CN114873644A - Preparation method of molecular carrier for molecular detection - Google Patents
Preparation method of molecular carrier for molecular detection Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002073 nanorod Substances 0.000 claims abstract description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- -1 modified sodium gadolinium tungstate Chemical class 0.000 claims abstract description 27
- 239000003999 initiator Substances 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 239000004088 foaming agent Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000005469 granulation Methods 0.000 claims abstract description 6
- 230000003179 granulation Effects 0.000 claims abstract description 6
- 238000000465 moulding Methods 0.000 claims abstract description 6
- 239000012466 permeate Substances 0.000 claims abstract description 6
- UZPIQWSRYNIAEI-UHFFFAOYSA-N gadolinium sodium Chemical compound [Na][Gd] UZPIQWSRYNIAEI-UHFFFAOYSA-N 0.000 claims description 24
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 claims description 24
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 20
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 5
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 5
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 5
- 229920002101 Chitin Polymers 0.000 claims description 5
- 102000004190 Enzymes Human genes 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000005642 Oleic acid Substances 0.000 claims description 5
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 5
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 abstract description 6
- 239000003814 drug Substances 0.000 abstract description 4
- 229940079593 drug Drugs 0.000 abstract description 3
- 239000000693 micelle Substances 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 3
- 238000004557 single molecule detection Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000013459 approach Methods 0.000 description 2
- 230000006399 behavior Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000011896 sensitive detection Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001712 DNA sequencing Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000007877 drug screening Methods 0.000 description 1
- 238000013399 early diagnosis Methods 0.000 description 1
- 238000000329 molecular dynamics simulation Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000001575 pathological effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/006—Compounds containing, besides tungsten, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Nanotechnology (AREA)
- Medicinal Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Food Science & Technology (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
Abstract
The invention discloses a preparation method of a molecular carrier for molecular detection, which comprises the following steps: s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content; s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, putting the mixture into a double-screw extruder for extrusion molding; s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 10-13 times of atmospheric pressure, continuously reducing the pressure for 30-40min, quickly reducing the pressure for 1-2min to normal pressure to obtain a matrix, and then throwing the content into a centrifugal machine to throw out and permeate the content into the matrix. The molecular carrier prepared by the method has high drug loading capacity, stable micelle structure, high pH sensitivity of target release, high biocompatibility, small external influence on molecular detection and good loading capacity.
Description
Technical Field
The invention relates to the technical field of molecular detection, in particular to a preparation method of a molecular carrier for molecular detection.
Background
Single molecule detection is an ultra-sensitive detection technology that has been rapidly developed in the last decade, and opens a new door for analytical chemists. Single Molecule Detection (SMD) and its analysis is a delicate approach to examine dynamic changes and material interactions in cellular systems. At present, people can not only detect and image single molecules in a solution, but also measure the spectral properties of the single molecules, thereby monitoring the approach of chemical reaction in real time, and particularly detecting biomacromolecules to improve the information between the structure and the function of the molecules. Meanwhile, the single molecule detection technology is an ultra-sensitive detection technology, can detect single molecules, and is widely applied to the fields of chemical analysis, DNA sequencing, nano material analysis, medical diagnosis, molecular dynamics mechanism, food safety and the like. Compared with the traditional analysis method, the single molecule detection method researches the individual behaviors of the system in a non-equilibrium state or the fluctuation behaviors in an equilibrium state, so the method is particularly suitable for researching the kinetics of chemical and biochemical reactions, the interaction of biological molecules, structural and functional information, early diagnosis of serious diseases, pathological research, high-throughput drug screening and the like.
In the single-molecule detection technology, a detection object of a sample to be detected is generally extracted and then placed on a molecular carrier for detection, and most of the molecular carriers adopted in the detection adopt a hard substrate. In the field of medicine, factors of high drug loading capacity, stable micelle structure, pH sensitivity of target release and high biocompatibility are important factors for judging the performance of a molecular carrier, and the existing molecular carrier cannot ensure the stability of the performance of the factors, so that certain errors exist in detection, and the detection complexity and difficulty are increased.
Disclosure of Invention
The present invention is directed to a method for preparing a molecular carrier for molecular detection, which solves the above-mentioned problems of the prior art.
The technical scheme of the invention provides a preparation method of a molecular carrier for molecular detection, which comprises the following steps:
s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content;
s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, and putting the mixture into a double-screw extruder for extrusion molding;
s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 10-13 times of atmospheric pressure, continuously reducing the pressure for 30-40min, quickly reducing the pressure for 1-2min to normal pressure to obtain a matrix, and then throwing the content into a centrifugal machine to throw out and permeate the content into the matrix.
In a preferred embodiment, the mesoporous silica, the modified sodium gadolinium tungstate nanorod, the content, the compatilizer, the initiator, the biological affinity agent and the foaming agent are respectively in parts by weight: 60-70 parts of mesoporous silica, 30-40 parts of modified sodium gadolinium tungstate nanorods, 20-30 parts of contents, 3-4 parts of compatilizer, 3-4 parts of initiator, 2-4 parts of foaming agent and 2-3 parts of biological affinity agent.
In a preferred embodiment, the content is active enzyme content, the initiator is acrylic acid, the specific gravity agent is light calcium carbonate, and the biological affinity agent is chitin.
In a preferred embodiment, the preparation method of the modified sodium gadolinium tungstate nanorod comprises the following steps:
a1: mixing oleic acid, octadecene and GdCl 3 ·6H 2 Mixing O powder, introducing argon, heating to 150-160 ℃, stirring to obtain a light yellow clarified liquid, and stopping heating to naturally cool the system to room temperature;
a2: na-containing solution is slowly dripped 2 WO 4 ·2H 2 Sealing and stirring the ammonia water solution of O at room temperature to obtain a yellowish white solution;
a3: introducing argon, keeping the temperature at 40-60 ℃ for 50-80min, keeping the temperature at 80-85 ℃ for 60-70min, then keeping the temperature at 110-130 ℃ for 50-60min to remove ammonia water, connecting a condensation pipe after removing ammonia water, raising the temperature of the system to 260-280 ℃ and keeping the temperature for 40-50min, and then naturally cooling to room temperature;
a4: centrifuging, discarding the supernatant, adding cyclohexane, performing ultrasonic dispersion, adding alcohol, performing ultrasonic dispersion, centrifuging, collecting, discarding the supernatant to obtain a cyclohexane solution of a sodium gadolinium tungstate nanorod, and extracting to obtain a sodium gadolinium tungstate nanorod;
a5: adding a cyclohexane solution of sodium gadolinium tungstate nanorods into deionized water, then dropwise adding concentrated hydrochloric acid, sealing and stirring, and transferring the sodium gadolinium tungstate nanorods from the cyclohexane on the upper layer into the deionized water; and (4) centrifugally collecting, washing with deionized water, ultrasonically dispersing and drying to obtain the modified sodium gadolinium tungstate nanorod.
In a preferred embodiment, the temperatures of the zones of the single screw granulator are: the first zone is 150-170 ℃, the second zone is 160-175 ℃, the third zone is 180-190 ℃, and the fourth zone is 190-200 ℃; the temperature of each subarea of the double-screw extruder is 180-class temperature in the first area, 185-class temperature in the second area, 195-class temperature in the third area, 190-class temperature in the third area and 200-class temperature in the fourth area, 190-class temperature in the fourth area and 200-class temperature in the fourth area.
The technical scheme of the invention has the beneficial effects that:
the molecular carrier prepared by the method has high drug loading capacity, stable micelle structure, high pH sensitivity of target release, high biocompatibility, small external influence on molecular detection and good loading capacity.
The mesoporous silica modified gadolinium sodium tungstate nanorod and the content are used as basic materials, and the compatilizer, the initiator, the biological affinity agent and the foaming agent are used as auxiliary materials. The sodium gadolinium tungstate nanorod prepared by the pyrolysis method is lipophilic, and in order to coat mesoporous silica on the surface of the sodium gadolinium tungstate nanorod, the sodium gadolinium tungstate nanorod needs to be subjected to hydrophilic modification. The sodium gadolinium tungstate nanorod NaxGdWO3 is treated by concentrated hydrochloric acid, and then microwave modification is carried out, so that the subsequent mesoporous silica adsorption rate is improved, and the loading capacity of a molecular carrier is increased.
Detailed Description
The following embodiments are further illustrative of the present invention. The embodiments of the present invention have been presented for purposes of illustration and description, and are not intended to be exhaustive or limited to the invention in the form disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art. The embodiment was chosen and described in order to best explain the principles of the invention and the practical application, and to enable others of ordinary skill in the art to understand the invention for various embodiments with various modifications as are suited to the particular use contemplated.
Example 1
The technical scheme of the invention provides a preparation method of a molecular carrier for molecular detection, which comprises the following steps:
s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content;
s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, putting the mixture into a double-screw extruder for extrusion molding;
s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 13 times of atmospheric pressure, keeping the pressure for 30min, quickly reducing the pressure for 1min to normal pressure to obtain a matrix, and throwing the content into a centrifugal machine to throw out and permeate into the matrix.
In a preferred embodiment, the mesoporous silica, the modified sodium gadolinium tungstate nanorod, the content, the compatilizer, the initiator, the biological affinity agent and the foaming agent are respectively in parts by weight: 60-70 parts of mesoporous silica, 30-40 parts of modified sodium gadolinium tungstate nanorods, 20-30 parts of contents, 3-4 parts of compatilizer, 3-4 parts of initiator, 2-4 parts of foaming agent and 2-3 parts of biological affinity agent.
In a preferred embodiment, the content is active enzyme content, the initiator is acrylic acid, the specific gravity agent is light calcium carbonate, and the biological affinity agent is chitin.
In a preferred embodiment, the preparation method of the modified sodium gadolinium tungstate nanorod comprises the following steps:
a1: mixing oleic acid, octadecene and GdCl 3 ·6H 2 Mixing O powder, introducing argon, heating to 150-160 ℃, stirring to obtain a light yellow clarified liquid, and stopping heating to naturally cool the system to room temperature;
a2: na-containing solution is slowly dripped 2 WO 4 ·2H 2 Sealing and stirring the ammonia water solution of O at room temperature to obtain a yellowish white solution;
a3: introducing argon, keeping the temperature at 40 ℃ for 50min, keeping the temperature at 80 ℃ for 60min, then keeping the temperature at 110-130 ℃ for 50min to remove ammonia water, connecting a condensation pipe after removing ammonia water, heating the system to 260 ℃, keeping the temperature for 40min, and then naturally cooling to room temperature;
a4: centrifuging, discarding the supernatant, adding cyclohexane, performing ultrasonic dispersion, adding alcohol, performing ultrasonic dispersion, centrifuging, collecting, discarding the supernatant to obtain a cyclohexane solution of a sodium gadolinium tungstate nanorod, and extracting to obtain a sodium gadolinium tungstate nanorod;
a5: adding a cyclohexane solution of sodium gadolinium tungstate nanorods into deionized water, then dropwise adding concentrated hydrochloric acid, sealing and stirring, and transferring the sodium gadolinium tungstate nanorods from the cyclohexane on the upper layer into the deionized water; and (4) centrifugally collecting, washing with deionized water, ultrasonically dispersing and drying to obtain the modified sodium gadolinium tungstate nanorod.
In a preferred embodiment, the temperatures of the zones of the single screw granulator are: the temperature of the first area is 150 ℃, the temperature of the second area is 160 ℃, the temperature of the third area is 180 ℃, and the temperature of the fourth area is 190 ℃; the temperature of each subarea of the double-screw extruder is 180 ℃ in the first area, 185 ℃ in the second area, 190 ℃ in the third area and 190 ℃ in the fourth area.
Example 2
The technical scheme of the invention provides a preparation method of a molecular carrier for molecular detection, which comprises the following steps:
s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content;
s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, and putting the mixture into a double-screw extruder for extrusion molding;
s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 10 times of atmospheric pressure, keeping for 40min, quickly reducing the pressure for 2min to normal pressure to obtain a matrix, and throwing the content into a centrifugal machine to throw out and permeate into the matrix.
In a preferred embodiment, the mesoporous silica, the modified sodium gadolinium tungstate nanorod, the content, the compatilizer, the initiator, the biological affinity agent and the foaming agent are respectively in parts by weight: 70 parts of mesoporous silica, 40 parts of modified sodium gadolinium tungstate nanorods, 30 parts of contents, 4 parts of compatilizer, 4 parts of initiator, 4 parts of foaming agent and 3 parts of biological affinity agent.
In a preferred embodiment, the content is active enzyme content, the initiator is acrylic acid, the specific gravity agent is light calcium carbonate, and the biological affinity agent is chitin.
In a preferred embodiment, the preparation method of the modified sodium gadolinium tungstate nanorod comprises the following steps:
a1: mixing oleic acid, octadecene and GdCl 3 ·6H 2 Mixing O powder, introducing argon, heating to the temperature of 150-160 ℃, stirring to obtain a light yellow clarified liquid, and then stopping heating to naturally cool the system to room temperature;
a2: na-containing solution is slowly dripped 2 WO 4 ·2H 2 Sealing and stirring the ammonia water solution of O at room temperature to obtain a yellowish white solution;
a3: introducing argon, keeping the temperature at 60 ℃ for 80min, keeping the temperature at 85 ℃ for 70min, keeping the temperature at 130 ℃ for 60min to remove ammonia water, connecting a condensation pipe after removing ammonia water, heating the system to 280 ℃, keeping the temperature for 50min, and naturally cooling to room temperature;
a4: centrifuging, discarding the supernatant, adding cyclohexane, performing ultrasonic dispersion, adding alcohol, performing ultrasonic dispersion, centrifuging, collecting, discarding the supernatant to obtain a cyclohexane solution of a sodium gadolinium tungstate nanorod, and extracting to obtain a sodium gadolinium tungstate nanorod;
a5: adding a cyclohexane solution of sodium gadolinium tungstate nanorods into deionized water, then dropwise adding concentrated hydrochloric acid, sealing and stirring, and transferring the sodium gadolinium tungstate nanorods from the cyclohexane on the upper layer into the deionized water; and (4) centrifugally collecting, washing with deionized water, ultrasonically dispersing and drying to obtain the modified sodium gadolinium tungstate nanorod.
In a preferred embodiment, the temperatures of the zones of the single screw granulator are: 170 ℃ in the first area, 175 ℃ in the second area, 190 ℃ in the third area and 200 ℃ in the fourth area; the temperature of each subarea of the double-screw extruder is 190 ℃ in a first area, 195 ℃ in a second area, 200 ℃ in a third area and 200 ℃ in a fourth area.
Example 3
The technical scheme of the invention provides a preparation method of a molecular carrier for molecular detection, which comprises the following steps:
s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content;
s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, and putting the mixture into a double-screw extruder for extrusion molding;
s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 12 times of atmospheric pressure, quickly reducing the pressure for 1-2min to normal pressure after continuously maintaining for 35min to obtain a matrix, and throwing the content into a centrifugal machine to throw out and permeate into the matrix.
In a preferred embodiment, the mesoporous silica, the modified sodium gadolinium tungstate nanorod, the content, the compatilizer, the initiator, the biological affinity agent and the foaming agent are respectively in parts by weight: 65 parts of mesoporous silicon dioxide, 35 parts of modified sodium gadolinium tungstate nanorods, 25 parts of contents, 3.5 parts of compatilizer, 3.4 parts of initiator, 3 parts of foaming agent and 2.5 parts of biological affinity agent.
In a preferred embodiment, the content is active enzyme content, the initiator is acrylic acid, the specific gravity agent is light calcium carbonate, and the biological affinity agent is chitin.
In a preferred embodiment, the preparation method of the modified sodium gadolinium tungstate nanorod comprises the following steps:
a1: mixing oleic acid, octadecene and GdCl 3 ·6H 2 Mixing O powder, introducing argon, heating to 155 ℃, stirring to obtain a light yellow clarified liquid, and stopping heating to naturally cool the system to room temperature;
a2: na-containing solution is slowly dripped 2 WO 4 ·2H 2 Sealing and stirring the ammonia water solution of O at room temperature to obtain a yellowish white solution;
a3: introducing argon, keeping the temperature at 50 ℃ for 75min, keeping the temperature at 85 ℃ for 70min, keeping the temperature at 120 ℃ for 55min to remove ammonia water, connecting a condensation pipe after removing ammonia water, heating the system to 270 ℃, keeping the temperature for 45min, and naturally cooling to room temperature;
a4: centrifuging, discarding the supernatant, adding cyclohexane, performing ultrasonic dispersion, adding alcohol, performing ultrasonic dispersion, centrifuging, collecting, discarding the supernatant to obtain a cyclohexane solution of a sodium gadolinium tungstate nanorod, and extracting to obtain a sodium gadolinium tungstate nanorod;
a5: adding a cyclohexane solution of sodium gadolinium tungstate nanorods into deionized water, then dropwise adding concentrated hydrochloric acid, sealing and stirring, and transferring the sodium gadolinium tungstate nanorods from the cyclohexane on the upper layer into the deionized water; and (4) centrifugally collecting, washing with deionized water, ultrasonically dispersing and drying to obtain the modified sodium gadolinium tungstate nanorod.
In a preferred embodiment, the temperatures of the zones of the single screw granulator are: the first zone is 150-170 ℃, the second zone is 160-175 ℃, the third zone is 180-190 ℃, and the fourth zone is 190-200 ℃; the temperature of each subarea of the double-screw extruder is 180-class temperature in the first area, 185-class temperature in the second area, 195-class temperature in the third area, 190-class temperature in the third area and 200-class temperature in the fourth area, 190-class temperature in the fourth area and 200-class temperature in the fourth area.
It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by one of ordinary skill in the art and related arts based on the embodiments of the present invention without any creative effort, shall fall within the protection scope of the present invention. Structures, devices, and methods of operation not specifically described or illustrated herein are generally practiced in the art without specific recitation or limitation.
Claims (5)
1. A method for preparing a molecular carrier for molecular detection is characterized by comprising the following steps:
s1: selecting a base material, wherein the base material comprises mesoporous silica, a modified sodium gadolinium tungstate nanorod and a content;
s2: mixing the base materials, adding a compatilizer, an initiator and a biological affinity agent, putting the mixture into a single-screw granulator for extrusion granulation, adding a foaming agent, and putting the mixture into a double-screw extruder for extrusion molding;
s3: and (3) after molding, feeding the mixture into a high-pressure chamber, controlling the pressure of high-pressure air to be 10-13 times of atmospheric pressure, continuously reducing the pressure for 30-40min, quickly reducing the pressure for 1-2min to normal pressure to obtain a matrix, and then throwing the content into a centrifugal machine to throw out and permeate the content into the matrix.
2. The method for preparing the molecular carrier for molecular detection according to claim 1, wherein the mesoporous silica, the modified sodium gadolinium tungstate nanorod, the content, the compatilizer, the initiator, the biological affinity agent and the foaming agent are respectively in parts by weight as follows: 60-70 parts of mesoporous silica, 30-40 parts of modified sodium gadolinium tungstate nanorods, 20-30 parts of contents, 3-4 parts of compatilizer, 3-4 parts of initiator, 2-4 parts of foaming agent and 2-3 parts of biological affinity agent.
3. The method of claim 1, wherein the content is active enzyme content, the initiator is acrylic acid, the specific weight agent is light calcium carbonate, and the bio-affinity agent is chitin.
4. The preparation method of the molecular carrier for molecular detection according to claim 1, wherein the preparation method of the modified sodium gadolinium tungstate nanorod is as follows:
a1: mixing oleic acid, octadecene and GdCl 3 ·6H 2 Mixing O powder, introducing argon, heating to 150-160 ℃, stirring to obtain a light yellow clarified liquid, and stopping heating to naturally cool the system to room temperature;
a2: na-containing solution is slowly dripped 2 WO 4 ·2H 2 Sealing and stirring the ammonia water solution of O at room temperature to obtain a yellowish white solution;
a3: introducing argon, keeping the temperature at 40-60 ℃ for 50-80min, keeping the temperature at 80-85 ℃ for 60-70min, then keeping the temperature at 110-130 ℃ for 50-60min to remove ammonia water, connecting a condensation pipe after removing ammonia water, raising the temperature of the system to 260-280 ℃ and keeping the temperature for 40-50min, and then naturally cooling to room temperature;
a4: centrifuging, discarding the supernatant, adding cyclohexane, performing ultrasonic dispersion, adding alcohol, performing ultrasonic dispersion, centrifuging, collecting, discarding the supernatant to obtain a cyclohexane solution of a sodium gadolinium tungstate nanorod, and extracting to obtain a sodium gadolinium tungstate nanorod;
a5: adding a cyclohexane solution of sodium gadolinium tungstate nanorods into deionized water, then dropwise adding concentrated hydrochloric acid, sealing and stirring, and transferring the sodium gadolinium tungstate nanorods from the cyclohexane on the upper layer into the deionized water; and (4) centrifugally collecting, washing with deionized water, ultrasonically dispersing and drying to obtain the modified sodium gadolinium tungstate nanorod.
5. The method for preparing a molecular carrier for molecular detection according to claim 1, wherein the temperatures of the zones of the single-screw pelletizer are as follows: the first zone is 150-170 ℃, the second zone is 160-175 ℃, the third zone is 180-190 ℃, and the fourth zone is 190-200 ℃; the temperature of each subarea of the double-screw extruder is 180-class temperature in the first area, 185-class temperature in the second area, 195-class temperature in the third area, 190-class temperature in the third area and 200-class temperature in the fourth area, 190-class temperature in the fourth area and 200-class temperature in the fourth area.
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