CN106479484A - A kind of composite preparation process of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure - Google Patents
A kind of composite preparation process of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure Download PDFInfo
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- 239000013543 active substance Substances 0.000 claims description 4
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Abstract
A kind of composite preparation process of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure；It includes：The nucleocapsid structure that the infrared up conversion nano material of blue light-emitting is formed with the magnetic bead with immune performance；Above-mentioned material surface is modified process respectively；Nuclear structure with infrared up conversion nano material as composite, the shell structurre with immunomagnetic beadses as composite, there is the immune magnetic Nano up-conversion luminescent material of nucleocapsid structure by the synthesis of chemical hydro-thermal reaction.
Description
Technical field
The invention belongs to luminescent material applied technical field.
Background technology
Upconverting fluorescent material has obtained a certain degree of application as label in biological field, its uniqueness upper turn
Change light characteristic so that Measurement for Biotechnique have good stability, sensitivity high, easy and simple to handle quick, can qualitative, quantitative etc. excellent
Point.But this traditional direct excitation-emission pattern so that detection process must rely on the means such as solid phase material realize not with inspection
Survey being completely separated of the free label that thing combines, otherwise the free label of any residual all can become coming of false positive signal
Source.Patent 200410034105.5,200410034104.0, upconverting fluorescent material in 200420049580.5 pairs of biological fields
Application process is sufficiently introduced.
Immunomagnetic beadses (Immunomagneticbeads, IMB), are being combined into by carrier microballoons and immunoligand
Plant nanometer materials.Immuno magnetic cell separation technology is with the magnetic microsphere of high homogeneity as solid support, by immunoligand (such as
Antibody, antigen etc.) formation immune magnetic microsphere on magnetic carrier is attached to by functional group, anti-using specific immunology
Should, under magneticaction, occur mechanics to move, isolate specific target substance from mixed solution.There is separating rate fast,
Efficiency high, favorable repeatability, simple to operate it is not necessary to the instrument and equipment of costliness.
A kind of immune magnetic Nano up-conversion luminescent material with nucleocapsid structure of the present invention, is a kind of the red of blue light-emitting
Outer up-conversion nano material and the composite construction of the magnetic bead material with immune performance, excite blue of generation by near-infrared laser
Light.Add the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure in the solution of measuring samples, immunoligand is (such as
Antibody, antigen etc.) formation immune magnetic microsphere on magnetic carrier is attached to by functional group, anti-using specific immunology
Should, under magneticaction, occur mechanics to move, separation detection target substance from mixed solution, and pass through Infrared fluorescence quantum dot
Add, realize detection self identity, reverse verification.Any lock out operation that in actual applications need not be follow-up, only needing will be to be checked
Sample mixes i.e. achievable simple and efficient qualitative and quantitative detection with composite.Meanwhile, during the course of the reaction can be at any time to can
See that light is detected, to monitor speed and the degree that biological respinse is carried out, meet the different demands of applied research and basic research.
Content of the invention
A kind of composite preparation process of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure；It includes：Send out
The nucleocapsid structure that the infrared up conversion nano material of blue light is formed with the magnetic bead with immune performance；Above-mentioned material surface makes respectively
Different groups can be formed in particle surface with sol-gel process moditied processing, be conducive to the immunoligand that covalent bond is different
Active substances such as (as enzyme, cell, antibody, antigen, DNA, RNA)；Core with infrared up conversion nano material as composite
Structure, the shell structurre with immunomagnetic beadses as composite, the upper conversion nano of 15%-30% is configured with deionized water for dispersion liquid
The solution of material, is subsequently adding the immunomagnetic beadses of 1%-15%, passes through chemical hydro-thermal reaction synthesis at ambient temperature and has nucleocapsid
The immune magnetic Nano up-conversion luminescent material of structure, for biological detection.
The infrared up conversion method of manufacturing fluorescent material of the blue light-emitting in the present invention is, the fluoride material containing Y, Gd, La
One of material or more than one mixture are host material, add the YbF of 45-50% weight ratio in host material3, simultaneously
12-25% weight is added to compare TmF in host material3, after uniformly mixing, in argon, sinter 1-6 hour, system in 300-450 degree
Standby go out to have the infrared up conversion fluorescence granular material of blue-light-emitting, it can produce 440-480nm blue in 980nm laser excitation
Luminous, granularity is in 70-800nm.In preparation process, argon can effectively stop material oxidized, improves luminous efficiency and control
Excitation；Low temperature can suppress the growth of granule.With 3- aminopropyl trimethoxysilane for surface silanization material, with penta 2
Aldehyde is surface aldehydes material, uses sol-gel process moditied processing in infrared up conversion nano-material surface, makes material surface
After silanization and aldehyde radicalization are processed, its surface is suitable for connecting different bioactive substances, is conducive to linking in particle surface
Other different groups are conducive to immunomagnetic beadses granule in the absorption on surface.
The magnetic bead material preparation method with immune performance in the present invention is：With thioglycolic as stabilizer, configuration is dense
Spend stabilizing solution for 15% and then 600Constant temperature stirring under C, by Fe2+With Fe3+By 2：3 mol ratio adds in stabilizing solution, then
Adding NaOH solution to adjust reaction system is alkalescence, and constant temperature stirring reaction 1 hour prepares the ferriferrous oxide nano magnetic of black
Granule.With Oleic acid for surface carboxyl groups raw material, with potassium permanganate catalyst, using sol-gel process moditied processing, there is immunity
The magnetic bead material surface of performance, can form carboxyl in particle surface after the nanometer magnetic bead surface of synthesis carries out carboxylated process,
Can the active substances such as the different immunoligand of covalent bond (as enzyme, cell, antibody, antigen, DNA, RNA), can be used for biology
Detection.Quantum dot fluorescence material granule is usually 1-10 nanometer, and it can add in magnetic bead material preparatory phase, or in magnetic bead
Material is added with the up-conversion luminescent material shelling stage and mixes.
The nucleocapsid knot that the infrared up conversion nano material of the blue light-emitting in the present invention is formed with the magnetic bead with immune performance
Structure material surface adds vulcanized lead Infrared fluorescence quantum dot, and vulcanized lead Infrared fluorescence quantum dot absorbs visible ray, launches near-infrared
Light, and absorbed by up-conversion nano material.Or by excited by visible light, another wave band is launched from up-conversion luminescent material
Light.Present invention achieves visible ray, infrared light mutually excite conversion so that for more accurate quick during bio-diversity detection
Uniquely, and reach reagent detection self identity, reverse verification is it is possible to by Beads enrichment in mixing.
Specific embodiment
The infrared up conversion method of manufacturing fluorescent material of the blue light-emitting in the present invention is：Fluoride material containing Y, Gd, La
One of material or more than one mixture are host materials, add the YbF of 45-50% weight ratio in host material3, simultaneously
12-25% weight is added to compare TmF3, sinter 1-6 hour in 300-450 degree in argon, prepare the infrared upper of blue-light-emitting and turn
Change fluorescence micro particulate materials, it can send 440-480nm blue-light-emitting, granule is in 70-800nm by 980nm laser excitation.When
Sintering temperature is less than 350 degree, and the time is less than 2 hours, can prepare diameter averagely in 100 nm particles below, and it is luminous strong
Degree is weaker；When sintering temperature is more than 400 degree, the time is more than 4 hours, and material becomes block, can prepare diameter after crushed
The average granule in 700 more than nm, its luminous intensity is stronger；Sintering process should be carried out in argon atmosphere, preparation process
Middle argon can effectively stop material oxidized, improve luminous efficiency and control excitation；Low temperature can suppress the life of granule
Long.
The magnetic bead material preparation method with immune performance in the present invention is：With thioglycolic as stabilizer, configuration is dense
Spend stabilizing solution for 15% and then 600Constant temperature stirring under C, by Fe2+With Fe3+By 2：3 mol ratio adds in stabilizing solution, then
Adding NaOH solution to adjust reaction system is alkalescence, and granularity is prepared in 30nm 50nm in constant temperature stirring reaction 1 hour under room temperature
Black ferriferrous oxide nano magnetic-particle.
Infrared up conversion nano-material surface in the present invention use sol-gel process moditied processing, with ethylene glycol be divide
Powder, be configured to 30% up-conversion nano material dispersion, be subsequently adding the 3- aminopropyl trimethoxysilane of 1%-3%
For surface silanization material, 60 under the protection of nitrogen0Constant temperature stirring reaction 10 hours under C, use anhydrous second after the completion of reaction
Alcohol cleans to neutrality, and the glutaraldehyde being subsequently adding 0.5% 1% is surface aldehydes material, and logical nitrogen protection is stirred at room temperature
Mix reaction 6 hours, then deionized water is washed till neutrality, dries standby at room temperature；Make material surface through silanization and aldehyde
After baseization is processed, its surface is suitable for connecting different bioactive substances, and being conducive to linking other different groups in particle surface has
Beneficial to the absorption on surface for the immunomagnetic beadses granule.
The magnetic bead material surface with immune performance in the present invention uses sol-gel process moditied processing, with deionization
Water is dispersant, is configured to 10% 25% dispersion, and the Oleic acid being subsequently adding 2% 4% is surface carboxyl groups raw material,
700Continuously stirred 1 hour under C, then use washes of absolute alcohol 2 times to clean unnecessary Oleic acid, be finally washed with deionized
To neutral, be eventually adding 0.5% potassium permanganate catalyst, ultrasonic vibration 8 hours in being cleaned by ultrasonic instrument, after the completion of wash 3
Time, then naturally dry at room temperature.Can be formed in particle surface after the nanometer magnetic bead surface of synthesis carries out carboxylated process
Carboxyl, can the active substances such as the different immunoligand of covalent bond (as enzyme, cell, antibody, antigen, DNA, RNA), can use
In biological detection.
Above-mentioned material surface in the present invention can form difference in particle surface using sol-gel process moditied processing respectively
Group, be conducive to the thing active matters such as the different immunoligand of covalent bond (as enzyme, cell, antibody, antigen, DNA, RNA)
Matter；Nuclear structure with infrared up conversion nano material as composite, the shell structurre with immunomagnetic beadses as composite, to go
Ionized water configures the solution of the up-conversion nano material of 15%-30% for dispersion liquid, is subsequently adding the immunomagnetic beadses of 1%-15%, in room
There is the immune magnetic Nano up-conversion luminescent material of nucleocapsid structure by chemical hydro-thermal reaction synthesis, for biology under the conditions of temperature
Detection.
Vulcanized lead Infrared fluorescence quantum dot in the present invention is prepared using hydro-thermal method, granularity 2-10 nanometer, launching light
900-1500 nanometer, absorbing light ultraviolet and visible ray, launch more than light absorbing near infrared light, and by up-conversion nano material
Absorb.Or by excited by visible light, another wave band visible ray is launched by up-conversion luminescent material.Present invention achieves it is visible
Light, infrared light mutually excite conversion so that more accurate quick is unique when detecting for bio-diversity, and reaches reagent detection
Self identity, reverse verification.As excited infrared quantum point material using green glow, it launches 900-1000 nanometer infrared light, and
Absorbed by the infrared up conversion nano material of blue light-emitting, launch blue light, then formation green glow, infrared light, blue light are mutually changed.
Advantage of the present invention
Using specific immunological response, under magneticaction, mechanics is occurred to move, separation detection target from mixed solution
Matter.Simplify the operating process of Site Detection, and the detection time shortening.
Measuring samples only need to mixs with composite and get final product reality by any lock out operation that in actual applications need not be follow-up
Existing simple and efficient qualitative and quantitative detection.Meanwhile, can at any time visible ray be detected during the course of the reaction, biological anti-to monitor
The speed that should carry out and degree.
Produce simple, easily produce in batches, industrialization.
Specific embodiment
Embodiment 1
Prepare the infrared up conversion fluorescent material of blue light-emitting：Take YF390g, GdF310g, adds YbF345g, TmF313g, in argon
In 400 in protection0C sinters 2 hours, and the infrared up conversion fluorescent material prepared, in 980nm laser excitation, can send 450nm
Blue-light-emitting, granule is in 100nm.
Take out above infrared up conversion fluorescent material 30g to add in there-necked flask, be subsequently adding the stirring point of 100ml ethylene glycol
Dissipate uniformly, the 3- aminopropyl trimethoxysilane being subsequently adding 0.5g is surface silanization material, under the protection of nitrogen
600Constant temperature stirring reaction 10 hours under C, with washes of absolute alcohol to neutrality after the completion of reaction, then deionized water is diluted to
100ml, the glutaraldehyde being subsequently adding 0.2g is surface aldehydes material, logical nitrogen protection, and reaction 6 hour is stirred at room temperature,
Then deionized water is washed till neutrality, dries standby at room temperature, obtains the up-conversion nano material of surface aldehydes.
Preparation has the preparation of the magnetic bead of immune performance：Take 15g thioglycolic to be subsequently adding 100ml deionized water, burning
It is configured to stabilizing solution in cup, be then respectively adding the Fe of 0.8mol/L3+The Fe of solution 90ml and 0.8mol/L2+Solution 60ml, stirs
Mix 30min, mix homogeneously；It is eventually adding NaOH solution 300ml of 1mol/L, reaction 1 hour is stirred at room temperature, finally spends
Ionized water cleans to neutrality, obtains the magnetic bead particles of 30nm.
Take prepared magnetic bead particles 15g, be subsequently adding 100ml ionized water and be configured to dispersion solution, be then slowly added into
The Oleic acid of 0.5g, 700Continuously stirred 1 hour under C, then use washes of absolute alcohol 2 times to clean unnecessary Oleic acid, finally use
To neutrality, then deionized water is configured to the solution of 100ml to deionized water wash, is eventually adding the potassium permanganate of 0.1g,
Be cleaned by ultrasonic ultrasonic vibration 8 hours in instrument, ultrasonic after the completion of wash 3 times, then naturally dry at room temperature, obtain surface carboxyl groups
The nanometer magnetic bead granule changed.
Prepare the immune magnetic Nano up-conversion of nucleocapsid structure：Take the upper conversion nano of 30g surface aldehydes first
Material, is subsequently adding 150ml deionized water and is configured to dispersion, be subsequently adding the nanometer magnetic bead of 3.0g surface carboxyl groups
Grain, passes through the immune magnetic Nano up-conversion luminescent material that chemical hydro-thermal reaction synthesis has nucleocapsid structure at ambient temperature.
Then clean to neutrality in deionized water, finally 00C—100Stored refrigerated under C.
Embodiment 2
Prepare the infrared up conversion fluorescent material of blue light-emitting：Take YF3100 grams, add YbF350 grams, TmF320 grams, in argon
In sinter 5 hours in 450 degree, the infrared up conversion fluorescent material prepared grinds and morcels, and under 980nm laser excitation, can produce
Raw 470nm blue-light-emitting, granule is in 800nm.
Take out above infrared up conversion fluorescent material 15g to add in there-necked flask, be subsequently adding the stirring point of 100ml ethylene glycol
Dissipate uniformly, the 3- aminopropyl trimethoxysilane being subsequently adding 0.2g is surface silanization material, under the protection of nitrogen
600Constant temperature stirring reaction 10 hours under C, with washes of absolute alcohol to neutrality after the completion of reaction, then deionized water is diluted to
100ml, the glutaraldehyde being subsequently adding 0.15g is surface aldehydes material, logical nitrogen protection, and reaction 6 hour is stirred at room temperature,
Then deionized water is washed till neutrality, dries standby at room temperature, obtains the up-conversion nano material of surface aldehydes.
Preparation has the preparation of the magnetic bead of immune performance：Take 30g thioglycolic to be subsequently adding 200ml deionized water, burning
It is configured to stabilizing solution in cup, be then respectively adding the Fe of 0.8mol/L3+The Fe of solution 150ml and 0.8mol/L2+Solution 100ml,
Stirring 30min, mix homogeneously；It is eventually adding NaOH solution 500ml of 1mol/L, reaction 2 hour is stirred at room temperature, finally uses
Deionized water cleans to neutrality, obtains the magnetic bead particles of 50nm.
Take prepared magnetic bead particles 30g, be subsequently adding 200ml ionized water and be configured to dispersion solution, be then slowly added into
The Oleic acid of 1.2g, 700Continuously stirred 2 hours under C, then use washes of absolute alcohol 2 times to clean unnecessary Oleic acid, finally use
To neutrality, then deionized water is configured to the solution of 200ml to deionized water wash, is eventually adding the potassium permanganate of 0.3g,
Be cleaned by ultrasonic ultrasonic vibration 10 hours in instrument, ultrasonic after the completion of wash 3 times, then naturally dry at room temperature, obtain surface carboxylic
The nanometer magnetic bead granule of base.
Prepare the immune magnetic Nano up-conversion of nucleocapsid structure：Take the upper conversion nano of 50g surface aldehydes first
Material, is subsequently adding 150ml deionized water and is configured to dispersion, be subsequently adding the nanometer magnetic bead of 6.0g surface carboxyl groups
Grain, passes through the immune magnetic Nano up-conversion luminescent material that chemical hydro-thermal reaction synthesis has nucleocapsid structure at ambient temperature.
Then clean to neutrality in deionized water, finally 00C—100Stored refrigerated under C.
After having made to illustrate above for the preferable embodiment of the present invention, to one skilled in the art should
It is realized that, in the case of without departing from the spirit and scope of the present invention, any changes and improvements made for the present invention all exist
In the scope of the present invention.
Claims (7)
1. a kind of composite preparation process of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure；It includes：Turn blue
The nucleocapsid structure that the infrared up conversion nano material of light is formed with the magnetic bead with immune performance；Above-mentioned material surface is repaiied respectively
Decorations are processed；Nuclear structure with infrared up conversion nano material as composite, the shell structurre with immunomagnetic beadses as composite,
There is the immune magnetic Nano up-conversion luminescent material of nucleocapsid structure by the synthesis of chemical hydro-thermal reaction.
2. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method is it is characterised in that the infrared up conversion preparation method of nano material of described blue light-emitting is：Fluoride containing Y, Gd, La
One of material or more than one mixture are host material, add the YbF of 45-50% weight ratio in host material3, with
When add 12-25% weight ratio TmF3, in 300 in argon0C -4500C sinters 1-6 hour, prepares blue-light-emitting
Infrared up conversion fluorescence granular material, it produces 440-480nm blue-light-emitting, granularity is in 70- in 980nm laser excitation
800nm.
3. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method is it is characterised in that the described magnetic bead material preparation method with immune performance is：With thioglycolic as stabilizer, join
Put the stabilizing solution that concentration is 15%, then 600Constant temperature stirring under C, by Fe2+With Fe3+By 2：3 mol ratio adds in stabilizing solution,
Being subsequently adding NaOH solution and adjusting reaction system is alkalescence, and constant temperature stirring reaction 1 hour prepares the ferriferrous oxide nano of black
Magnetic-particle.
4. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method is it is characterised in that described infrared up conversion nano-material surface uses sol-gel process moditied processing, with 3- aminopropyl
Trimethoxy silane is surface silanization material, with glutaraldehyde for surface aldehydes material, make material surface through silanization and
After aldehyde radicalization is processed, its surface is suitable for connecting different bioactive substances, is conducive to linking other different groups in particle surface
Be conducive to immunomagnetic beadses granule in the absorption on surface.
5. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method is it is characterised in that the described magnetic bead material surface with immune performance uses sol-gel process moditied processing, with Oleic acid
For surface carboxyl groups raw material, with potassium permanganate catalyst, in granule after the nanometer magnetic bead surface of synthesis carries out carboxylated process
Surface forms carboxyl so that the different immunoligand enzyme of covalent bond, cell, antibody, antigen, DNA, RNA active substances, uses
In biological detection.
6. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method, it is characterised in that configured the solution of the up-conversion nano material of 15%-30% with deionized water for dispersion liquid, is subsequently adding
The immunomagnetic beadses of 1%-15%, pass through the composite that chemical hydro-thermal reaction synthesis has nucleocapsid structure at ambient temperature.
7. a kind of compound preparation of the immune magnetic Nano up-conversion luminescent material with nucleocapsid structure as claimed in claim 1
Method it is characterised in that the infrared up conversion nano material of blue light-emitting with have immune performance magnetic bead form nucleocapsid structure material
Material surface adds vulcanized lead Infrared fluorescence quantum dot, and vulcanized lead Infrared fluorescence quantum dot absorbs visible ray, launches near infrared light, and
Absorbed by up-conversion nano material；Or by excited by visible light, another wave band visible ray is launched by up-conversion luminescent material.
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