CN105548310A - Method for preparing high-sensitivity nano-zirconia-doped pafenolol molecular imprinting electrochemical sensor - Google Patents
Method for preparing high-sensitivity nano-zirconia-doped pafenolol molecular imprinting electrochemical sensor Download PDFInfo
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- CN105548310A CN105548310A CN201510956258.3A CN201510956258A CN105548310A CN 105548310 A CN105548310 A CN 105548310A CN 201510956258 A CN201510956258 A CN 201510956258A CN 105548310 A CN105548310 A CN 105548310A
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- pafenolol
- template molecule
- molecular imprinting
- electrochemical sensor
- zirconia
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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
- G01N27/28—Electrolytic cell components
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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
Abstract
The present invention discloses a method for preparing a high-sensitivity nano-zirconia-doped pafenolol molecular imprinting electrochemical sensor, the high-sensitivity nano-zirconia-doped pafenolol molecular imprinting electrochemical sensor is prepared by use of pafenolol as a template molecule, (5s, 8s)-3-(4'-chloro-3'-fluoro-4-vinyl-biphenyl-3-yl)-4-hydroxy-8-ethyoxyl-1-aza-spiro [4.5] dec-3-ene-2-one as a single function monomer, azobisisobutyronitrile as an initiator, nano-zirconia as a dopant and maleic rosin ethylene glycol acrylate as a crosslinking agent, wherein the maleic rosin ethylene glycol acrylate is prepared from rosin as a raw material, and the method is simple and practical, and overcomes the shortcomings that a conventional analysis method is complicated, expensive in equipment, and low in sensitivity.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, especially a kind of preparation method of pafenolol molecular imprinting electrochemical sensor of highly sensitive nano zircite doping.
Background technology
Pafenolol is the cardiopathic medicine of a kind of efficient treatment, alternative blocking-up β1receptor, without intrinsic sympathomimetic acitivity, also blocking effect is had to the beta receptor (beta 2 receptor) of bronchus and vascular smooth muscle, bronchial spasm and schneiderian membrane fine vascular can be caused to shrink, main function is used for the treatment of heart disease, hypertension, but because long-term or excessive this type of medicine of use can cause addicted to medicine problem or insomnia, the spinoff such as to feel sick, even produce fatal risk when discontinuing medication suddenly, being therefore classified as controlled substance by most country in the world.
The method measuring pafenolol has ultraviolet spectroscopy, high-efficient liquid phase color method etc.But these methods are owing to needing expensive instrument and equipment, there is the shortcomings such as high, the consuming time length of cost, sensitivity is not high; Therefore, that study a kind of high sensibility, easy pafenolol assay method has very important significance.
Molecular imprinting is for template molecule with target molecule to be measured, to be combined with template molecule by covalently or non-covalently key to form monomer template molecular complex by having in structure complementary functional monomer, add crosslinking chemical again to make it to carry out polyreaction with monomer and form template molecule polymkeric substance, template molecule is removed by physics or chemical method after having reacted, obtain molecularly imprinted polymer, formed complementary with former microsphere space structure in the polymer and there is the hole in Multiple recognition site.Current method can not be mated with template molecule rightly due to the function monomer chosen, and crosslinked rigidity is also poor, and therefore sensitivity is not high.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method that a kind of equipment is simple, make the pafenolol molecular imprinting electrochemical sensor of easy, highly sensitive nano zircite doping.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: take pafenolol as template molecule, (5s, 8s)-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone is function monomer, azoisobutyronitrile is initiating agent, nano zircite is adulterant, with maleic rosin acrylic acid glycol ester for prepared by crosslinking chemical.
The preparation method of the pafenolol molecular imprinting electrochemical sensor of above-mentioned a kind of highly sensitive nano zircite doping, take pafenolol as template molecule, (5s, 8s)-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone is function monomer, azoisobutyronitrile is initiating agent, with maleic rosin acrylic acid glycol ester for crosslinking chemical, nano zircite is adulterant, diameter 2mm glassy carbon electrode surface is formed a kind of hybridized nanometer zirconia pafenolol molecular imprinting polymer membrane, then adopt the acetic acid of eluant, eluent mol ratio 2: 3 and alcohol mixed solvent by template molecule elution, obtain.
The preparation method of the pafenolol molecular imprinting electrochemical sensor of above-mentioned a kind of highly sensitive nano zircite doping, comprises the following steps:
< 1 > is in 10.0mL etoh solvent, add 0.1mmol ~ 0.9mmol template molecule pafenolol, 1.0mmol ~ 6.0mmol function monomer (5s successively, 8s) nano zircite of-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone, 4.5mmol crosslinking chemical maleic rosin acrylic acid glycol ester, 0.2mmol initiating agent azoisobutyronitrile and 0.0100g ~ 0.0250g, often adds a kind of chemical reagent ultrasound wave and dissolves 5 minutes;
The potpourri 8 μ L that < 2 > gets step < 1 > is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 5 hours, thermal polymerization 2.5 hours in the vacuum drying chamber that electrode after modifying is placed in 80 DEG C, then adopt eluant, eluent mol ratio be 2: 3 acetic acid and alcohol mixed solvent by template molecule elution, to obtain final product.
Research finds, take pafenolol as template molecule, (5s, 8s)-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone is function monomer, azoisobutyronitrile is initiating agent, nano zircite is adulterant, with the pafenolol molecular imprinting electrochemical sensor that maleic rosin acrylic acid glycol ester is prepared for crosslinking chemical, can be used for the content measuring pafenolol.Application the present invention sets up the electrochemical analysis method measuring pafenolol, has very outstanding sensitivity; The concentration of pafenolol is 1.0 × 10
-8~ 2.5 × 10
-4present good linear relationship (linearly dependent coefficient is R=0.9994) within the scope of mol/L, detection limit (S/N=3) is 2.0 × 10
-9mol/L, therefore, the pafenolol molecular imprinting electrochemical sensor of nano zircite doping has higher sensitivity, exceedes current detection method; And equipment is simple, it is simple and easy to make.
Accompanying drawing explanation
Fig. 1 is the working curve diagram of the preparation method of the pafenolol molecular imprinting electrochemical sensor of a kind of highly sensitive nano zircite doping in embodiment 1.
Embodiment
Embodiment 1
One, the process of glass-carbon electrode
Glass-carbon electrode is used on polishing cloth the alumina powder polishing of 1.0 μm, 0.3 μm and 0.05 μm successively, then put into the ultrasonic 8min of nitric acid that volume ratio is 1: 1, then put into the ultrasonic 8min of absolute ethyl alcohol, finally use pure water ultrasonic cleaning clean.
Two, the preparation of pafenolol molecular imprinting electrochemical sensor
< 1 > is in 10.0mL etoh solvent, add 0.6mmol template molecule pafenolol, 2.0mmol function monomer (5s successively, 8s) nano zircite of-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone, 4.5mmol crosslinking chemical maleic rosin acrylic acid glycol ester, 0.2mmol initiating agent azoisobutyronitrile and 0.0150g, often adds a kind of chemical reagent ultrasound wave and dissolves 5 minutes;
The potpourri 8 μ L that < 2 > gets step < 1 > is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 5 hours, thermal polymerization 2.5 hours in the vacuum drying chamber that electrode after modifying is placed in 80 DEG C, then adopt the acetic acid of eluant, eluent mol ratio 2: 3 and alcohol mixed solvent by template molecule elution, by magnetic agitation eluted template molecule, until can't detect template molecule in eluent, the solvent of trace electrode surface is washed away again with ultrapure water, then trace electrode is stored in ultrapure water stand-by.
Three, the drafting of working curve and the mensuration of detection limit
Carry out the experiment of the pafenolol molecular engram electrode response characteristic of nano zircite doping with differential pulse voltammetry, measure the range of linearity and detection limit.By nano zircite adulterate pafenolol molecular engram electrode respectively in the pafenolol solution of variable concentrations cultivate within 6 minutes, (end liquid is 5.0mmol/LK
3[Fe (CN)
6] the phosphate buffered solution solution of-0.5mol/LpH=7.5), then carry out differential pulse voltammetry measurement.Pafenolol solution concentration is 1.0 × 10
-8~ 2.5 × 10
-4good linear relationship is presented within the scope of mol/L; Linear equation is Ip (μ A)=-0.1047c (μm ol/L)+23.24, and linearly dependent coefficient is R=0.9994, and detection limit (S/N=3) is 2.0 × 10
-9mol/L.
Therefore, the pafenolol molecular engram electrode of this nano zircite doping has high sensitivity.
Claims (1)
1. the preparation method of the pafenolol molecular imprinting electrochemical sensor of a highly sensitive nano zircite doping, it is characterized in that with the pafenolol of 0.01mmol/mL ~ 0.09mmol/ml for template molecule, 0.1mmol/ml ~ 0.6mmol/ml (5s, 8s)-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone is function monomer, 0.02mmol/ml azoisobutyronitrile is initiating agent, 0.45mmol/ml maleic rosin acrylic acid glycol ester is crosslinking chemical, 0.0010g/ml ~ 0.0025g/ml nano zircite is adulterant, glassy carbon electrode surface is formed a kind of hybridized nanometer zirconia pafenolol molecular imprinting polymer membrane, then adopt eluant, eluent acetic acid and alcohol mixed solvent eluted template molecule and get final product,
Specifically undertaken by following operation:
<1> is in 10.0mL etoh solvent, add 0.1mmol ~ 0.9mmol template molecule pafenolol, 1.0mmol ~ 6.0mmol function monomer (5s successively, 8s) nano zircite of-3-(4 '-chloro-3 '-fluoro-4-vinyl biphenyl-3-base)-4-hydroxyl-8-ethoxy-1-azaspiro [4.5]-3-in last of the ten Heavenly stems alkene-2-ketone, 4.5mmol crosslinking chemical maleic rosin acrylic acid glycol ester, 0.2mmol initiating agent azoisobutyronitrile and 0.0100g ~ 0.0250g, often adds a kind of chemical reagent ultrasound wave and dissolves 5 minutes;
The potpourri 8 μ L that <2> gets step <1> is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 5 hours, thermal polymerization 2.5 hours in the vacuum drying chamber that electrode after modifying is placed in 80 DEG C, then adopt eluant, eluent mol ratio be 2: 3 acetic acid and alcohol mixed solvent by template molecule elution, to obtain final product.
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| CN107917945A (en) * | 2017-12-02 | 2018-04-17 | 广西民族大学 | A kind of preparation method of Timiperone molecular imprinting electrochemical sensor |
| CN107941878A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of depamide molecular imprinting electrochemical sensor |
| CN107941883A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of gastrodin molecular engram electrochemical sensor |
| CN107941877A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of Pimozide molecular imprinting electrochemical sensor |
| CN107957443A (en) * | 2017-12-02 | 2018-04-24 | 广西民族大学 | A kind of preparation method of ethymal molecular imprinting electrochemical sensor |
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| CN107991498A (en) * | 2017-12-02 | 2018-05-04 | 广西民族大学 | A kind of preparation method of phensuximide molecular imprinting electrochemical sensor |
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| CN107917945A (en) * | 2017-12-02 | 2018-04-17 | 广西民族大学 | A kind of preparation method of Timiperone molecular imprinting electrochemical sensor |
| CN107941878A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of depamide molecular imprinting electrochemical sensor |
| CN107941883A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of gastrodin molecular engram electrochemical sensor |
| CN107941877A (en) * | 2017-12-02 | 2018-04-20 | 广西民族大学 | A kind of preparation method of Pimozide molecular imprinting electrochemical sensor |
| CN107957443A (en) * | 2017-12-02 | 2018-04-24 | 广西民族大学 | A kind of preparation method of ethymal molecular imprinting electrochemical sensor |
| CN107957445A (en) * | 2017-12-02 | 2018-04-24 | 广西民族大学 | A kind of preparation method of bromocryptine molecular imprinting electrochemical sensor |
| CN107957444A (en) * | 2017-12-02 | 2018-04-24 | 广西民族大学 | A kind of preparation method of easypro thiazine molecular imprinting electrochemical sensor |
| CN107957438A (en) * | 2017-12-02 | 2018-04-24 | 广西民族大学 | A kind of preparation method of eszopiclone molecular imprinting electrochemical sensor |
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