CN106546651A - A kind of preparation method of highly sensitive isocarboxazid molecular imprinting electrochemical sensor - Google Patents
A kind of preparation method of highly sensitive isocarboxazid molecular imprinting electrochemical sensor Download PDFInfo
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- CN106546651A CN106546651A CN201710015254.4A CN201710015254A CN106546651A CN 106546651 A CN106546651 A CN 106546651A CN 201710015254 A CN201710015254 A CN 201710015254A CN 106546651 A CN106546651 A CN 106546651A
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Abstract
The invention discloses a kind of preparation method of highly sensitive isocarboxazid molecular imprinting electrochemical sensor, with isocarboxazid as template molecule, resveratrol as function monomer, azodiisobutyronitrile as initiator, nickel based metal organic framework materials are as dopant, using obaculactone as cross-linking agent, a kind of highly sensitive isocarboxazid molecular imprinting electrochemical sensor is prepared for accordingly, the analysis method is simple and practical, overcomes the low shortcoming of conventional analysis method complexity, apparatus expensive, sensitivity.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, especially a kind of highly sensitive isocarboxazid molecular engram electricity
The preparation method of chemical sensor.
Background technology
Isocarboxazid (Isocarboxazid) indication：Isocarboxazid is non-selective monoamine oxidase inhibitor, with list
Amino oxidase A and B produce irreversibility combination, affect the metabolism of monoamine neurotransmitter.After monoamine oxidase, MAO is suppressed,
Nervus centraliss position monoamine content can be increased, antidepressant effect is played. it is main in central nerve inhibition, play the effect of calmness.But
As life-time service or excessive such medicine can cause hyperpyrexia and hypertensive crises, severe patient can lethal and kidney, hepatic insufficiency.
The method for determining isocarboxazid 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 to be different
Card ripple hydrazine detection method is 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 cross-linking agent and be allowed to enter with monomer
Row polyreaction 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 cross-linking 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 easily, a kind of highly sensitive different card
The preparation method of ripple hydrazine molecular imprinting electrochemical sensor.
To solve above-mentioned technical problem, the present invention is adopted the following technical scheme that：With isocarboxazid as template molecule, white hellebore
Alcohol is function monomer, azodiisobutyronitrile is initiator, nickel based metal organic framework materials are dopant, with obaculactone is
It is prepared by cross-linking agent.
A kind of preparation method of above-mentioned highly sensitive isocarboxazid molecular imprinting electrochemical sensor, with isocarboxazid be
Template molecule, resveratrol be function monomer, azodiisobutyronitrile be initiator, with obaculactone as cross-linking agent, azo two
Isopropyl cyanide is initiator, nickel based metal organic framework materials are dopant, forms a kind of Ni-based gold of hydridization in glassy carbon electrode surface
Category organic framework materials isocarboxazid molecular imprinting polymer membrane, template molecule elution is obtained final product.
A kind of preparation method of above-mentioned highly sensitive isocarboxazid molecular imprinting electrochemical sensor, including following step
Suddenly：
<1>With water be solvent compound concentration as 0.5mol/L nickel sulfate solution 10ml, with DMF
For solvent compound concentration for 0.05mol/L salicylic acid solution 50ml, then take the 10ml nickel sulfate solutions of preparation with 5 drops/
The speed of second is added drop-wise in the 50ml salicylic acid solutions of preparation, is stirred vigorously with 3000 revs/min of speed during Deca, 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
Methylformamide 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 nickel based metal organic framework materials material with outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, sequentially add 0.20mmol～0.65mmol template molecule isocarboxazid,
The function monomer resveratrol of 2.0mmol～9.0mmol, the cross-linking agent obaculactone of 3.0mmol, the initiator of 0.20mmol
Azodiisobutyronitrile and step<1>The nickel based metal organic framework materials 0.010g～0.060g of preparation, often adds a kind of chemistry
Reagent ultrasound wave dissolves 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 70 DEG C of vacuum drying oven, is then mixed using the acetonitrile and acetic acid of mol ratio 1: 2
Template molecule elution is obtained final product by solvent eluant.
Experiment find, with isocarboxazid as template molecule, resveratrol as function monomer, azodiisobutyronitrile be cause
Agent, nickel based metal organic framework materials are dopant, with the isocarboxazid molecular engram electricity that obaculactone is prepared as cross-linking agent
Chemical sensor, delicately can be used for determining the content of isocarboxazid very much.The electrification for determining isocarboxazid is set up using the present invention
Analysis method is learned, with especially outstanding sensitivity；The concentration of isocarboxazid is 2.2 × 10-8～1.8 × 10-4Mol/L scopes
Interior that good linear relationship (linearly dependent coefficient is R=0.9995) is presented, detection limit (S/N=3) is 2.5 × 10-9Mol/L,
Therefore, the isocarboxazid molecular imprinting electrochemical sensor of nickel based metal organic framework materials doping has higher sensitive
Degree, 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 isocarboxazid 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 dehydrated alcohol, be finally cleaned by ultrasonic with pure water clean.
2nd, the preparation of isocarboxazid molecular imprinting electrochemical sensor
<1>With water be solvent compound concentration as 0.5mol/L nickel sulfate solution 10ml, with DMF
For solvent compound concentration for 0.05mol/L salicylic acid solution 50ml, then take the 10ml nickel sulfate solutions of preparation with 5 drops/
The speed of second is added drop-wise in the 50ml salicylic acid solutions of preparation, is stirred vigorously with 3000 revs/min of speed during Deca, 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
Methylformamide 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 nickel based metal organic framework materials material with outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, 0.5mmol template molecule isocarboxazid, 3.0mmol resveratrols are sequentially added
Function monomer, the cross-linking agent obaculactone of 3.0mmol, the initiator azodiisobutyronitrile of 0.20mmol and step<1>Nickel
Base Metal organic framework materials 0.020g, often adds a kind of chemical reagent ultrasound 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 70 DEG C of vacuum drying oven, 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 isocarboxazid molecular imprinting electrochemical sensor electrode response characteristic is carried out with differential pulse voltammetry, is determined
The range of linearity and detection limit.The isocarboxazid molecular engram electrode is cultivated into 9 respectively in the isocarboxazid solution of variable concentrations
Minute, (bottom liquid was 5.0mmol/L K3[Fe(CN)6] -0.5mol/L pH=7.5 phosphate buffered solution solution), Ran Houjin
Row differential pulse voltammetry is measured.Isocarboxazid solution concentration is 2.2 × 10-8～1.8 × 10-4Present in the range of mol/L good
Linear relationship；Linear equation is Ip (μ A)=- 0.1112c (μm ol/L)+23.37, and linearly dependent coefficient is R=0.9995,
Detection limit (S/N=3) is 2.5 × 10-9mol/L。
Therefore, the isocarboxazid molecular engram sensor has higher sensitivity.
Claims (1)
1. a kind of preparation method of highly sensitive isocarboxazid molecular imprinting electrochemical sensor, it is characterised in that the sensor
It is prepared by the following method：The isocarboxazid of concentration 0.020mmol/mL～0.065mmol/ml is template molecule, concentration
The resveratrol of 0.20mmol/ml～0.90mmol/ml is function monomer, the azodiisobutyronitrile of concentration 0.02mmol/ml is
Initiator, the obaculactone of concentration 0.30mmol/ml are cross-linking agent, the Ni-based gold of concentration 0.0010g/ml～0.0060g/ml
Category organic framework materials are dopant, form a kind of hydridization nickel based metal organic framework materials isocarboxazid in glassy carbon electrode surface
Molecular imprinting polymer membrane, then using the acetonitrile and acetic acid mixed solvent eluted template molecule of eluant mol ratio 1: 2 be
；
Specifically carry out by following operation：
<1>With water be solvent compound concentration as 0.5mol/L nickel sulfate solution 10ml, with DMF as molten
Agent compound concentration is the salicylic acid solution 50ml of 0.05mol/L, then takes the 10ml nickel sulfate solutions of preparation with 5 drops/sec
Speed is added drop-wise in the 50ml salicylic acid solutions of preparation, is stirred vigorously with 3000 revs/min of speed during Deca, then in 100ml
Hot water kettle in reaction 11 hours is carried out at 118 DEG C, the precipitation of gained is collected by centrifugation after cooling, N, N- dimethyl methyls is respectively adopted
Amide and absolute ethanol washing 2 times, are collected by centrifugation precipitation, being deposited at 45 DEG C of collecting is vacuum dried, that is, is had
There are the nickel based metal organic framework materials of outstanding sensing capabilities；
<2>To in 10.0mL etoh solvents, sequentially add 0.20mmol～0.65mmol template molecule isocarboxazid,
The function monomer resveratrol of 2.0mmol～9.0mmol, the cross-linking agent obaculactone of 3.0mmol, the initiator of 0.20mmol
Azodiisobutyronitrile and step<1>The nickel based metal organic framework materials 0.010g～0.060g of preparation, often adds a kind of chemistry
Reagent ultrasound wave dissolves 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 70 DEG C of vacuum drying oven, then using the acetonitrile and acetic acid mixed solvent of mol ratio 1: 2
Template molecule elution is obtained final product by eluant.
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| CN105628762A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized silver nanoparticle-doped aniracetam MIECS (Molecular Imprinting Electrochemical Sensor) |
| 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) |
| 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 |
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2017
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| 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 |
| CN105628762A (en) * | 2016-01-04 | 2016-06-01 | 广西民族大学 | Preparation method of high-sensitivity functionalized silver nanoparticle-doped aniracetam MIECS (Molecular Imprinting Electrochemical Sensor) |
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Application publication date: 20170329 |