CN108133794B - The detection application of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine * * class drug - Google Patents
The detection application of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine * * class drug Download PDFInfo
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- CN108133794B CN108133794B CN201810148564.8A CN201810148564A CN108133794B CN 108133794 B CN108133794 B CN 108133794B CN 201810148564 A CN201810148564 A CN 201810148564A CN 108133794 B CN108133794 B CN 108133794B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/42—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of organic or organo-metallic materials, e.g. graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
A kind of monodisperse superparamagnetic nanometer magnetic bead and its benzodiazepine *The detection application of class drug is used for detection benzodiazepine *Class drug, specifically: body fluid to be measured is dissolved in ammonia spirit, the above-mentioned monodisperse superparamagnetic nanometer magnetic bead being prepared is added and benzodiazepine * is surveyed by liquid chromatography mass joint inspection after absorption and elutionThe content of class drug.The present invention utilizes functionalized nano magnetic bead and benzodiazepine *The advantage of class drug selectivity enrichment and separation, can significantly improve pre-treatment efficiency, reduce the influence of human factor, largely improve the accuracy of detection, be trace benzodiazepine *Accurate examine of class drug provides more reliable guarantee.
Description
Technical field
It is specifically a kind of based on Magnetic solid phases extraction automation the present invention relates to a kind of technology of field of chemical detection
Technology is for detecting benzodiazepine *The method of class drug.
Background technique
Benzodiazepine *Class drug has the characteristics that dosage is few, metabolism is fast, half-life short, dense in tissue and body fluid in vivo
Degree is very low, and the overwhelming majority is changed into metabolin and excretes quickly with urine, and is usually by sample product in judicial expertise
Urine, saliva or blood after subject medication a few hours or even after tens of hours, therefore benzodiazepine *Class drug and its metabolism
Object content is lower, needs to have highly sensitive detection method.
Summary of the invention
The present invention is directed to existing detection benzodiazepine *The generally existing complex steps of the method for class drug are time-consuming, reagent consumption
Amount is big, by the defect that operator is influenced or reliability is bad, propose a kind of monodisperse superparamagnetic nanometer magnetic bead and its
Benzodiazepine *The detection application of class drug prepares the stable monodisperse superparamagnetic of sulfonate radical by improved hydrothermal synthesis method
Nano ferriferrous oxide modifies upper epsilon-caprolactams base and phenyl structure by silane-modified later, the two structures is utilized to assist
Same-action, selectively by benzene phenodiazine from biological sampleClass Drug absorbability;The present invention utilizes functionalized nano magnetic bead and benzene
And phenodiazineThe advantage of class drug selectivity enrichment and separation, can significantly improve pre-treatment efficiency, reduce the influence of human factor,
The accuracy of detection is largely improved, is trace benzodiazepine *Accurate examine of class drug provides more reliable guarantee.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of preparation method of monodisperse superparamagnetic nanometer magnetic bead, by into iron particle solution successively
The kayexalate and sodium acetate as dispersing agent is added, heated reaction obtains monodisperse superparamagnetic ferroso-ferric oxide
Nanosphere;Then it is mixed with tetraethyl orthosilicate, γ-methacryloxypropyl trimethoxy silane and acetic acid with reality
Existing vinyl modified;Finally by modified magnetic ferroferric oxide nanometer ball and oil-soluble initiator, N- vinyl-ε-in oneself
Amide and vinyl benzene-like compounds react in a nitrogen environment realizes polymer coated modification, obtains monodisperse superparamagnetic nanometer
Magnetic bead.
The iron particle solution is the glycol solution of anhydrous ferric chloride, which uses but be not limited to ethylene glycol, a contracting
Dipropylene glycol, triethylene glycol, 1,2-PD, 1,2- hexylene glycol, 2- methyl-1,3-propanediol or combinations thereof, preferably second two
Alcohol, dipropylene glycol and 1,2- propylene glycol.
The quality of the dispersing agent is 40~90% of anhydrous ferric chloride in iron particle solution, and the dispersing agent is for improving
The dispersibility of ferriferrous oxide nano sphere, kayexalate are a kind of polyanion electrolyte, sulfonate group and trivalent
Coordination occurs for iron ion, can control the partial size of ferriferrous oxide nano sphere, the surface band of final four oxidations three-body nanosphere
There is the group that sulfonate radical is stable, can make entire magnetic bead by the repulsive force stable suspersion of negative electricity in aqueous solution.
The heating reaction, it is preferred to use ptfe autoclave is reacted 5~30 hours at 160~220 DEG C.
γ-methacryloxypropyl trimethoxy silane quality be tetraethyl orthosilicate quality 15~
50%, preferably tetraethyl orthosilicate 20%, in which: tetraethyl orthosilicate and γ-methacryloxypropyl trimethoxy
Silane can produce the structure of crosslinking net in acid condition cohydrolysis, improve γ-methacryloxypropyl trimethoxy
Silane hydrolyzate rate and the number for modifying upper double bond.
The vinyl modified reacts 6~12 hours preferably under 40~70 DEG C of environment.
The modification preferably first disperses modified magnetic ferroferric oxide nanometer ball in inert organic solvents,
The inert organic solvents are used but are not limited to: acetonitrile, ether, methyl ether, toluene, acetone, isopropanol, ethyl alcohol, methanol, benzene, tetrahydro
Furans, dimethylformamide and dioxane;Preferably acetonitrile, toluene, isopropanol and ethyl alcohol.
The oil-soluble initiator is the initiator of peroxide, uses but is not limited to: dibenzoyl peroxide, mistake
Aoxidize lauroyl, tert-Butyl peroxypivalate or perbenzoic acid;Preferably dibenzoyl peroxide.
The vinyl benzene-like compounds, contain divinylbenzene as crosslinking agent, using but be not limited to: 4- methoxy
Base styrene, styrene, divinylbenzene, 3- chlorostyrene, α-methylstyrene, trans--Beta-methyl styrene, methyl 4- second
Enyl benzoate or combinations thereof;The preferably mixture of divinylbenzene and other vinyl benzene classes.
The mass ratio of the N- vinyl-Epsilon-caprolactam and vinyl benzene-like compounds is 1:0.1~10;Preferably
1:0.2~4, phenyl ring and benzene phenodiazine in vinyl benzene-like compoundsThe phenyl ring generation π-πconjugation of class drug, and N-
Vinyl-ε-caprolactam has the similar interior amide ring of structure to seven yuan of imines lactam nucleus, therefore to acyl in seven yuan of imines
Amine has certain electrophilicity.Benzodiazepine *Class drug major part metabolite all exists with hydrochloride form, when addition alkali
Hydrophobicity is stronger after property substance makes it slough hydrochloride, is more advantageous to and is total to by N- vinyl-Epsilon-caprolactam and vinyl benzene class
The magnetisable material of modification is adsorbed.
The modification is preferably heated to reacting 5~20 hours at 70~90 DEG C in a nitrogen environment.
The present invention relates to a kind of applications of nanometer magnetic bead being prepared based on the above method, are used for detection benzo two
NitrogenClass drug, specifically: body fluid to be measured is dissolved in ammonia spirit, the above-mentioned monodisperse superparamagnetic being prepared is added
Nanometer magnetic bead simultaneously surveys benzodiazepine * by liquid chromatography mass joint inspection after absorption and elutionThe content of class drug.
Technical effect
Compared with prior art, the present invention prepares monodispersed four oxygen of super-paramagnetism nano by improved hydrothermal synthesis method
Change three-iron and is finally modified to caprolactam base and phenyl structure.Using Magnetic solid phases extraction combine automated processing equipment as
Pretreatment technology develops benzodiazepine * in urineThe detection method of class drug.The step of this solution simplifies pre-treatments, together
When have manual intervention it is few, high-throughput processing advantage.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph of the monodisperse superparamagnetic ferriferrous oxide nano sphere of 500nm prepared by embodiment 2;
Fig. 2 is sweeping for the monodisperse superparamagnetic ferriferrous oxide nano sphere of 500nm vinyl modified prepared by embodiment 3
Retouch electron microscope;
Fig. 3 is 500nmN- vinyl-Epsilon-caprolactam prepared by embodiment 4 and the co-modified nano magnetic of divinylbenzene
The scanning electron microscope (SEM) photograph of pearl.
Specific embodiment
Embodiment 1
The present embodiment specifically includes the following steps: by 0.65g anhydrous ferric chloride be dissolved to 30mL dipropylene glycol and
In the ethylene glycol mixture of 30mL, be added 0.35g kayexalate, stirring 1 hour to uniformly after, add 3.5g vinegar
Then above-mentioned mixed liquor is poured onto the reaction kettle of polytetrafluoroethylene (PTFE), and put it into baking to uniform after stirring 1 hour by sour sodium
Case reacts 8 hours at 200 DEG C.It is clean that Ion Cleaning is spent after being cooled to room temperature, is dried at 60 DEG C, and the monodisperse of 100nm is obtained
Superparamagnetic iron oxide nanosphere (Fe3O4)。
Embodiment 2
The present embodiment is specifically includes the following steps: 2g anhydrous ferric chloride is dissolved in the ethylene glycol of 110mL, addition 1.5g
Kayexalate, stirring 1 hour add 8g sodium acetate to after uniformly, then stirring 1 hour above-mentioned will be mixed to uniform
The reaction kettle that liquid is poured onto polytetrafluoroethylene (PTFE) is closed, baking oven is put into and is reacted 10 hours at 200 DEG C.Deionization is used after being cooled to room temperature
It cleans up, is dried at 60 DEG C, obtain the monodisperse superparamagnetic ferriferrous oxide nano sphere (Fe of 500nm3O4)。
Embodiment 3
The present embodiment is specifically includes the following steps: the oxidation of 500nm monodisperse superparamagnetic four three prepared by 2g embodiment 2
Iron nanosphere is scattered in 350mL isopropanol and 100mL deionized water, and ultrasonic disperse 30 minutes, addition 6g tetraethyl orthosilicate,
γ-methacryloxypropyl trimethoxy silane of 2g and the acetic acid of 1mL, mechanical stirring are simultaneously heated to 60 DEG C, and reaction 6 is small
When, it is cleaned up after being cooled to room temperature with deionization and ethyl alcohol, is dried at 60 DEG C, obtain the monodisperse of the vinyl modified of 500nm
Superparamagnetic iron oxide nanosphere (Fe3O4@vinyl)。
Embodiment 4
The present embodiment is specifically includes the following steps: the monodisperse of 500nm vinyl modified prepared by 2g embodiment 3 is super suitable
Magnetic ferroferric oxide nanometer ball is scattered in acetonitrile, and 1.2g dibenzoyl peroxide, 2g N- vinyl-ε-acyl in oneself is added
Amine and 4g divinylbenzene are passed through nitrogen 30 minutes after mechanical stirring 30 minutes, then react 10 hours at 75 DEG C.It is cooling
It is cleaned up after to room temperature with deionization and ethyl alcohol, is dried at 60 DEG C, obtain 500nm N- vinyl-Epsilon-caprolactam and divinyl
The co-modified nanometer magnetic bead of base benzene.
Embodiment 5
The present embodiment is specifically includes the following steps: the monodisperse that 1.5g is implemented the 500nm vinyl modified of 3 preparations is super suitable
Magnetic ferroferric oxide nanometer ball is scattered in dioxane, and after ultrasonic disperse 30 minutes, the tertiary fourth of 2g peroxidating neopentanoic acid is added
Ester, 8g N- vinyl-Epsilon-caprolactam and 4g styrene and 2g divinylbenzene are passed through nitrogen after mechanical stirring 30 minutes
It 30 minutes, is reacted 20 hours at 70 DEG C.It is cleaned up after being cooled to room temperature with deionization and ethyl alcohol, dries, obtain at 60 DEG C
500nmN- vinyl-Epsilon-caprolactam, styrene and the co-modified nanometer magnetic bead of divinylbenzene.
Embodiment 6
The present embodiment is specifically includes the following steps: the monodisperse of 500nm vinyl modified prepared by 3g embodiment 3 is super suitable
Magnetic ferroferric oxide nanometer ball is scattered in acetone, and ultrasonic disperse 30 minutes, 2g tert-Butyl peroxypivalate, 8g is added
N- vinyl-Epsilon-caprolactam and 2g divinylbenzene are passed through nitrogen 30 minutes after mechanical stirring 30 minutes, anti-at 90 DEG C
It answers 6 hours.It is cleaned up after being cooled to room temperature with deionization and methanol, is dried at 60 DEG C, obtain 500nmN- vinyl-ε-in oneself
Amide and the co-modified nanometer magnetic bead of divinylbenzene.
Embodiment 7
The present embodiment is specifically includes the following steps: 1mL feminine gender urine sample addition 100 μ L, 5% ammonia spirit is uniformly mixed
It closes 10 minutes, different amounts of benzodiazepine * is addedClass pharmaceutical standards mixed liquor, and as the first row of 96 conventional orifice plates
In.The function of preparing from embodiment 6 that 400 μ L 50mg/mL are scattered in deionized water is added in secondary series in 96 orifice plates
Change nanometer magnetic bead suspension.The acetonitrile of 500 μ L is added in the 6th column of 96 orifice plates.It is 20 points that setting program parameter, which is adsorption time,
Clock, elution time are 5 minutes.It takes the 6th column eluted sample to be put into sample injection bottle, is detected by liquid chromatography mass combination.
Chromatographic parameter setting in the liquid chromatography mass combination are as follows:
Chromatographic column: Xterra MS C182.1x150mm, 3.5 μm (Waters company);
Mobile phase A: ammonium formate containing 5mmol/L, the deionized water of 10mmol/L ammonium carbonate and 0.05% formic acid;
Mobile phase B ammonium formate containing 5mmol/L, 20mmol/L ammonium carbonate, the acetonitrile of 0.05% formic acid and mixing for deionized water
It closes liquid (acetonitrile 96%, water 4%);It is flowed by 1 gradient of table.
Column temperature: 45 DEG C, flow velocity 0.2mL/min;Sample volume: 5 μ L.
Mass spectrometry parameters associated with the liquid chromatography mass are arranged are as follows:
Detection mode: MRM;Scanning mode: cation scans simultaneously;Electron spray voltage: 3200V;Source stabilization 115
℃;Collision gas: helium.MRM parameter is each medicament selection parent ion and daughter ion pair, and qualitative in conjunction with retention time, kurtosis is strong
Ion it is quantitative, detailed parameter is shown in Table 2.
Preferably, the third in step b) to the 5th column can put cleaning solution, it can the cleaning of three steps be realized, to different
For sample, urine specimen can be cleaned 0~2 time, and saliva sample cleans 1~2 time, and blood sample cleans 2~3 times, i.e. method
At most clean 3 times.It is further preferable that urine specimen is not cleaned, saliva sample is cleaned 1 time, and blood sample cleans 2 times.It is more excellent
Selection of land, the volume of cleaning solution are 500~1000 μ L.
Preferably, in the conventional bar magnet method self-reacting device in step b), for the instrument of commercialization, as English Rui Cheng is biochemical
The ETP32 and ETP300 of scientific and technological (Shanghai) Co., Ltd. are all 32 automation extraction apparatus, can once complete 32 parts of samples automatically
This extraction.It can certainly be 16 of other companies, 32,96 bar magnet method self-reacting devices.
Preferably, the eluting solvent in step b) is acetonitrile, acetone, methylene chloride, it is further preferable that eluting solvent is second
Nitrile.
The gradient of 1 mobile phase of table
Step | Time (min) | A% | B% | Curve |
1 | 0.00 | 90% | 10% | 1 |
2 | 1.00 | 80% | 20% | 6 |
3 | 4.00 | 40% | 60% | 6 |
4 | 10.00 | 30% | 70% | 6 |
5 | 16.00 | 60% | 40% | 6 |
6 | 18.50 | 95% | 5% | 6 |
2 benzodiazepine * of tableThe mass spectrum MRM parameter of class drug
It is determined as minimum quantitative detection limit, each benzene when daughter ion peak intensity signal-to-noise ratio (S/N)=10 lower with peak intensity
And phenodiazineThe detection of class drug is limited referring to table 3.Different amounts of benzodiazepine * is taken respectivelyClass pharmaceutical standards mixed liquor, blank urine
In be made into high and low 2 concentration sample carry out each concentration in a few days replication 5 times withinday precision, METHOD FOR CONTINUOUS DETERMINATION 3 days
Day to day precision the results are shown in Table 4.
Benzodiazepine * in 3 urine specimen of tableThe detection limit and linear relationship of class drug
Benzodiazepine * in 4 urine specimen of tableClass drug is in a few days and day to day precision
Embodiment 8
0.5mL saliva sample addition 0.5mL deionized water and 100 μ L, 5% ammonia spirit is taken uniformly to mix 10 minutes, and
As in the first row of 96 conventional orifice plates.Secondary series in 96 orifice plates is added 500 μ L 50mg/mL and disperses the sub- water of deionization
The functionalized nano bead suspension prepared from embodiment 5.The acetonitrile of 500 μ L is added as elution in the 6th column of 96 orifice plates
Liquid.Third column and the 4th column put 500 μ L cleaning solutions, and cleaning solution is 50mmol/L ammonium chloride-ammonia spirit of pH 10.5.Setting
Program parameter is that adsorption time is 20 minutes, and elution time is 10 minutes.It takes the 6th column eluted sample to be put into sample injection bottle, passes through
Liquid chromatography mass combination is detected.It is determined as most when daughter ion peak intensity signal-to-noise ratio (S/N)=10 lower with peak intensity
Low basis weight detection limit, each benzodiazepine *The detection of class drug is limited referring to table 5.
Benzodiazepine * in 5 saliva sample of tableThe detection limit and linear relationship of class drug
Above-mentioned specific implementation can by those skilled in the art under the premise of without departing substantially from the principle of the invention and objective with difference
Mode carry out local directed complete set to it, protection scope of the present invention is subject to claims and not by above-mentioned specific implementation institute
Limit, each implementation within its scope is by the constraint of the present invention.
Claims (10)
1. a kind of preparation method of monodisperse superparamagnetic nanometer magnetic bead, which is characterized in that by into iron particle solution successively
The kayexalate and sodium acetate as dispersing agent is added, heated reaction obtains monodisperse superparamagnetic ferroso-ferric oxide
Nanosphere;Then it is mixed with tetraethyl orthosilicate, γ-methacryloxypropyl trimethoxy silane and acetic acid with reality
Existing vinyl modified;Finally by modified magnetic ferroferric oxide nanometer ball and oil-soluble initiator, N- vinyl-ε-in oneself
Amide and vinyl benzene-like compounds react realization modification in a nitrogen environment, obtain monodisperse superparamagnetic nanometer magnetic bead.
2. according to the method described in claim 1, it is characterized in that, the iron particle solution be anhydrous ferric chloride glycol it is molten
Liquid, the glycol use ethylene glycol, dipropylene glycol, triethylene glycol, 1,2-PD, 1,2- hexylene glycol, 2- methyl-1,3- third
Glycol or combinations thereof.
3. according to the method described in claim 2, it is characterized in that, the quality of the dispersing agent is anhydrous chlorine in iron particle solution
Change the 40~90% of iron.
4. according to the method described in claim 1, it is characterized in that, the described heating reaction uses ptfe autoclave,
It is reacted 5~30 hours at 160~220 DEG C.
5. according to the method described in claim 1, it is characterized in that, the γ-methacryloxypropyl trimethoxy silicon
The quality of alkane is the 15~50% of tetraethyl orthosilicate quality.
6. according to the method described in claim 1, it is characterized in that, the oil-soluble initiator be peroxide initiator,
It is used: dibenzoyl peroxide, lauroyl peroxide, tert-Butyl peroxypivalate or perbenzoic acid.
7. according to the method described in claim 1, it is characterized in that, the vinyl benzene-like compounds use: 4- methoxybenzene
Ethylene, styrene, divinylbenzene, 3- chlorostyrene, α-methylstyrene, trans--Beta-methyl styrene, methyl 4- vinyl
Benzoic ether or combinations thereof.
8. method according to claim 1 or claim 7, characterized in that the N- vinyl-Epsilon-caprolactam and vinyl benzene
The mass ratio of class compound is 1:0.1~10.
9. a kind of monodisperse superparamagnetic nanometer magnetic bead, which is characterized in that any the method system according to claim 1~8
It is standby to obtain.
10. a kind of application for the nanometer magnetic bead being prepared based on the method any in claim 1~8, which is characterized in that
It is used for detection benzodiazepine *Class drug, specifically: body fluid to be measured is dissolved in ammonia spirit, above-mentioned be prepared into is added
The monodisperse superparamagnetic nanometer magnetic bead that arrives simultaneously surveys benzodiazepine * by liquid chromatography mass joint inspection after absorption and elutionClass
The content of drug.
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分散液相微萃取-气相色谱法检测尿中的三种苯并二氮杂类药物;张强等;《分析实验室》;20111231;全文 |
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