CN106525937A - Preparation method of high-sensitivity amoxapine molecularly imprinted electrochemical sensor - Google Patents
Preparation method of high-sensitivity amoxapine molecularly imprinted electrochemical sensor Download PDFInfo
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- CN106525937A CN106525937A CN201710014737.2A CN201710014737A CN106525937A CN 106525937 A CN106525937 A CN 106525937A CN 201710014737 A CN201710014737 A CN 201710014737A CN 106525937 A CN106525937 A CN 106525937A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
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- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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Abstract
The invention discloses a preparation method of a high-sensitivity amoxapine molecularly imprinted electrochemical sensor. The high-sensitivity amoxapine molecularly imprinted electrochemical sensor is prepared by using amoxapine as a template molecule, gentiopicrin as a functional monomer, azodiisobutyronitrile as an initiator, a copper-base metal organic framework material as a dopant and isoalantolactone as a crosslinking agent. The analysis method is simple and practical, and overcomes the defects of high complexity, expensive equipment and low sensitivity in the past analysis methods.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, especially a kind of highly sensitive amoxapine molecular engram electricity
The preparation method of chemical sensor.
Background technology
Amoxapine (Amoxapine) is antidepressants, compared with imipramine, with similar antidepressant effect, but is risen
Effect is fast, and low to cardiac toxic, cholinolytic effect is weak with sedation.But as Long-Time Service or excessive such medicine can be caused
The heart, kidney, dyshepatia, or even myocardial infarction.
The method for determining amoxapine has high performance liquid chromatography, application of gas chromatorgraphy/mass method etc..But these methods are due to needing
Expensive instrument and equipment, exist high cost, time-consuming, it is sensitive not high the shortcomings of.Therefore, study a kind of high sensibility, easy Ah
Sapin detection method is not significant.
Molecular imprinting is, with target molecule to be measured as template molecule, will to lead to functional monomer complementary in structure
Cross covalently or non-covalently key and monomer template molecular complex is combined to form with template molecule, add crosslinking agent and be allowed to enter with monomer
Row polymerisation forms template molecule polymer, by either physically or chemically removing template molecule after the completion of reaction, is divided
Sub- imprinted polymer, forms and sky with multiple action site complementary with former microsphere space structure in the polymer
Cave.Current method is incorrect as the function monomer for selecting is matched with template molecule and crosslinking agent, and the rigidity being crosslinked
It is poor, therefore sensitivity is not high.
The content of the invention
The technical problem to be solved in the present invention is to provide that a kind of equipment is simple, make easy, a kind of highly sensitive Ah not
The preparation method of sapin molecular imprinting electrochemical sensor.
To solve above-mentioned technical problem, the present invention is adopted the following technical scheme that：With amoxapine as template molecule, rough gentian it is bitter
Glycosides is function monomer, azodiisobutyronitrile is initiator, copper base metal organic framework materials are dopant, with isoalantolactone
Prepare for crosslinking agent.
A kind of preparation method of above-mentioned highly sensitive amoxapine molecular imprinting electrochemical sensor, with amoxapine be
Template molecule, gentiamarin be function monomer, azodiisobutyronitrile be initiator, with isoalantolactone as crosslinking agent, azo
Bis-isobutyronitrile is initiator, copper base metal organic framework materials are dopant, forms a kind of hydridization in glassy carbon electrode surface copper-based
Metal-organic framework material amoxapine molecular imprinting polymer membrane, template molecule elution is obtained final product.
A kind of preparation method of above-mentioned highly sensitive amoxapine molecular imprinting electrochemical sensor, including following step
Suddenly：
<1>With water be solvent compound concentration as 0.5mol/L copper sulfate solution 10ml, with DMF
For molten
Trimesic acid solution 50ml of the agent compound concentration for 0.05mol/L, the 10ml copper sulphate for then taking preparation are water-soluble
Liquid is added drop-wise in the 50ml benzenetricarboxylic acid solution of preparation with 5 drops/sec of speed, violent with 3000 revs/min of speed during dropwise addition
Stirring, then 118 DEG C in the hot water kettle of 100ml at carry out reaction 11 hours, be collected by centrifugation after cooling gained precipitation, adopt respectively
With DMF and absolute ethanol washing 2 times, precipitation is collected by centrifugation, being deposited at 45 DEG C of collecting is carried out into vacuum
It is dried, that is, obtains the copper base metal organic framework materials with outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, sequentially add 0.30mmol～0.80mmol template molecule amoxapine,
The function monomer gentiamarin of 3.0mmol～8.0mmol, the crosslinking agent isoalantolactone of 1.0mmol, the initiation of 0.10mmol
Agent azodiisobutyronitrile and step<1>The copper base metal organic framework materials 0.020g～0.050g of preparation, often adds one kindization
Learn reagent ultrasonic wave to dissolve 5 minutes；
<3>Take step<2>9 μ L of mixture be applied to clean smooth glassy carbon electrode surface, after placing 8 hours, will modification
Electrode afterwards is placed in thermal polymerization 2.0 hours in 75 DEG C of vacuum drying chamber, is then mixed using the acetonitrile and acetic acid of mol ratio 1: 2
Template molecule elution is obtained final product by solvent eluant, eluent.
Experiment find, with amoxapine as template molecule, gentiamarin as function monomer, azodiisobutyronitrile be cause
Agent, copper base metal organic framework materials are dopant, with the amoxapine molecular engram that isoalantolactone is prepared as crosslinking agent
Electrochemical sensor, delicately can be used for determining the content of amoxapine very much.The electricity for determining amoxapine is set up using the present invention
Chemical analysis method, with especially outstanding sensitivity；The concentration of amoxapine is 1.5 × 10-8～1.8 × 10-4Mol/L models
The good linear relationship (linearly dependent coefficient is R=0.9998) of interior presentation is enclosed, detection limit (S/N=3) is 2.5 × 10-9mol/
L, therefore, the amoxapine molecular imprinting electrochemical sensor has higher sensitivity, more than current detection method, and
Equipment is simple, make easy.
Description of the drawings
Fig. 1 is a kind of preparation method of highly sensitive amoxapine molecular imprinting electrochemical sensor in embodiment 1
Working curve diagram.
Specific embodiment
Embodiment 1
First, the process of glass-carbon electrode
Glass-carbon electrode is polished with 1.0 μm, 0.3 μm and 0.05 μm of alumina powder on polishing cloth successively, is then placed in
Volume ratio be 1: 1 nitric acid in ultrasound 6min, place into ultrasound 6min in absolute ethyl alcohol, be finally cleaned by ultrasonic with pure water clean.
2nd, the preparation of amoxapine molecular imprinting electrochemical sensor
<1>With water be solvent compound concentration as 0.5mol/L copper sulfate solution 10ml, with DMF
Be the trimesic acid solution 50ml of 0.05mol/L for solvent compound concentration, the 10ml copper sulfate solutions of preparation are then taken with 5
Drop/sec speed be added drop-wise in the 50ml benzenetricarboxylic acid solution of preparation, be stirred vigorously with 3000 revs/min of speed during dropwise addition,
Again 118 DEG C in the hot water kettle of 100ml at carry out reaction 11 hours, be collected by centrifugation after cooling gained precipitation, N is respectively adopted,
Dinethylformamide and absolute ethanol washing 2 times, are collected by centrifugation precipitation, being deposited at 45 DEG C of collecting is carried out vacuum and is done
It is dry, that is, obtain the copper base metal organic framework materials with outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, 0.6mmol template molecule amoxapines, 5.0mmol gentiamarins are sequentially added
Function monomer, the crosslinking agent isoalantolactone of 1.0mmol, the initiator azodiisobutyronitrile of 0.10mmol and step<1>'s
Copper base metal organic framework materials 0.050g, often adds a kind of chemical reagent ultrasonic wave to dissolve 5 minutes；
<3>Take step<2>9 μ L of mixture be applied to clean smooth glassy carbon electrode surface, after placing 8 hours, will modification
Electrode afterwards is placed in thermal polymerization 2.0 hours in 75 DEG C of vacuum drying chamber, then using 1: 2 acetonitrile and acetic acid mixtures of eluents
By template molecule elution, by magnetic agitation eluted template molecule, until can not detect template molecule in eluent, then with ultrapure
The solvent acetonitrile and acetic acid of trace electrode surface is removed in washing, is then stored in trace electrode stand-by in ultra-pure water.
3rd, the measure of the drafting of working curve and detection limit
The experiment of amoxapine molecular imprinting electrochemical sensor electrode response characteristic is carried out with differential pulse voltammetry, is determined
The range of linearity and detection limit.By 8 points of the cultivation in the amoxapine solution of variable concentrations respectively of amoxapine molecular engram electrode
(bottom liquid is 5.0mmol/L K to clock3[Fe(CN)6] -0.5mol/L pH=7.5 PBS solution), then carry out
Differential pulse voltammetry is measured.Amoxapine solution concentration is 1.5 × 10-8～1.8 × 10-4Present in the range of mol/L good
Linear relationship；Linear equation is Ip (μ A)=- 0.1011c (μm ol/L)+23.17, and linearly dependent coefficient is R=0.9998, inspection
Rising limit (S/N=3) is 2.5 × 10-9mol/L。
Therefore, the amoxapine molecular engram sensor has higher sensitivity.
Claims (1)
1. a kind of preparation method of highly sensitive amoxapine molecular imprinting electrochemical sensor, it is characterised in that the sensor
It is prepared by the following method：The amoxapine of concentration 0.030mmol/mL～0.080mmol/ml is template molecule, concentration
The gentiamarin of 0.30mmol/ml～0.80mmol/ml is function monomer, the azodiisobutyronitrile of concentration 0.01mmol/ml is
Initiator, the isoalantolactone of concentration 0.10mmol/ml are the copper gold of crosslinking agent, concentration 0.0020g/ml～0.0050g/ml
Category organic framework materials are dopant, form a kind of hydridization copper base metal organic framework materials amoxapine in glassy carbon electrode surface
Molecular imprinting polymer membrane, then using the acetonitrile and acetic acid mixed solvent eluted template molecule of eluant, eluent mol ratio 1: 2 be
；
Specifically carry out by following operation：
<1>With water be solvent compound concentration as 0.5mol/L copper sulfate solution 10ml, with DMF as molten
Trimesic acid solution 50ml of the agent compound concentration for 0.05mol/L, then take the 10ml copper sulfate solutions of preparation with 5 drops/
The speed of second is added drop-wise in the 50ml benzenetricarboxylic acid solution of preparation, is stirred vigorously with 3000 revs/min of speed during dropwise addition, then
Reaction 11 hours is carried out at 118 DEG C in the hot water kettle of 100ml, the precipitation of gained is collected by centrifugation after cooling, N, N- bis- is respectively adopted
NMF and absolute ethanol washing 2 times, are collected by centrifugation precipitation, being deposited at 45 DEG C of collecting are vacuum dried, i.e.,
Obtain the copper base metal organic framework materials with outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, sequentially add 0.30mmol～0.80mmol template molecule amoxapine,
The function monomer gentiamarin of 3.0mmol～8.0mmol, the crosslinking agent isoalantolactone of 1.0mmol, the initiation of 0.10mmol
Agent azodiisobutyronitrile and step<1>The copper base metal organic framework materials 0.020g～0.050g of preparation, often adds one kindization
Learn reagent ultrasonic wave to dissolve 5 minutes；
<3>Take step<2>9 μ L of mixture be applied to clean smooth glassy carbon electrode surface, after placing 8 hours, after modification
Electrode is placed in thermal polymerization 2.0 hours in 75 DEG C of vacuum drying chamber, then using the acetonitrile and acetic acid mixed solvent of mol ratio 1: 2
Template molecule elution is obtained final product by eluant, eluent.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898566A (en) * | 2011-07-28 | 2013-01-30 | 天津科技大学 | Preparation method of metal organic framework molecularly imprinted polymer used for enriching trace amounts of Metolcarb |
| CN104014320A (en) * | 2014-06-19 | 2014-09-03 | 天津科技大学 | Aqueous phase metal organic framework molecular imprinting material of enriched trace meta-tolyl-N-methylcarbamate (MTMC) |
| CN104844762A (en) * | 2015-05-22 | 2015-08-19 | 天津科技大学 | Preparation method for thermo-sensitive type molecularly imprinted polymer with metal frame |
| CN105628777A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized gold nanoparticle-doped phenprobamate MIECS (Molecular Imprinting Electrochemical Sensor) |
| CN105628775A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized silver nanoparticle-doped keppra MIECS (Molecular Imprinting Electrochemical Sensor) |
| CN106198701A (en) * | 2016-08-18 | 2016-12-07 | 济南大学 | A kind of metal-organic framework material area load molecular imprinted polymer membrane is for the electrochemical detection method of orthene |
-
2017
- 2017-01-09 CN CN201710014737.2A patent/CN106525937A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898566A (en) * | 2011-07-28 | 2013-01-30 | 天津科技大学 | Preparation method of metal organic framework molecularly imprinted polymer used for enriching trace amounts of Metolcarb |
| CN104014320A (en) * | 2014-06-19 | 2014-09-03 | 天津科技大学 | Aqueous phase metal organic framework molecular imprinting material of enriched trace meta-tolyl-N-methylcarbamate (MTMC) |
| CN104844762A (en) * | 2015-05-22 | 2015-08-19 | 天津科技大学 | Preparation method for thermo-sensitive type molecularly imprinted polymer with metal frame |
| CN105628777A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized gold nanoparticle-doped phenprobamate MIECS (Molecular Imprinting Electrochemical Sensor) |
| CN105628775A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized silver nanoparticle-doped keppra MIECS (Molecular Imprinting Electrochemical Sensor) |
| CN106198701A (en) * | 2016-08-18 | 2016-12-07 | 济南大学 | A kind of metal-organic framework material area load molecular imprinted polymer membrane is for the electrochemical detection method of orthene |
Non-Patent Citations (3)
| Title |
|---|
| JIAN ZHOU等: "The Cu-MOF-199/single-walled carbon nanotubes modified electrode for simultaneous determination of hydroquinone and catechol with extended linear ranges and lower detection limits", 《ANALYTICA CHIMICA ACTA》 * |
| ZHENGANG GUO 等: "Electrochemical performance of graphene and copper oxide composites synthesized from a metal–organic framework (Cu-MOF)", 《RSC ADVANCES》 * |
| 王迎进 等: "龙胆苦苷与人血清白蛋白作用机制", 《计算机与应用化学》 * |
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Application publication date: 20170322 |