CN107652689A - A kind of sensing membrane, preparation method and applications - Google Patents
A kind of sensing membrane, preparation method and applications Download PDFInfo
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- CN107652689A CN107652689A CN201710964613.0A CN201710964613A CN107652689A CN 107652689 A CN107652689 A CN 107652689A CN 201710964613 A CN201710964613 A CN 201710964613A CN 107652689 A CN107652689 A CN 107652689A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6486—Measuring fluorescence of biological material, e.g. DNA, RNA, cells
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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Abstract
The invention discloses a kind of sensing membrane, by being mixed with the base resin of pH indicator with being formed after hydrogen-containing siloxane crosslinking curing, the base resin is branched vinylsiloxane, and the mol ratio of pH indicator and base resin is 1:4×103~8 × 103.Indicator, can be embedded in inside cross-linked polymer, the sensing membrane has porous open architecture, H by sensing membrane of the present invention as obtained by the base resin and hydrogen-containing siloxane that are mixed with indicator are carried out into crosslinking curing+、OH‑Or CO2It can be reacted by the intermolecular space of silica gel with indicator to develop the color, after indicator embeds with silica gel copolymerization, the stability of indicator can be significantly improved, room temperature need not be kept in dark place sensing membrane developing sensitivity plan in 2 years and not change, and avoid the generation of false positive and false negative.
Description
Technical field
The present invention relates to blood culture detection field, and in particular to a kind of sensing membrane, preparation method and applications.
Background technology
The blood of Healthy People is sterile, and when pathogenic infection microorganism enters in blood, breeding is thin beyond mononuclear phagocyte rapidly
When born of the same parents' system removes the ability of these microorganisms, that is, lasting bacteremia is produced, and extravascular tissue can be infected, the micro- life of cause of disease
Thing is directly entered blood flow outside blood vessel through lymphatic vessel, and intravascular infection can occur for patient, and (such as infectious endocarditis, fungoid is moved
Arteries and veins knurl, suppurative phlebitis, infectious fistula of artery and sucquet's canal are scorching), form bacteremia or Fungemia.Bacteremia is to face
One of common critical illness of bed, case fatality rate is up to 20%-50%.Microorganism is detected in the blood of patient to examine infectious diseases
Disconnected, treatment and prognosis have important clinical meaning.Blood culture is to diagnose the mostly important means of bacteremia, separates autoblood
Bacterium the reason for being probably septicemia, this just makes a definite diagnosis for the cause of disease and provides important foundation, and may further be correct antibiosis
Extract for treating provides foundation.
The principle of automatic blood culture inserts a kind of sensing membrane for Blood culture bottle bottom of bottle, and acid, production alkali are produced during bacterial metabolism
Or produce CO2, H+、OH-Or CO2Indicator reaction through pellicle and blake bottle bottom cause color change or
The change (enhancing or quenching) of fluorescence intensity.Disclosed sensing membrane technology is placed in training for indicator physics is fixed on carrier
Bottom of bottle is supported, then in one layer of pellicle of its upper, it is known that many indicator particularly pH indicator (including fluorescence instruction
Agent etc.) it is more sensitive to light and temperature, storage process easily causes properties of product to decline, and causes the production of false positive and false negative
It is raw.Show according to open source information, false positive rate and false negative rate are up to more than 5% in current technology, wherein more than 3% is blood culture
Bottle sensing membrane cause for quality causes, and delays effective treatment of patient.Secondly, the cumbersome indicator distribution of existing disclosed technical operation
It is uneven, and cause one of the insensitive reason that develops the color.
Two kinds of the coloured former method of sensing membrane technology and fluorescence method, chromogen method indicator indicate for conventional chemistry disclosed in existing
Agent, such as bromocresol green, Yihong, methylene blue.Fluorescence method is more using rhodamine, fluoresceins fluorescence probe.These fluorescence
Probe quantum yield is relatively low, and universal all existence and stabilities are poor, and particularly photostability is poor, and it is relatively low very to easily cause positive rate
To in the result into false positive and false negative.
The detection time of the blake bottle of other prior art is long, and the stand-by period is longer, and detector efficiency is not high.
The content of the invention
Present invention aims at a kind of sensing membrane is provided, solves the sensing membrane of prior art in storing process under performance
Drop, the problem of detection time is long.Additionally provide a kind of preparation method and applications of sensing membrane.
The present invention is achieved through the following technical solutions：
A kind of sensing membrane, by being mixed with the base resin of pH indicator with being formed after hydrogen-containing siloxane crosslinking curing, the base
Plinth resin is branched vinylsiloxane, and the mol ratio of pH indicator and base resin is 1:4×103~8 × 103。
The base resin is one kind in following compound：VTES, vinyl trimethoxy silicon
Alkane, vinyl three ('beta '-methoxy ethyoxyl) silane, vinyl three (dimethyl siloxane) silane.
PH indicator is methylene blue, the one or two of bromothymol blue.
PH indicator be such as the fluorine boron pyrroles in formula (I),
Wherein R be it is following in one kind
Hydrogen-containing siloxane is one kind in following：
A kind of foregoing sensing membrane, the application on blood culture detection blake bottle is prepared.
A kind of foregoing preparation method of sensing membrane, the base resin for being mixed with indicator addition hydrogen-containing siloxane is entered
Row crosslinking curing and obtain, wherein base resin is branched vinylsiloxane, the mol ratio of pH indicator and base resin
For 1:4×103~8 × 103。
Also need to be stirred under vacuum deaeration 5min, resolidification after crosslinking.
The concrete operations for being mixed with the base resin of indicator are：Grinding or high speed shear mix.
A kind of preparation method of blood culture detection blake bottle, after the base resin for being mixed with indicator is adjusted into pH to 7.2~7.4
Add hydrogen-containing siloxane and carry out cross-linking reaction, be stirred under vacuum deaeration 5-10min, dispense to blake bottle, cold curing, wherein basis
Resin is branched vinylsiloxane, and the mol ratio of pH indicator and base resin is 1:4×103~8 × 103。
The present invention compared with prior art, has the following advantages and advantages：
1st, sensing of the present invention as obtained by the base resin and hydrogen-containing siloxane that are mixed with indicator are carried out into crosslinking curing
Film, indicator can be embedded in inside cross-linked polymer, the sensing membrane has porous open architecture, H+、OH-Or CO2Energy
Enough reacted by the intermolecular space of silica gel with indicator to develop the color, can be notable after indicator embeds with silica gel copolymerization
The stability of indicator is improved, room temperature need not be kept in dark place sensing membrane developing sensitivity plan in 2 years and not change, avoid
The generation of false positive and false negative.
2nd, the detection time of sensing membrane prepared by the present invention is significantly better than import and domestic famous brand name, and stability
Get well and false positive and false negative can be avoided.
Brief description of the drawings
Accompanying drawing described herein is used for providing further understanding the embodiment of the present invention, forms one of the application
Point, do not form the restriction to the embodiment of the present invention.In the accompanying drawings：
Accompanying drawing 1 is the detection time comparison diagram of the positive group 1 of chromogen method；
Accompanying drawing 2 is the detection time comparison diagram of the positive group 2 of chromogen method；
Accompanying drawing 3 is the detection time comparison diagram of the positive group 1 of fluorescence method；
Accompanying drawing 4 is the detection time comparison diagram of the positive group 2 of fluorescence method.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment and accompanying drawing, to this
Invention is described in further detail, and exemplary embodiment of the invention and its explanation are only used for explaining the present invention, do not make
For limitation of the invention.
Embodiment 1
0.5mmol bromine musk deer grass phenol indigo plant, 0.5mmol methylene blues and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added
In 4mol VTESs, grinding or high speed shear mix, add appropriate sodium hydroxide adjustment PH be 7.2~
7.4, then add 1molDeaeration 5Min is stirred under vacuum, i.e.,
Sensing membrane is obtained, if need to cultivate to blake bottle, continues packing to blake bottle, cold curing.
Embodiment 2
0.5mmol fluorine boron pyrroles and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added into 4mol vinyl trimethoxy silicon
In alkane, grinding or high speed shear mix, and it is 7.2~7.4 to add appropriate sodium hydroxide adjustment PH, then adds 1mol crosslinkings
AgentDeaeration 5Min is stirred under vacuum, is dispensed to blake bottle, room temperature
Solidification.
R substituent wherein in fluorine boron pyrroles is
Embodiment 3
0.5mmol fluorine boron pyrroles and 0.1mL1% isopropyl alcohol solution of chloroplatinic acid are added into (the 'beta '-methoxy of 4mol vinyl three
Ethyoxyl) in silane, grinding or high speed shear mix, and it is 7.2~7.4, Ran Houjia to add appropriate sodium hydroxide adjustment PH
Enter 1molDeaeration 5Min is stirred under vacuum, is dispensed to blake bottle,
R substituent in cold curing, wherein fluorine boron pyrroles is
Embodiment 4
0.5mmol fluorine boron pyrroles and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added into (the dimethyl-silicon of 4mol vinyl three
Oxyalkyl) in silane, grinding or high speed shear mix, and it is 7.2~7.4, Ran Houjia to add appropriate sodium hydroxide adjustment PH
Enter 1molDeaeration 5Min is stirred under vacuum, is dispensed to blake bottle,
R substituent in cold curing, wherein fluorine boron pyrroles is
Embodiment 5
0.5mmol fluorine boron pyrroles and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added into 4mol vinyl trimethoxy silicon
In alkane, grinding or high speed shear mix, and it is 7.2~7.4 to add appropriate sodium hydroxide adjustment PH, then adds 1mol
Deaeration 5Min is stirred under vacuum, dispenses to blake bottle, cold curing and is
Can.
R substituent wherein in fluorine boron pyrroles is
Embodiment 6
0.5mmol fluorine boron pyrroles and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added into 6mol vinyl trimethoxy silicon
In alkane, grinding or high speed shear mix, and it is 7.2~7.4 to add appropriate sodium hydroxide adjustment PH, then adds 1mol
Deaeration 5Min is stirred under vacuum, dispenses to blake bottle, cold curing and is
Can.R substituent wherein in fluorine boron pyrroles is
Embodiment 7
0.5mmol fluorine boron pyrroles in claim and the isopropyl alcohol solution of chloroplatinic acid of 0.1mL 1% are added into 8mol ethene
In base trimethoxy silane, grinding or high speed shear mix, and it is 7.2~7.4 to add appropriate sodium hydroxide adjustment PH, then
Add 1molDeaeration 5Min is stirred under vacuum, dispenses to blake bottle, cold curing and is
Can.
R substituent wherein in fluorine boron pyrroles is
For further illustrate beneficial effects of the present invention, inventor carried out sensing membrane blood culture detect to having a competition
Test.Content of the test and result are as follows：
The chromogen method Blood culture bottle (numbering is R1 i.e. embodiment 1) and certain import product for using present invention sensing membrane technology to prepare
Board chromogen method Blood culture bottle (numbering M) and certain domestic brand chromogen method Blood culture bottle (numbering D) are in Bact/ALERT 3D
Contrast examination is carried out on 120 Full-automatic blood culture instruments, use the present invention sensing membrane technology prepare fluorescence method Blood culture bottle (numbering for
R2 is embodiment 2) (compiled with certain import brand fluorescence method Blood culture bottle (numbering B) and certain domestic brand fluorescence method Blood culture bottle
Number it is H) contrast test is carried out on the Full-automatic blood culture instruments of BACET 9120, specific method is each to prepare every kind of Blood culture bottle
300 bottles, and by every kind of Blood culture bottle be divided into negative group, positive group 1, positive 2 three groups, every group 100 bottles of group.Negative control group is inoculated with
Sterile blood plasma 10mL, blood plasma 10mL of the inoculation containing ETEC (ATCC25922) 10-100cfu of positive group 1, positive group 2
Blood plasma 10mL of the inoculation containing staphylococcus aureus (ATCC25923) 10-100cfu, cultivates 96h statistical results.If report sun, is needed
It is seeded to blood plate and confirms have bacteria growing to be designated as the positive, is otherwise designated as false positive.96h does not report sun to take out observation without obvious yet
Discoloration or muddiness are calculated as feminine gender, if obvious discoloration or muddiness are seeded to blood plate and confirm have bacterium to be designated as false negative.Result of the test is such as
Following table and Fig. 1-4：
Table 1
From experimental result：Table 1 and Fig. 1-4 are as can be seen that the detection time of the sensing membrane prepared using the method is significantly better than
Import and domestic famous brand name, and stability is good and can avoid false positive and false negative.
Above-described embodiment, the purpose of the present invention, technical scheme and beneficial effect are carried out further
Describe in detail, should be understood that the embodiment that the foregoing is only the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution and improvements done etc., all should include
Within protection scope of the present invention.
Claims (10)
1. a kind of sensing membrane, it is characterised in that by being mixed with the base resin of pH indicator and shape after hydrogen-containing siloxane crosslinking curing
It is branched vinylsiloxane into, the base resin, the mol ratio of pH indicator and base resin is 1:4×103~8
×103。
2. a kind of sensing membrane according to claim 1, it is characterised in that the base resin is one in following compound
Kind：VTES, vinyltrimethoxy silane, vinyl three ('beta '-methoxy ethyoxyl) silane, molecular formula,
Vinyl three (dimethyl siloxane) silane.
3. a kind of sensing membrane according to claim 1, it is characterised in that pH indicator is methylene blue, bromine thymol
Blue one or two.
A kind of 4. sensing membrane according to claim 1, it is characterised in that pH indicator be such as the fluorine boron pyrroles in formula (I),
Wherein R be it is following in one kind
5. a kind of sensing membrane according to claim 1, it is characterised in that hydrogen-containing siloxane is one kind in following：
6. a kind of sensing membrane as described in claim any one of 1-5, the application on blood culture detection blake bottle is prepared.
7. the preparation method of a kind of sensing membrane as described in claim any one of 1-5, it is characterised in that indicator will be mixed with
Base resin adds hydrogen-containing siloxane and carries out crosslinking curing and obtain, and wherein base resin is branched vinylsiloxane, pH
The mol ratio of indicator and base resin is 1:4×103~8 × 103。
8. preparation method according to claim 7, it is characterised in that also need to be stirred under vacuum deaeration 5min after crosslinking, then
Solidification.
9. preparation method according to claim 7, it is characterised in that be mixed with the concrete operations of the base resin of indicator
For：Grinding or high speed shear mix.
10. a kind of preparation method of blood culture detection blake bottle, it is characterised in that the base resin for being mixed with indicator is adjusted into pH extremely
Hydrogen-containing siloxane is added after 7.2~7.4 and carries out cross-linking reaction, deaeration 5-10min is stirred under vacuum, dispenses solid to blake bottle, room temperature
Change, wherein base resin be branched vinylsiloxane, and the mol ratio of pH indicator and base resin is 1:4×103~8
×103。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710964613.0A CN107652689A (en) | 2017-10-17 | 2017-10-17 | A kind of sensing membrane, preparation method and applications |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019163290A1 (en) * | 2018-02-22 | 2019-08-29 | 信越化学工業株式会社 | Room-temperature-curable organopolysiloxane composition, structure, and method for assessing cured state of said composition |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019163290A1 (en) * | 2018-02-22 | 2019-08-29 | 信越化学工業株式会社 | Room-temperature-curable organopolysiloxane composition, structure, and method for assessing cured state of said composition |
| JPWO2019163290A1 (en) * | 2018-02-22 | 2021-02-04 | 信越化学工業株式会社 | Room temperature curable organopolysiloxane composition and structure, and method for determining the cured state of the composition |
| US11518884B2 (en) | 2018-02-22 | 2022-12-06 | Shin-Etsu Chemical Co., Ltd. | Room-temperature-curable organopolysiloxane composition, structure, and method for assessing cured state of said composition |
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