptanonitrile to form a mixed material, and adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate; the mass ratio of the vinyl-terminated hyperbranched polyether ketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the azobisisoheptonitrile is 3.5:1:1:0.15:1: 0.06;
step S3, surface modification: soaking the glass slide substrate prepared in the step S2 in an aqueous solution of nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen-trimethyl ammonium chloride with the mass percentage concentration of 13% at 53 ℃ for 14 hours, taking out, washing with water for 4 times, drying in a vacuum drying oven at 92 ℃ to constant weight, and sterilizing at high temperature to obtain a glass slide for medical detection; the temperature of the high-temperature sterilization is 130 ℃.
A slide for medical examination prepared according to the method for preparing a slide for medical examination.
Example 3
A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyetherketone containing reactive fluorine atoms, 2- (allyloxy) phenol, cesium carbonate and tetrachlorobenzoquinone into a flask containing N, N-dimethylacetamide, heating to 190 ℃ at the speed of 3.5 ℃/min, purging with neon, carrying out heat preservation reaction for 5 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 5 times, and finally carrying out rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyetherketone; the mass ratio of the hyperbranched polyether ketone containing reactive fluorine atoms to the 2- (allyloxy) phenol to the cesium carbonate to the tetrachlorobenzoquinone to the N, N-dimethylacetamide is 2.5:1:1.2:0.25: 20;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and azodiisoheptanonitrile to form a mixed material, and adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate; the mass ratio of the vinyl-terminated hyperbranched polyether ketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the azobisisoheptonitrile is 4:1:1:0.2:1: 0.065;
step S3, surface modification: soaking the glass slide substrate prepared in the step S2 in an aqueous solution of nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen-trimethyl ammonium chloride with the mass percentage concentration of 15% at 55 ℃ for 16 hours, then taking out, washing with water for 5 times, then placing in a vacuum drying oven for drying at 95 ℃ to constant weight, and then sterilizing at high temperature to obtain a glass slide for medical detection; the temperature of the high-temperature sterilization is 135 ℃.
A slide for medical examination prepared according to the method for preparing a slide for medical examination.
Example 4
A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, a basic catalyst and a polymerization inhibitor into a flask filled with a high-boiling-point solvent, heating to 200 ℃ at the speed of 4.5 ℃/min, purging with argon, carrying out heat preservation reaction for 5.5 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 6 times, and finally carrying out rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyether ketone; the mass ratio of the hyperbranched polyether ketone containing reactive fluorine atoms to the 2- (allyloxy) phenol to the basic catalyst to the polymerization inhibitor to the high-boiling-point solvent is 2.8:1:1.4:0.28: 23; the alkaline catalyst is formed by mixing potassium carbonate, sodium carbonate and cesium carbonate according to the mass ratio of 1:3: 2; the polymerization inhibitor is formed by mixing tetrachlorobenzoquinone and 1, 4-naphthoquinone according to the mass ratio of 3: 5; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:1:3: 2;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and an initiator to form a mixed material, and then adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate; the mass ratio of the vinyl-terminated hyperbranched polyether ketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the initiator is 4.5:1:1:0.25:1: 0.075; the initiator is formed by mixing azodiisobutyronitrile and azodiisoheptonitrile according to the mass ratio of 3: 5;
step S3, surface modification: soaking the glass slide substrate prepared in the step S2 in an aqueous solution of 18 mass percent of N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride at 50-60 ℃ for 19 hours, then taking out, washing with water for 6 times, then placing in a vacuum drying oven at 98 ℃ for drying to constant weight, and then sterilizing at high temperature to obtain a glass slide for medical detection; the temperature of the high-temperature sterilization is 140 ℃.
A slide for medical examination prepared according to the method for preparing a slide for medical examination.
Example 5
A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, potassium carbonate and 1, 4-naphthoquinone into a flask containing N-methylpyrrolidone, heating to 210 ℃ at the speed of 5 ℃/min, purging with nitrogen at the same time, carrying out heat preservation reaction for 6 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 6 times, and finally carrying out rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyether ketone; the mass ratio of the hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, potassium carbonate, 1, 4-naphthoquinone and N-methylpyrrolidone is 3:1:1.5:0.3: 25;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and azobisisobutyronitrile to form a mixed material, and adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate; the mass ratio of the vinyl-terminated hyperbranched polyether ketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the azobisisobutyronitrile is 5:1:1:0.3:1: 0.08;
step S3, surface modification: soaking the glass slide substrate prepared in the step S2 in an aqueous solution of 20 mass percent of N-trimethoxysilylpropyl-N, N-trimethyl ammonium chloride at 60 ℃ for 20 hours, taking out, washing with water for 7 times, drying in a vacuum drying oven at 100 ℃ to constant weight, and sterilizing at high temperature to obtain a glass slide for medical detection; the temperature of the high-temperature sterilization is 150 ℃.
A slide for medical examination prepared according to the method for preparing a slide for medical examination.
Comparative example 1
This example provides a slide for medical testing, which is formulated and prepared as in example 1, except that (4E) -2, 6-diamino-4-hexenoic acid is not added.
Comparative example 2
This example provides a slide for medical testing, which was formulated and prepared as in example 1, except that no epoxy- β -cyclodextrin was added.
Comparative example 3
This example provides a glass slide for medical examination, which is prepared according to the same formulation and preparation method as example 1, except that no vinyl-terminated hyperbranched polyetherketone is added.
The performance test was performed on the slides for medical examination obtained in examples 1 to 5 and comparative examples 1 to 3 described above, and the test methods and test results are shown in Table 1.
TABLE 1
Item Contact angle Tensile Properties Biocompatibility
Unit of Degree of rotation MPa
Test standard ISO15989-2004 GB/T14344-2003 GB/T16886
Example 1 61 83 Without rejection
Example 2 59 86 Without rejection
Example 3 58 90 Without rejection
Example 4 56 92 Without rejection
Example 5 55 95 Without rejection
Comparative example 1 73 71 Without rejection
Comparative example 2 70 70 Without rejection
Comparative example 3 60 67 Without rejection
As can be seen from table 1, the glass slide for medical examination disclosed in the examples of the present invention has better hydrophilicity and biocompatibility and more excellent mechanical properties than the comparative examples.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (10)

1. A method of preparing a slide for medical testing, comprising the steps of:
step S1, preparation of vinyl-terminated hyperbranched polyether ketone: adding hyperbranched polyether ketone containing reactive fluorine atoms, 2- (allyloxy) phenol, a basic catalyst and a polymerization inhibitor into a flask filled with a high-boiling-point solvent, heating to 210 ℃ at the speed of 2-5 ℃/min, purging with nitrogen or inert gas, carrying out heat preservation reaction for 4-6 hours, cooling to room temperature after the reaction is finished, precipitating a reaction product in water, filtering to obtain a precipitate, washing the product with diethyl ether for 3-6 times, and finally carrying out rotary evaporation to remove the diethyl ether to obtain vinyl-terminated hyperbranched polyether ketone;
step S2, slide molding: uniformly mixing the vinyl-terminated hyperbranched polyether ketone prepared in the step S1, methyl methacrylate, (4E) -2, 6-diamino-4-hexenoic acid, epoxy-beta-cyclodextrin, acrylonitrile and an initiator to form a mixed material, and then adding the mixed material into a double-screw extruder for melt extrusion molding to obtain a glass slide substrate;
step S3, surface modification: and (3) soaking the glass slide substrate prepared in the step (S2) in an aqueous solution of nitrogen-trimethoxysilylpropyl-nitrogen, nitrogen-trimethyl ammonium chloride with the mass percentage concentration of 10-20% at 50-60 ℃ for 12-20 hours, taking out, washing with water for 3-7 times, drying in a vacuum drying oven at 90-100 ℃ to constant weight, and sterilizing at high temperature to obtain the glass slide for medical detection.
2. The method of claim 1, wherein the mass ratio of the hyperbranched polyetherketone containing reactive fluorine atoms, the 2- (allyloxy) phenol, the basic catalyst, the polymerization inhibitor, and the high-boiling solvent in step S1 is (2-3) to 1 (0.8-1.5) to (0.2-0.3) to (15-25).
3. The method for preparing a glass slide for medical examination, according to claim 1, wherein the basic catalyst is at least one of potassium carbonate, sodium carbonate and cesium carbonate.
4. The method as claimed in claim 1, wherein the polymerization inhibitor is at least one of chloranil and 1, 4-naphthoquinone.
5. The method for preparing a slide glass for medical examination according to claim 1, wherein the inert gas is any one of helium, neon and argon.
6. The method of claim 1, wherein the high boiling point solvent is at least one of dimethylsulfoxide, N-dimethylformamide, N-dimethylacetamide, and N-methylpyrrolidone.
7. The method for preparing a glass slide for medical detection according to claim 1, wherein the mass ratio of the vinyl-terminated hyperbranched polyetherketone, the methyl methacrylate, the (4E) -2, 6-diamino-4-hexenoic acid, the epoxy-beta-cyclodextrin, the acrylonitrile and the initiator in step S2 is (3-5):1:1, (0.1-0.3):1, (0.05-0.08).
8. The method of claim 1, wherein the initiator is at least one of azobisisobutyronitrile and azobisisoheptonitrile.
9. The method as claimed in claim 1, wherein the temperature of the high temperature sterilization in step S3 is 120-150 ℃.
10. A slide for medical examination prepared by the method for preparing a slide for medical examination according to any one of claims 1 to 9.
CN202010494349.0A 2020-06-03 2020-06-03 Glass slide for medical detection and preparation method thereof Withdrawn CN111621053A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010494349.0A CN111621053A (en) 2020-06-03 2020-06-03 Glass slide for medical detection and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010494349.0A CN111621053A (en) 2020-06-03 2020-06-03 Glass slide for medical detection and preparation method thereof

Publications (1)

Publication Number Publication Date
CN111621053A true CN111621053A (en) 2020-09-04

Family

ID=72257324

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010494349.0A Withdrawn CN111621053A (en) 2020-06-03 2020-06-03 Glass slide for medical detection and preparation method thereof

Country Status (1)

Country Link
CN (1) CN111621053A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111318239A (en) * 2020-02-26 2020-06-23 上海应用技术大学 Essence nanocapsule based on epoxy- β -cyclodextrin and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111318239A (en) * 2020-02-26 2020-06-23 上海应用技术大学 Essence nanocapsule based on epoxy- β -cyclodextrin and preparation method thereof
CN111318239B (en) * 2020-02-26 2022-06-10 上海应用技术大学 Essence nanocapsule based on epoxy-beta-cyclodextrin and preparation method thereof

Similar Documents

Publication Publication Date Title
CN113698653B (en) Hydrophilic coating based on acrylic polymerization and photocuring and preparation method thereof
CN111621053A (en) Glass slide for medical detection and preparation method thereof
CN108467451B (en) Preparation method of hydrophilic polyvinylidene fluoride resin
CN112175244B (en) Cellulose acetate nanocomposite with ultraviolet shielding and antibacterial properties and preparation method thereof
CN111393031B (en) Etching solution for preparing filter glass and preparation method of filter glass
CN109364296B (en) Surface-modified polyaryl ether bone implant material containing phthalazinone structure and preparation method thereof
CN108097072A (en) A kind of hydrophilic modifying CPVA-PVDF ultrafiltration membranes and preparation method thereof
CN108484814B (en) Hydrophilic polyvinylidene fluoride resin
CN107063812A (en) A kind of low flake rate of liquid-based culture hydrophily adheres to the preparation method of slide
CN112945671A (en) Adhesive glass slide and preparation method and application thereof
WO2024087828A1 (en) Pet film for cell culture in cell and gene therapy, and use thereof
KR20180131131A (en) A method for the detection of saccharides from hydrogel polymer
CN114409972A (en) Sodium alginate composite material with ammonia response and antibacterial functions and preparation method thereof
CN108641634B (en) Adhesive composition for slide glass coating and single-side coating process
CN113321770B (en) Preparation method of temperature-sensitive hydrogel
CN109612808B (en) Hydrophilic glass slide for medical detection
CN112480750A (en) Super-hydrophilic coating for cell culture and preparation method thereof
CN105219836B (en) A kind of microarray modifies substrate with active aldehyde radical
CN111253850A (en) Medical hydrophilic coating composition and preparation method and application thereof
CN101583655A (en) Method for production of molded resin article
CN112961381B (en) Polyether ketone film and preparation method and application thereof
CN115353703B (en) Outdoor anti-aging acrylic plate and preparation process thereof
CN113150334B (en) Preparation process of nitrocellulose membrane
CN114958198B (en) Polymer casting solution, anti-fog coating, and preparation methods and applications thereof
CN115353835A (en) Preparation method and application of adhesive

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20200904

WW01 Invention patent application withdrawn after publication