CN106802312A - A kind of preparation method of highly sensitive Moclobemide molecular imprinting electrochemical sensor - Google Patents
A kind of preparation method of highly sensitive Moclobemide molecular imprinting electrochemical sensor Download PDFInfo
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- CN106802312A CN106802312A CN201710015251.0A CN201710015251A CN106802312A CN 106802312 A CN106802312 A CN 106802312A CN 201710015251 A CN201710015251 A CN 201710015251A CN 106802312 A CN106802312 A CN 106802312A
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Abstract
The invention discloses a kind of preparation method of highly sensitive Moclobemide molecular imprinting electrochemical sensor, with Moclobemide as template molecule, resveratrol as function monomer, azodiisobutyronitrile as initiator, nickel based metal organic framework materials are as dopant, using evodin as crosslinking agent, a kind of highly sensitive Moclobemide 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 Moclobemide molecular engram electricity
The preparation method of chemical sensor.
Background technology
Moclobemide (Moclobemide) indication：Moclobemide is MAOI class antidepressants, its work
With being by reversible inhibition intracerebral A MAO-B Bs, so as to improve intracerebral norepinephrine, dopamine and serotonin
Level, play antidepressant effect, it is fast with effect, the characteristics of activity of monoamine oxidase recovers fast after drug withdrawal.But due to long-term
Using or excessive such medicine can cause mild nausea, headache, perspiration, palpitaition, insomnia, postural hypotension etc..It is heavy dose of
Shi Keneng induces epilepsy, and severe patient can lethal and kidney, liver function hepatic disorder.
The method for determining Moclobemide 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, a kind of high sensibility, easy is studied
Clofibride detection method is significant.
Molecular imprinting technology 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 combine to form monomer template molecular complex 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 with the complementation of former microsphere space structure and with the sky in multiple action site in the polymer
Cave.Current method is incorrect because 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 easily, a kind of highly sensitive chlorine
The preparation method of shellfish amine molecule trace electrochemical sensor.
In order to solve the above technical problems, the present invention is adopted the following technical scheme that：With Moclobemide as template molecule, white black false hellebore
Alcohol is function monomer, azodiisobutyronitrile is initiator, nickel based metal organic framework materials are dopant, is with evodin
It is prepared by crosslinking agent.
A kind of preparation method of above-mentioned highly sensitive Moclobemide molecular imprinting electrochemical sensor, be with Moclobemide
Template molecule, resveratrol be function monomer, azodiisobutyronitrile be initiator, with evodin as crosslinking agent, azo two
Isobutyronitrile is initiator, nickel based metal organic framework materials are dopant, and a kind of Ni-based gold of hydridization is formed in glassy carbon electrode surface
Category organic framework materials Moclobemide molecular imprinting polymer membrane, template molecule elution is obtained final product.
A kind of preparation method of above-mentioned highly sensitive Moclobemide 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
Be solvent compound concentration for 0.05mol/L salicylic acid solution 50ml, then take the 10ml nickel sulfate solutions of preparation with 5 drop/
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 dropwise addition, then
Reaction 11 hours is carried out in the hot water kettle of 100ml at 118 DEG C, 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 nickel based metal organic framework materials with outstanding sensing capabilities；
<2>In to 10.0mL etoh solvents, sequentially add 0.20mmol~0.90mmol template molecule Moclobemide,
The function monomer resveratrol of 2.0mmol~9.0mmol, the crosslinking agent evodin of 2.0mmol, the initiator of 0.30mmol
Azodiisobutyronitrile and step<1>The nickel based metal organic framework materials 0.010g~0.080g of preparation, often adds a kind of chemistry
Reagent ultrasonic wave dissolves 5 minutes；
<3>Take step<2>The μ L of mixture 9 be applied to clean smooth glassy carbon electrode surface, after placing 8 hours, will modify
Electrode afterwards is placed in thermal polymerization 2.0 hours in 70 DEG C of vacuum drying chamber, is then mixed using the acetonitrile and acetic acid of mol ratio 1: 2
Solvent eluant, eluent obtains final product template molecule elution.
Experiment find, with Moclobemide as template molecule, resveratrol as function monomer, azodiisobutyronitrile for trigger
Agent, nickel based metal organic framework materials are dopant, with the Moclobemide molecular engram electricity that evodin is prepared as crosslinking agent
Chemical sensor, delicately can be used to determine the content of Moclobemide very much.The electrification for determining Moclobemide is set up using the present invention
Analysis method is learned, with especially outstanding sensitivity；The concentration of Moclobemide is 2.0 × 10-8~2.0 × 10-4Mol/L scopes
Interior that good linear relationship (linearly dependent coefficient is R=0.9992) is presented, detection limit (S/N=3) is 1.5 × 10-9Mol/L,
Therefore, the Moclobemide molecular imprinting electrochemical sensor has sensitivity higher, more than current detection method；And set
Standby simple, making is easy.
Brief description of the drawings
Fig. 1 is a kind of preparation method of highly sensitive Moclobemide molecular imprinting electrochemical sensor in embodiment 1
Working curve diagram.
Specific embodiment
Embodiment 1
First, the treatment of glass-carbon electrode
Glass-carbon electrode is polished with 1.0 μm, 0.3 μm and 0.05 μm of alumina powder successively on polishing cloth, 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 Moclobemide molecular imprinting electrochemical sensor
<1>With water be solvent compound concentration as 0.5mol/L nickel sulfate solution 10ml, with DMF
Be solvent compound concentration for 0.05mol/L salicylic acid solution 50ml, then take the 10ml nickel sulfate solutions of preparation with 5 drop/
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 dropwise addition, then
Reaction 11 hours is carried out in the hot water kettle of 100ml at 118 DEG C, 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 nickel based metal organic framework materials material with outstanding sensing capabilities；
<2>In to 10.0mL etoh solvents, 0.5mmol template molecules Moclobemide, 3.0mmol resveratrols are sequentially added
Function monomer, the crosslinking agent evodin of 2.0mmol, the initiator azodiisobutyronitrile and step of 0.30mmol<1>Nickel
Base Metal organic framework materials 0.020g, often adds a kind of chemical reagent ultrasonic wave to dissolve 5 minutes；
<3>Take step<2>The μ L of mixture 9 be applied to clean smooth glassy carbon electrode surface, after placing 8 hours, will modify
Electrode afterwards is placed in thermal polymerization 2.0 hours in 70 DEG C of vacuum drying chamber, then the acetonitrile and acetic acid mixtures of eluents using 1: 2
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 are removed in washing, are 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 Moclobemide molecular imprinting electrochemical sensor electrode response characteristic is carried out with differential pulse voltammetry, is determined
The range of linearity and detection limit.Moclobemide molecular engram electrode is cultivated 9 points in the Moclobemide solution of various concentrations respectively
(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.Moclobemide solution concentration is 2.0 × 10-8~2.0 × 10-4Presented in the range of mol/L good
Linear relationship；Linear equation is Ip (μ A)=- 0.1027c (μm ol/L)+23.28, and linearly dependent coefficient is R=0.9992, inspection
Rising limit (S/N=3) is 1.5 × 10-9mol/L。
Therefore, the Moclobemide molecular engram sensor has sensitivity higher.
Claims (1)
1. a kind of preparation method of highly sensitive Moclobemide molecular imprinting electrochemical sensor, it is characterised in that the sensor
It is prepared by the following method：The Moclobemide of concentration 0.020mmol/mL~0.090mmol/ml is template molecule, concentration
The resveratrol of 0.20mmol/ml~0.90mmol/ml is function monomer, the azodiisobutyronitrile of concentration 0.03mmol/ml is
Initiator, the evodin of concentration 0.20mmol/ml are crosslinking agent, the Ni-based gold of concentration 0.0010g/ml~0.0080g/ml
Category organic framework materials are dopant, and a kind of hydridization nickel based metal organic framework materials Moclobemide is formed in glassy carbon electrode surface
Molecular imprinting polymer membrane, be then using the acetonitrile and acetic acid mixed solvent eluted template molecule of eluant, eluent mol ratio 1: 2
；
Specifically carried 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 dropwise addition, 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
Acid amides and absolute ethanol washing 2 times, are collected by centrifugation precipitation, and being deposited at 45 DEG C of collecting is vacuum dried, that is, had
There are the nickel based metal organic framework materials of outstanding sensing capabilities；
<2>In to 10.0mL etoh solvents, sequentially add 0.20mmol~0.90mmol template molecule Moclobemide,
The function monomer resveratrol of 2.0mmol~9.0mmol, the crosslinking agent evodin of 2.0mmol, the initiator of 0.30mmol
Azodiisobutyronitrile and step<1>The nickel based metal organic framework materials 0.010g~0.080g of preparation, often adds a kind of chemistry
Reagent ultrasonic wave dissolves 5 minutes；
<3>Take step<2>The μ L of mixture 9 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 chamber, then using the acetonitrile and acetic acid mixed solvent of mol ratio 1: 2
Eluant, eluent obtains final product template molecule elution.
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Citations (5)
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| CN103086867A (en) * | 2011-10-27 | 2013-05-08 | 中国科学院大连化学物理研究所 | Nickel base micropore material and preparation method thereof |
| CN103926287A (en) * | 2014-04-25 | 2014-07-16 | 广西民族大学 | Nano cobaltous oxide-doped minocycline hydrochloride molecular imprinting electrochemical sensor with high sensitivity and preparation method thereof |
| CN105566654A (en) * | 2016-01-28 | 2016-05-11 | 浙江省肿瘤医院 | One-dimensional structure metal-organic framework compound and preparation method thereof |
| 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 |
-
2017
- 2017-01-09 CN CN201710015251.0A patent/CN106802312A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN103086867A (en) * | 2011-10-27 | 2013-05-08 | 中国科学院大连化学物理研究所 | Nickel base micropore material and preparation method thereof |
| CN103926287A (en) * | 2014-04-25 | 2014-07-16 | 广西民族大学 | Nano cobaltous oxide-doped minocycline hydrochloride molecular imprinting electrochemical sensor with high sensitivity and preparation method thereof |
| 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) |
| CN105566654A (en) * | 2016-01-28 | 2016-05-11 | 浙江省肿瘤医院 | One-dimensional structure metal-organic framework compound and preparation method thereof |
| 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 (2)
| Title |
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| ZHENZHONG GUO, ET AL.: "Molecularly Imprinted Polymer/Metal Organic Framework Based Chemical Sensors", 《COATINGS》 * |
| 朱荣华 等: "高效液相色谱法测定人血清中吗氯贝胺浓度", 《中国临床药理学杂志》 * |
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