CN112083162A - Diagnostic preparation for determining immunity level - Google Patents
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- CN112083162A CN112083162A CN202010764136.5A CN202010764136A CN112083162A CN 112083162 A CN112083162 A CN 112083162A CN 202010764136 A CN202010764136 A CN 202010764136A CN 112083162 A CN112083162 A CN 112083162A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 230000036039 immunity Effects 0.000 title claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 310
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 155
- 238000002156 mixing Methods 0.000 claims abstract description 126
- 239000000427 antigen Substances 0.000 claims abstract description 57
- 102000036639 antigens Human genes 0.000 claims abstract description 57
- 108091007433 antigens Proteins 0.000 claims abstract description 57
- 238000003756 stirring Methods 0.000 claims abstract description 51
- 229920002518 Polyallylamine hydrochloride Polymers 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 30
- 239000001509 sodium citrate Substances 0.000 claims abstract description 21
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims abstract description 21
- 229940038773 trisodium citrate Drugs 0.000 claims abstract description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 claims abstract description 9
- QNILTEGFHQSKFF-UHFFFAOYSA-N n-propan-2-ylprop-2-enamide Chemical compound CC(C)NC(=O)C=C QNILTEGFHQSKFF-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 239000000203 mixture Substances 0.000 claims description 36
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 35
- 239000007864 aqueous solution Substances 0.000 claims description 35
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical compound CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 12
- 239000012065 filter cake Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 8
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 5
- 229920003043 Cellulose fiber Polymers 0.000 claims description 5
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims description 5
- 229940014800 succinic anhydride Drugs 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 11
- 239000007822 coupling agent Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- ZEMHQYNMVKDBFJ-UHFFFAOYSA-N n-(3-hydroxypropyl)prop-2-enamide Chemical compound OCCCNC(=O)C=C ZEMHQYNMVKDBFJ-UHFFFAOYSA-N 0.000 abstract description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000003745 diagnosis Methods 0.000 abstract 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 23
- 239000010931 gold Substances 0.000 description 16
- 229910052737 gold Inorganic materials 0.000 description 16
- 239000000047 product Substances 0.000 description 15
- 239000002245 particle Substances 0.000 description 12
- 238000005457 optimization Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 8
- 239000006249 magnetic particle Substances 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 241000212749 Zesius chrysomallus Species 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000002372 labelling Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 2
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 206010057249 Phagocytosis Diseases 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- GNBHRKFJIUUOQI-UHFFFAOYSA-N fluorescein Chemical compound O1C(=O)C2=CC=CC=C2C21C1=CC=C(O)C=C1OC1=CC(O)=CC=C21 GNBHRKFJIUUOQI-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000001900 immune effect Effects 0.000 description 1
- 238000003018 immunoassay Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000008782 phagocytosis Effects 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
- G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
- G01N33/54313—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals the carrier being characterised by its particulate form
- G01N33/54326—Magnetic particles
-
- 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
- G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
- G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
- G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
- G01N33/531—Production of immunochemical test materials
- G01N33/532—Production of labelled immunochemicals
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- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- Biomedical Technology (AREA)
- Chemical & Material Sciences (AREA)
- Hematology (AREA)
- Urology & Nephrology (AREA)
- Food Science & Technology (AREA)
- Biochemistry (AREA)
- Cell Biology (AREA)
- Biotechnology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Microbiology (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Medicinal Preparation (AREA)
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a diagnostic preparation for measuring immunity level, belonging to the field of biomedicine. The method comprises the steps of modifying magnetic mesoporous silica by an aminosilane coupling agent, gamma-mercaptopropyl trimethoxy silane, N-isopropyl acrylamide, N-hydroxypropyl acrylamide, concentrated sulfuric acid and hydrogen peroxide to obtain modified mesoporous silica, mixing the modified mesoporous silica with polyallylamine hydrochloride, adding chloroauric acid, stirring and mixing, adding trisodium citrate for reduction to obtain a product blank, and mixing the product blank with an antigen to obtain the diagnostic preparation for measuring the immunity level. The diagnostic preparation for measuring the immunity level has sensitive immunity diagnosis performance and has better judgment effect on the immunity level.
Description
Technical Field
The invention relates to the field of biomedicine, in particular to a diagnostic preparation for determining an immune level.
Background
The immune colloidal gold technology is a new immunological method, has a rapid development, and is increasingly widely applied to various research fields of biomedicine, particularly medical examination. Colloidal gold has become a non-radioactive standard more commonly used in immunolabeling techniques, following fluorescein, radioisotopes and enzymes.
The colloidal gold is formed by polymerizing chloroauric acid under the action of a reducing agent such as tannic acid and trisodium citrate to form gold particles with specific sizes, and is in a stable colloidal state due to electrostatic interaction, and has the characteristics of high electron density and capability of being combined with various biological macromolecules. The immune gold labeling technology mainly utilizes the characteristic of gold particles, black brown particles can be seen under a microscope when gold-labeled proteins are combined, and red or purple red spots can be seen by naked eyes when the targets are massively aggregated at corresponding ligands, so that the immune gold labeling technology is used in a qualitative or semi-quantitative rapid immunoassay method.
Immunomagnetic particle technology is a new technology developed in recent years, and is widely used in experiments such as separation and concentration. Magnetic particles are capable of covalently binding to proteins without affecting their activity and are therefore often used to capture specific proteins or isolate proteins. The principle is as follows: the antibody-labeled magnetic particles are put into a solution containing target antigens, and after full mixing reaction, an antigen-antibody magnetic particle mixture is formed, the solution passes through a magnetic column, and the target antigens are intercepted because the magnetic particles are adsorbed. Meanwhile, the magnetic sensor can be used for quantitative detection, and the quantity of the captured antibody or antigen can be determined according to the strength of magnetism.
At present, the application of the immune colloidal gold technology on a gold-labeled detection reagent has the following disadvantages:
1. due to methodological limitations, diagnostic formulations built using solely immune colloidal gold technology have low sensitivity.
2. For some samples with extremely low antigen or antibody content, the sensitivity of the rapid diagnostic preparation established by the technology is limited, so that the immune level cannot be directly and effectively judged.
Disclosure of Invention
The invention aims to provide a diagnostic preparation for measuring immunity level and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the diagnostic preparation for measuring the immunity level is characterized by mainly comprising the following raw material components in parts by weight: 20-30 parts of modified mesoporous silica, 10-12 parts of antigen, 2-4 parts of trisodium citrate and 5-8 parts of chloroauric acid; the modified mesoporous silica can adsorb antigen, so that the antibody can be effectively contacted with the antigen in the immunodiagnosis treatment.
The diagnostic preparation for measuring the immunity level is characterized by further comprising the following raw material components in parts by weight: 5-10 parts of polyallylamine hydrochloride; the polyallylamine hydrochloride is added, so that chloroauric acid ions in chloroauric acid can be adsorbed inside the modified mesoporous silica, a gold simple substance can be formed inside the modified mesoporous silica under the treatment of trisodium citrate and is sealed by the antigen, and when the antigen-times antibody phagocytosis happens, the macro-molecule property of the antigen disappears, so that the modified mesoporous gold simple substance and the magnetic particles are combined with the antibody to form macroscopic red or purple red spots, and the immunodiagnosis function is realized.
The modified mesoporous silica is prepared by jointly modifying magnetic mesoporous silica by using an aminosilane coupling agent, gamma-mercaptopropyl trimethoxy silane, N-isopropyl acrylamide, N-hydroxypropyl acrylamide, concentrated sulfuric acid and hydrogen peroxide; the magnetic mesoporous silica is prepared by mixing cellulose, mesoporous silica and magnetic particles; the addition of the cellulose can improve the adsorption performance of the mesoporous silica to the antigen.
As optimization, the diagnostic preparation for measuring the immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate, 6 parts of chloroauric acid and 8 parts of polyallylamine hydrochloride.
As optimization, the preparation method of the diagnostic preparation for measuring the immunity level mainly comprises the following preparation steps:
(1) treating magnetic mesoporous silica with concentrated sulfuric acid and hydrogen peroxide, then jointly modifying the magnetic mesoporous silica with aminosilane coupling agent, gamma-mercaptopropyl trimethoxy silane, N-isopropyl acrylamide and N-hydroxypropyl acrylamide, filtering and drying;
(2) mixing the substance obtained in the step (1) with a polyallylamine hydrochloride solution, sequentially adding chloroauric acid and trisodium citrate, stirring for reaction, filtering and drying;
(3) mixing the substance obtained in the step (2) with the antigen dispersion liquid under an alkaline condition, stirring for reaction, filtering and drying;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the preparation method of the diagnostic preparation for measuring the immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 10: 1-12: 1, mixing, stirring for reaction, filtering, washing and drying to obtain a modified mesoporous silica blank; mixing the modified mesoporous silica blank with absolute ethyl alcohol according to a mass ratio of 1: 50, adding aminopropyl trimethoxysilane and gamma-mercaptopropyl trimethoxysilane, wherein the mass of the aminopropyl trimethoxysilane is 0.1-0.3 times that of the modified mesoporous silica blank, the mass of the gamma-mercaptopropyl trimethoxysilane is 0.1-0.2 times that of the modified mesoporous silica blank, stirring for reaction, performing centrifugal separation to obtain a pretreated modified mesoporous silica blank, and mixing the pretreated modified mesoporous silica blank with N, N-dimethylformamide according to the mass ratio of 1: 10, mixing, adding succinic anhydride which is 2 times of the mass of the blank of the pretreated modified mesoporous silica, stirring for reaction, filtering, and drying to obtain the pretreated modified mesoporous silica; mixing the pretreated modified mesoporous silica and tetrahydrofuran according to a mass ratio of 1: 20-1: 30, adding N-isopropylacrylamide which is 10-12 times of the mass of the pretreated modified mesoporous silica, N-methylolacrylamide which is 0.8-1.2 times of the mass of the pretreated modified mesoporous silica and azodiisobutyronitrile which is 0.01-0.03 times of the mass of the pretreated modified mesoporous silica, stirring and reacting in a nitrogen atmosphere, filtering, washing and drying;
(2) mixing polyallylamine hydrochloride and water according to a mass ratio of 1: 10, adding a substance which is 4-5 times of the polyallylamine hydrochloride in mass and is obtained in the step (1), stirring and mixing to obtain a mixed dispersion liquid, and mixing the mixed dispersion liquid with chloroauric acid according to a mass ratio of 50: 1-80: 1, mixing, adding trisodium citrate with the mass of 0.02-0.05 time of that of the mixed dispersion liquid, stirring for reaction, filtering and drying;
(3) mixing the antigen and water according to a mass ratio of 1: 10, mixing, performing ultrasonic dispersion under the condition that the pH value is 8, adding a substance which is 4-6 times the mass of the antigen and is obtained in the step (2), stirring for reaction, filtering in a magnetic filter, removing the filtrate, and drying;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 200: 1-300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.1-0.2 times of the mass of a hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.1-0.3 times of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of hexadecyl trimethyl ammonium bromide with tetraethoxysilane according to a mass ratio of 40: 1, mixing, adding microfibrillated cellulose fibers with the mass 4-8 times that of ethyl orthosilicate, stirring for reaction, filtering, and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention uses modified mesoporous silicon dioxide when preparing the diagnostic preparation for measuring the immunity level, and polyallylamine hydrochloride is added at the same time; firstly, after the modified mesoporous silica is modified, acrylamide is grafted on pores inside the modified mesoporous silica, so that the modified mesoporous silica has pH sensitivity, that is, the pores of the modified mesoporous silica are expanded under acidic conditions, and the pores of the modified mesoporous silica are reduced when the pH is basic, and therefore, after the modified mesoporous silica is mixed with the chloroauric acid, when the chloroauric acid is reduced under the action of trisodium citrate, the pores in the modified mesoporous silica are simultaneously shrunk, so that the gold simple substance formed by reducing the chloroauric acid by the trisodium citrate can be fixed in the gap inside the modified mesoporous silica, secondly, after the modified mesoporous silica is mixed with the antigen, due to the shrinkage of the mesopores in the modified mesoporous silica, the gold particles can be prevented from being combined with the antigen to generate a color reaction, and the sensitivity of the product in the using process is improved; and polyallylamine hydrochloride is added in the preparation process of the product, and the inner surface of the modified mesoporous silica has negative charges, so that the polyallylamine hydrochloride can be adsorbed on the inner wall of the modified mesoporous silica under the action of electrostatic force after the modified mesoporous silica is mixed with the polyallylamine hydrochloride, and chloroauric acid ions can be adsorbed in the modified mesoporous silica after the modified mesoporous silica treated with the polyallylamine hydrochloride is mixed with the chloroauric acid, thereby providing conditions for the subsequent adsorption and fixation of gold simple substances by the modified mesoporous silica.
(2) The invention modifies the silicon dioxide when preparing the diagnostic preparation for measuring the immunity level, so that the mesoporous silicon dioxide has pH sensitivity, therefore, after the mesoporous silica adsorbs the antigen, the loss of the gold particles in the modified mesoporous silica can be effectively prevented through the sealing of the mesopores, and after the antigen is adsorbed, because of the macromolecule property of the antigen, the pH around the mesopores in the modified mesoporous silicon dioxide can be ensured to be stable when the antigen is not eliminated, thereby improving the sensitivity of the product, and when the antigen is eliminated, the pH around the internal pores of the modified mesoporous silica changes no matter how much the antigen is eliminated, therefore, the gold particles in the modified mesoporous silica are leaked, and due to the connectivity of the pores in the modified mesoporous silica, an obvious color reaction can be formed, so that the sensitivity of the product is further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the present invention, the following examples are given, and the methods for testing each index of the diagnostic preparation for measuring an immune level prepared in the following examples are as follows:
color rendering property: the immune level-determining diagnostic preparation obtained in each example and the comparative product were placed in an antibody solution corresponding to the antigen (concentration: 2 g/L) and observed for a color change
Determination of immune level: placing the diagnostic preparation for measuring the immunity level obtained in each example and a comparative product in antibody solutions corresponding to antigens with different concentrations, and observing the time for developing a color reaction; a shorter time of the color reaction indicates a higher level of immunity.
Example 1
A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate, 6 parts of chloroauric acid and 8 parts of polyallylamine hydrochloride.
A method for preparing a diagnostic preparation for measuring immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃ to obtain a modified mesoporous silica blank; mixing the modified mesoporous silica blank with absolute ethyl alcohol according to a mass ratio of 1: 50, mixing the mixture in a beaker, adding aminopropyltrimethoxysilane with the mass of 0.3 time of that of a modified mesoporous silica blank and gamma-mercaptopropyltrimethoxysilane with the mass of 0.2 time of that of the modified mesoporous silica blank into the beaker, stirring and reacting for 8 hours at the temperature of 65 ℃ and the rotating speed of 320r/min, then centrifugally separating to obtain a pretreated modified mesoporous silica blank, and mixing the pretreated modified mesoporous silica blank with N, N-dimethylformamide according to the mass ratio of 1: 10, mixing the mixture in a flask, adding succinic anhydride which is 2 times of the mass of the blank of the pretreated modified mesoporous silica into the flask, stirring and reacting for 6 hours at the temperature of 60 ℃ and the rotating speed of 300r/min, filtering to obtain filter residue, and drying the filter residue for 3 hours at the temperature of 80 ℃ to obtain the pretreated modified mesoporous silica; mixing the pretreated modified mesoporous silica and tetrahydrofuran according to a mass ratio of 1: 30, mixing the mixture in a four-neck flask, adding N-isopropylacrylamide which is 12 times the mass of the pretreated modified mesoporous silica, N-methylolacrylamide which is 1.2 times the mass of the pretreated modified mesoporous silica and azobisisobutyronitrile which is 0.03 times the mass of the pretreated modified mesoporous silica into the four-neck flask, introducing nitrogen into the four-neck flask at the speed of 50mL/min, stirring and reacting for 24 hours at the temperature of 80 ℃ and the rotating speed of 280r/min, filtering, removing filtrate, washing for 3 times by deionized water, and drying for 2 hours at the temperature of 60 ℃;
(2) mixing polyallylamine hydrochloride and water according to a mass ratio of 1: 10, adding a substance obtained in the step (1) with the mass 5 times that of the polyallylamine hydrochloride into a mixture of the polyallylamine hydrochloride and water, stirring and mixing for 30min under the conditions that the temperature is 40 ℃ and the rotating speed is 300r/min to obtain a mixed dispersion liquid, and mixing the mixed dispersion liquid and chloroauric acid according to the mass ratio of 80: 1, adding trisodium citrate with the mass 0.05 time that of the mixed dispersion into the mixture of the mixed dispersion and the chloroauric acid, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, adding microfibrillated cellulose fiber with the mass 8 times that of ethyl orthosilicate, stirring for reaction, filtering, and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Example 2
A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate, 6 parts of chloroauric acid and 8 parts of polyallylamine hydrochloride.
A method for preparing a diagnostic preparation for measuring immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃ to obtain a modified mesoporous silica blank; mixing the modified mesoporous silica blank with absolute ethyl alcohol according to a mass ratio of 1: 50, mixing the mixture in a beaker, adding aminopropyltrimethoxysilane with the mass of 0.3 time of that of a modified mesoporous silica blank and gamma-mercaptopropyltrimethoxysilane with the mass of 0.2 time of that of the modified mesoporous silica blank into the beaker, stirring and reacting for 8 hours at the temperature of 65 ℃ and the rotating speed of 320r/min, then centrifugally separating to obtain a pretreated modified mesoporous silica blank, and mixing the pretreated modified mesoporous silica blank with N, N-dimethylformamide according to the mass ratio of 1: 10, mixing the mixture in a flask, adding succinic anhydride which is 2 times of the mass of the blank of the pretreated modified mesoporous silica into the flask, stirring and reacting for 6 hours at the temperature of 60 ℃ and the rotating speed of 300r/min, filtering to obtain filter residue, and drying the filter residue for 3 hours at the temperature of 80 ℃ to obtain the pretreated modified mesoporous silica; mixing the pretreated modified mesoporous silica and tetrahydrofuran according to a mass ratio of 1: 30, mixing the mixture in a four-neck flask, adding N-isopropylacrylamide which is 12 times the mass of the pretreated modified mesoporous silica, N-methylolacrylamide which is 1.2 times the mass of the pretreated modified mesoporous silica and azobisisobutyronitrile which is 0.03 times the mass of the pretreated modified mesoporous silica into the four-neck flask, introducing nitrogen into the four-neck flask at the speed of 50mL/min, stirring and reacting for 24 hours at the temperature of 80 ℃ and the rotating speed of 280r/min, filtering, removing filtrate, washing for 3 times by deionized water, and drying for 2 hours at the temperature of 60 ℃;
(2) mixing polyallylamine hydrochloride and water according to a mass ratio of 1: 10, adding a substance obtained in the step (1) with the mass 5 times that of the polyallylamine hydrochloride into a mixture of the polyallylamine hydrochloride and water, stirring and mixing for 30min under the conditions that the temperature is 40 ℃ and the rotating speed is 300r/min to obtain a mixed dispersion liquid, and mixing the mixed dispersion liquid and chloroauric acid according to the mass ratio of 80: 1, adding trisodium citrate with the mass 0.05 time that of the mixed dispersion into the mixture of the mixed dispersion and the chloroauric acid, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, stirring for reaction, filtering and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Example 3
A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate and 6 parts of chloroauric acid.
A method for preparing a diagnostic preparation for measuring immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃ to obtain a modified mesoporous silica blank; mixing the modified mesoporous silica blank with absolute ethyl alcohol according to a mass ratio of 1: 50, mixing the mixture in a beaker, adding aminopropyltrimethoxysilane with the mass of 0.3 time of that of a modified mesoporous silica blank and gamma-mercaptopropyltrimethoxysilane with the mass of 0.2 time of that of the modified mesoporous silica blank into the beaker, stirring and reacting for 8 hours at the temperature of 65 ℃ and the rotating speed of 320r/min, then centrifugally separating to obtain a pretreated modified mesoporous silica blank, and mixing the pretreated modified mesoporous silica blank with N, N-dimethylformamide according to the mass ratio of 1: 10, mixing the mixture in a flask, adding succinic anhydride which is 2 times of the mass of the blank of the pretreated modified mesoporous silica into the flask, stirring and reacting for 6 hours at the temperature of 60 ℃ and the rotating speed of 300r/min, filtering to obtain filter residue, and drying the filter residue for 3 hours at the temperature of 80 ℃ to obtain the pretreated modified mesoporous silica; mixing the pretreated modified mesoporous silica and tetrahydrofuran according to a mass ratio of 1: 30, mixing the mixture in a four-neck flask, adding N-isopropylacrylamide which is 12 times the mass of the pretreated modified mesoporous silica, N-methylolacrylamide which is 1.2 times the mass of the pretreated modified mesoporous silica and azobisisobutyronitrile which is 0.03 times the mass of the pretreated modified mesoporous silica into the four-neck flask, introducing nitrogen into the four-neck flask at the speed of 50mL/min, stirring and reacting for 24 hours at the temperature of 80 ℃ and the rotating speed of 280r/min, filtering, removing filtrate, washing for 3 times by deionized water, and drying for 2 hours at the temperature of 60 ℃;
(2) mixing the substance obtained in the step (1) and water according to the mass ratio of 1: 10, mixing, adding chloroauric acid with the mass of 0.3 time of that of the substance obtained in the step (1) and trisodium citrate with the mass of 0.05 time of that of the substance obtained in the step (1) into a mixture of the substance obtained in the step (1) and water, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, adding microfibrillated cellulose fiber with the mass 8 times that of ethyl orthosilicate, stirring for reaction, filtering, and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Example 4
A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate, 6 parts of chloroauric acid and 8 parts of polyallylamine hydrochloride.
A method for preparing a diagnostic preparation for measuring immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃;
(2) mixing polyallylamine hydrochloride and water according to a mass ratio of 1: 10, adding a substance obtained in the step (1) with the mass 5 times that of the polyallylamine hydrochloride into a mixture of the polyallylamine hydrochloride and water, stirring and mixing for 30min under the conditions that the temperature is 40 ℃ and the rotating speed is 300r/min to obtain a mixed dispersion liquid, and mixing the mixed dispersion liquid and chloroauric acid according to the mass ratio of 80: 1, adding trisodium citrate with the mass 0.05 time that of the mixed dispersion into the mixture of the mixed dispersion and the chloroauric acid, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, adding microfibrillated cellulose fiber with the mass 8 times that of ethyl orthosilicate, stirring for reaction, filtering, and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Comparative example
A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate and 6 parts of chloroauric acid.
A method for preparing a diagnostic preparation for measuring immunity level mainly comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃;
(2) mixing the substance obtained in the step (1) and water according to the mass ratio of 1: 10, mixing, adding chloroauric acid with the mass of 0.3 time of that of the substance obtained in the step (1) and trisodium citrate with the mass of 0.05 time of that of the substance obtained in the step (1) into a mixture of the substance obtained in the step (1) and water, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) and (4) performing index analysis on the substance obtained in the step (3).
As optimization, the magnetic mesoporous silica in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, stirring for reaction, filtering and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
Examples of effects
The following table 1 shows the results of analysis of color rendering and immune level measurement using the diagnostic preparations for measuring immune level of examples 1 to 4 of the present invention and comparative example and the preparation methods thereof.
From the comparison of the implementation data of example 1 and the comparative example in table 1, it can be seen that when polyallylamine hydrochloride is added into the product and mesoporous silica is modified, the product has effective immunodiagnostic capability, and from the comparison of the color development time under the condition of different antibody concentrations, the product prepared by the invention can be found to have the capability of efficiently determining the immune level. As can be seen from the comparison between example 1 and example 2 in table 1, when no cellulose is added to the product, the adsorption property of the modified mesoporous silica to antigens is deteriorated, so that the gold particles in the modified mesoporous silica are easily lost, thereby reducing the color development time of the product, and as can be seen from the comparison between example 1 and example 3 in table 1, when no polyallylamine hydrochloride is added to the product, the adsorption property of the modified mesoporous silica to the gold particles is reduced, so that the gold particles cannot be immobilized in the modified mesoporous silica, and the product cannot diagnose the immune level; from the comparison between example 1 and example 4, it can be seen that, when the modified mesoporous silica added in the product has no pH sensitivity, the modified mesoporous silica cannot fix the gold particles during the reduction of the chloroauric acid, so that the gold particles are combined with the antigen, and the subsequent product cannot form a color reaction.
Claims (1)
1. A diagnostic preparation for measuring immunity level mainly comprises the following raw material components in parts by weight: 28 parts of modified mesoporous silica, 10 parts of antigen, 4 parts of trisodium citrate, 6 parts of chloroauric acid and 8 parts of polyallylamine hydrochloride;
the preparation method of the diagnostic preparation for determining the immunity level comprises the following preparation steps:
(1) mixing 98% concentrated sulfuric acid and 30% hydrogen peroxide according to a volume ratio of 7: 3, mixing to obtain a mixed treatment solution, and mixing the mixed treatment solution with the magnetic mesoporous silica according to a mass ratio of 12: 1, mixing, stirring and reacting for 2 hours at the temperature of 45 ℃ and the rotating speed of 300r/min, filtering to obtain a filter cake, washing the filter cake for 5 times by using water, and drying for 6 hours at the temperature of 80 ℃ to obtain a modified mesoporous silica blank; mixing the modified mesoporous silica blank with absolute ethyl alcohol according to a mass ratio of 1: 50, mixing the mixture in a beaker, adding aminopropyltrimethoxysilane with the mass of 0.3 time of that of a modified mesoporous silica blank and gamma-mercaptopropyltrimethoxysilane with the mass of 0.2 time of that of the modified mesoporous silica blank into the beaker, stirring and reacting for 8 hours at the temperature of 65 ℃ and the rotating speed of 320r/min, then centrifugally separating to obtain a pretreated modified mesoporous silica blank, and mixing the pretreated modified mesoporous silica blank with N, N-dimethylformamide according to the mass ratio of 1: 10, mixing the mixture in a flask, adding succinic anhydride which is 2 times of the mass of the blank of the pretreated modified mesoporous silica into the flask, stirring and reacting for 6 hours at the temperature of 60 ℃ and the rotating speed of 300r/min, filtering to obtain filter residue, and drying the filter residue for 3 hours at the temperature of 80 ℃ to obtain the pretreated modified mesoporous silica; mixing the pretreated modified mesoporous silica and tetrahydrofuran according to a mass ratio of 1: 30, mixing the mixture in a four-neck flask, adding N-isopropylacrylamide which is 12 times the mass of the pretreated modified mesoporous silica, N-methylolacrylamide which is 1.2 times the mass of the pretreated modified mesoporous silica and azobisisobutyronitrile which is 0.03 times the mass of the pretreated modified mesoporous silica into the four-neck flask, introducing nitrogen into the four-neck flask at the speed of 50mL/min, stirring and reacting for 24 hours at the temperature of 80 ℃ and the rotating speed of 280r/min, filtering, removing filtrate, washing for 3 times by deionized water, and drying for 2 hours at the temperature of 60 ℃;
(2) mixing polyallylamine hydrochloride and water according to a mass ratio of 1: 10, adding a substance obtained in the step (1) with the mass 5 times that of the polyallylamine hydrochloride into a mixture of the polyallylamine hydrochloride and water, stirring and mixing for 30min under the conditions that the temperature is 40 ℃ and the rotating speed is 300r/min to obtain a mixed dispersion liquid, and mixing the mixed dispersion liquid and chloroauric acid according to the mass ratio of 80: 1, adding trisodium citrate with the mass 0.05 time that of the mixed dispersion into the mixture of the mixed dispersion and the chloroauric acid, stirring and reacting for 3 hours at the temperature of 40 ℃ and the rotating speed of 280r/min, filtering, and drying in vacuum;
(3) mixing the antigen and water according to a mass ratio of 1: 10, regulating the pH value of a mixture of the antigen and water to 8 by using a sodium hydroxide solution with the mass fraction of 2%, ultrasonically dispersing for 10min under the condition of the frequency of 45kHz, adding a substance obtained in the step (2) with the mass of 6 times of the antigen into the mixture of the antigen and water, stirring and reacting for 5h under the conditions of the temperature of 30 ℃ and the rotating speed of 300r/min, removing filtrate by magnetic filtration to obtain a blank, and drying the blank for 12h under the condition of the temperature of 40 ℃;
(4) performing index analysis on the substance obtained in the step (3);
the magnetic mesoporous silica obtained in the step (1) is prepared by mixing an aqueous solution of hexadecyl trimethyl ammonium bromide with the mass fraction of 2% and nano ferroferric oxide according to the mass percentage of 300: 1, mixing, adding 1,3, 5-trimethylbenzene accounting for 0.2 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution and ammonia water accounting for 0.3 time of the mass of the hexadecyl trimethyl ammonium bromide aqueous solution, performing ultrasonic dispersion to obtain a mixed aqueous solution of the hexadecyl trimethyl ammonium bromide, and mixing the mixed aqueous solution of the hexadecyl trimethyl ammonium bromide with ethyl orthosilicate according to a mass ratio of 40: 1, mixing, adding microfibrillated cellulose fiber with the mass 8 times that of ethyl orthosilicate, stirring for reaction, filtering, and drying to obtain a magnetic mesoporous silica blank; magnetic mesoporous silica blank ammonium nitrate is added according to the mass ratio of 1: 2, mixing, adding absolute ethyl alcohol with the mass of 10 times of that of the magnetic mesoporous silica blank, condensing, refluxing, filtering and drying to obtain the magnetic mesoporous silica.
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