CN107957438A - A kind of preparation method of eszopiclone molecular imprinting electrochemical sensor - Google Patents
A kind of preparation method of eszopiclone molecular imprinting electrochemical sensor Download PDFInfo
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- CN107957438A CN107957438A CN201711253782.XA CN201711253782A CN107957438A CN 107957438 A CN107957438 A CN 107957438A CN 201711253782 A CN201711253782 A CN 201711253782A CN 107957438 A CN107957438 A CN 107957438A
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- eszopiclone
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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
Abstract
The invention discloses a kind of preparation method of eszopiclone molecular imprinting electrochemical sensor; using eszopiclone as template molecule, Oridonin be function monomer, azodiisobutyronitrile is initiator, nanoclay is dopant; crosslinking agent is used as to coumaric acyl tyrasamine so that N is trans; the eszopiclone molecular imprinting electrochemical sensor of highly sensitive nanoclay doping is prepared for accordingly; the analysis method is simple and practical, overcomes the shortcomings that conventional analysis method is complicated, equipment is expensive, sensitivity is low.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, especially a kind of eszopiclone molecular imprinting electrochemical sensing
The preparation method of device.
Background technology
Eszopiclone (Zopiclone) is a kind of hypnotic sedative agent, there is calmness, antianxiety, anticonvulsion and of flaccid muscles
Effect.Appropriate take this medicine can improve sleep, be good for your health, but for a long time or such medicine is excessively used can cause to medicine
The side effects such as injury gained in sports caused by thing sensitivity and cognitive ability damage, nausea and liver damage, therefore by most of in the world
Country is classified as controlled substance.
The method of measure eszopiclone has Gradient Elution method, reversed-phase high performance liquid chromatography-diode
Array Method and chromatography-mass spectroscopy on-line analysis method etc..But these methods are due to needing expensive instrument and equipment, there are it is of high cost,
The shortcomings of time-consuming, sensitivity is not high.Therefore, study a kind of high sensibility, easy eszopiclone assay method have it is non-
Often important meaning.
Molecular imprinting technology is using target molecule to be measured as template molecule, will be led to functional monomer complementary in structure
Cross covalently or non-covalently key and template molecule and combine to form monomer template molecular complex, add crosslinking agent be allowed to monomer into
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 complementary and with Multiple recognition site the sky with former microsphere space structure in the polymer
Cave.Current method is since the function monomer of selection cannot be properly matched with template molecule, and crosslinked rigidity is also poor,
Therefore sensitivity is not high.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of equipment it is simple, make a kind of easy eszopiclone molecule
The preparation method of trace electrochemical sensor.
In order to solve the above technical problems, the present invention adopts the following technical scheme that：Insulted by template molecule, winter of eszopiclone
Careless A prime is function monomer, azodiisobutyronitrile is initiator, nanometer is dopant, using N- it is trans-to coumaric acyl tyrasamine as
It is prepared by crosslinking agent.
The preparation method of above-mentioned a kind of eszopiclone molecular imprinting electrochemical sensor, using eszopiclone as template point
Son, Oridonin be function monomer, azodiisobutyronitrile be initiator, using N- it is trans-to coumaric acyl tyrasamine as crosslinking agent,
Nanoclay is dopant, and a kind of hybridized nanometer clay eszopiclone molecule print is formed in 2 mm glassy carbon electrode surfaces of diameter
Mark thin polymer film, then using eluant, eluent molar ratio 2:3 acetic acid and butanol mixed solvent are by template molecule elution, to obtain the final product.
A kind of preparation method of above-mentioned eszopiclone molecular imprinting electrochemical sensor, comprises the following steps：
<1>Into 10.0 mL etoh solvents, the mmol template molecules eszopiclone of 0.2 mmol~1.0,1.0 are sequentially added
The mmol function monomers Oridonin of mmol~5.0,2.5 mmol crosslinking agents N- are trans-to coumaric acyl tyrasamine, 0.1
The nanoclay of the g of mmol initiator azodiisobutyronitriles and 0.0100 g~0.0400, often adds a kind of chemical reagent ultrasonic wave
Dissolving 9 minutes；
<2>Take step<1>6 μ L of mixture be applied in the glassy carbon electrode surface of clean smooth a diameter of 2 mm, it is small to place 6
Shi Hou, when the electrode after modification is placed in thermal polymerization 1.5 is small in 80 DEG C of vacuum drying chamber, then using eluant, eluent molar ratio
For 2:3 acetic acid and butanol mixed solvent are by template molecule elution, to obtain the final product.
Research finds, is function monomer using eszopiclone as template molecule, Oridonin, azodiisobutyronitrile is draws
It is dopant to send out agent, nanoclay, using N- it is trans-the eszopiclone molecular engram that is prepared to coumaric acyl tyrasamine as crosslinking agent
Electrochemical sensor, the content available for measure eszopiclone.The electrochemistry for measuring eszopiclone is established using the present invention
Analysis method, has very outstanding sensitivity；The concentration of eszopiclone is 2.0 × 10-8 ~ 1.6×10-4Mol/L scopes
The good linear relationship (linearly dependent coefficient is R=0.9988) of interior presentation, detection limit (S/N=3) it is 1.8 × 10-9 mol/
L, therefore, the eszopiclone molecular imprinting electrochemical sensor of nanoclay doping have higher sensitivity, more than current
Detection method；And equipment is simple, it is simple to make.
Brief description of the drawings
Fig. 1 is a kind of working curve of the preparation method of eszopiclone molecular imprinting electrochemical sensor in embodiment 1
Figure.
Embodiment
Embodiment 1
First, the processing 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 body
Product is than being 1:8 min of ultrasound in 1 nitric acid, place into 8 min of ultrasound in absolute ethyl alcohol, are finally cleaned by ultrasonic with pure water clean.
2nd, the preparation of eszopiclone molecular imprinting electrochemical sensor
<1>Into 10.0 mL etoh solvents, 0.5 mmol template molecules eszopiclone, 2.5 mmol function lists are sequentially added
Body Oridonin, 2.5 mmol crosslinking agents N- are trans-to coumaric acyl tyrasamine, 0.1 mmol initiator azodiisobutyronitriles
And 0.0200 g nanoclay, often add a kind of chemical reagent ultrasonic wave and dissolve 9 minutes；
<2>Take step<1>6 μ L of mixture be applied in the glassy carbon electrode surface of clean smooth a diameter of 2 mm, it is small to place 6
Shi Hou, when the electrode after modification is placed in thermal polymerization 1.5 is small in 80 DEG C of vacuum drying chamber, then using eluant, eluent molar ratio
2:3 acetic acid and butanol mixed solvent are by template molecule elution, by magnetic agitation eluted template molecule, until being detected in eluent
Less than template molecule, then the solvent of trace electrode surface is washed away with ultra-pure water, then trace electrode is stored in ultra-pure water and is treated
With.
3rd, the measure of the drafting of working curve and detection limit
The experiment of the eszopiclone molecular engram electrode response characteristic of nanoclay doping is carried out with differential pulse voltammetry, is surveyed
Constant linear scope and detection limit.By the eszopiclone molecular engram electrode of nanoclay doping respectively in the right assistant of various concentrations
Clone solution in cultivate 6 minutes（Bottom liquid is 5.0 mmol/L K3[Fe(CN)6] -0.5 mol/L pH=7.5 phosphate
Buffer solution solution）, then carry out differential pulse voltammetry measurement.Eszopiclone solution concentration is 2.0 × 10-8 ~ 1.6×
10-4Good linear relationship is presented in the range of mol/L；Linear equation isIp(μA) = -0.1137 с (μmol/L) +
23.44, linearly dependent coefficient is R=0.9988, detection limit (S/N=3) it is 1.8 × 10-9 mol/L。
Therefore, the eszopiclone molecular engram electrode of nanoclay doping has high sensitivity.
Claims (1)
- A kind of 1. preparation method of eszopiclone molecular imprinting electrochemical sensor, it is characterised in that with 0.02 mmol/mL~ The eszopiclone of 0.10 mmol/mL is template molecule, the Oridonin of the mmol/mL of 0.10 mmol/mL~0.50 is work( Can monomer, 0.01 mmol/mL azodiisobutyronitrile for initiator, with the N- of 0.25 mmol/mL it is trans-to coumaric acyl junket Amine is crosslinking agent, the g/mL nanoclays of 0.0010 g/mL~0.0040 are dopant, is formed in glassy carbon electrode surface a kind of Hybridized nanometer clay eszopiclone molecular imprinting polymer membrane, is then eluted using eluant, eluent acetic acid and butanol mixed solvent Template molecule to obtain the final product；Specifically carried out by following operation：<1>Into 10.0 mL etoh solvents, the mmol template molecules eszopiclone of 0.2 mmol~1.0,1.0 are sequentially added The mmol function monomers Oridonin of mmol~5.0,2.5 mmol crosslinking agents N- are trans-to coumaric acyl tyrasamine, 0.1 The nanoclay of the g of mmol initiator azodiisobutyronitriles and 0.0100 g~0.0400, often adds a kind of chemical reagent ultrasonic wave Dissolving 9 minutes；<2>Take step<1>6 μ L of mixture be applied in the glassy carbon electrode surface of clean smooth a diameter of 2 mm, it is small to place 6 Shi Hou, when the electrode after modification is placed in thermal polymerization 1.5 is small in 80 DEG C of vacuum drying chamber, then using eluant, eluent molar ratio For 2:3 acetic acid and butanol mixed solvent are by template molecule elution, to obtain the final product.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105510415A (en) * | 2016-01-04 | 2016-04-20 | 广西民族大学 | Preparation method for high-sensitivity functionalized gold nanoparticle-doped meprobamate molecularly-imprinted electrochemical sensor |
| CN105548298A (en) * | 2015-12-21 | 2016-05-04 | 广西民族大学 | Method for preparing high-sensitivity nano-zirconia-doped dezocine molecular imprinting electrochemical sensor |
| CN105548310A (en) * | 2015-12-21 | 2016-05-04 | 广西民族大学 | Method for preparing high-sensitivity nano-zirconia-doped pafenolol 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) |
-
2017
- 2017-12-02 CN CN201711253782.XA patent/CN107957438A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105548298A (en) * | 2015-12-21 | 2016-05-04 | 广西民族大学 | Method for preparing high-sensitivity nano-zirconia-doped dezocine molecular imprinting electrochemical sensor |
| CN105548310A (en) * | 2015-12-21 | 2016-05-04 | 广西民族大学 | Method for preparing high-sensitivity nano-zirconia-doped pafenolol molecular imprinting electrochemical sensor |
| CN105510415A (en) * | 2016-01-04 | 2016-04-20 | 广西民族大学 | Preparation method for high-sensitivity functionalized gold nanoparticle-doped meprobamate molecularly-imprinted 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) |
Non-Patent Citations (1)
| Title |
|---|
| ZHANG, FU ET AL.: "Molecularly imprinted polymer doped with Hectorite for selective recognition of sinomenine hydrochloride", 《JOURNAL OF BIOMATERIALS SCIENCE. POLYMER EDITION》 * |
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