CN105510415A - Preparation method for high-sensitivity functionalized gold nanoparticle-doped meprobamate molecularly-imprinted electrochemical sensor - Google Patents
Preparation method for high-sensitivity functionalized gold nanoparticle-doped meprobamate molecularly-imprinted electrochemical sensor Download PDFInfo
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- CN105510415A CN105510415A CN201610000382.7A CN201610000382A CN105510415A CN 105510415 A CN105510415 A CN 105510415A CN 201610000382 A CN201610000382 A CN 201610000382A CN 105510415 A CN105510415 A CN 105510415A
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- meprobamate
- template molecule
- nanometer particle
- golden nanometer
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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
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
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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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
Abstract
The invention discloses a preparation method for a high-sensitivity functionalized gold nanoparticle-doped meprobamate molecularly-imprinted electrochemical sensor. According to the method, meprobamate serves as a template molecule, aminotadalafil serves as a functional monomer, azodiisobutyronitrile serves as an initiating agent, dodecanethiol functionalized gold nanoparticles serve as a doping agent, hydrocortisone acetate serves as a cross-linking agent, and then the high-sensitivity dodecanethiol functionalized gold nanoparticle-doped meprobamate molecularly-imprinted electrochemical sensor is prepared. The analytical method is simple and practical, and the defects that an original analytical method is complex, expensive in equipment, and low in sensitivity are overcome.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, especially a kind of preparation method of Meprobamate molecular imprinting electrochemical sensor of highly sensitive functionalized golden nanometer particle doping.
Background technology
Meprobamate primary treatment anxiety neurosis, alleviates the symptom such as anxiety, anxiety, uneasiness, insomnia, also can treat the disease of the too high or muscular rigidity of Muscle tensility.But because long-term or excessive this type of medicine of use can cause addicted to medicine problem or the spinoff such as drowsiness, kidney, lung, liver function damage, even produce fatal risk when discontinuing medication suddenly, being therefore classified as controlled substance by most country in the world.
The method measuring Meprobamate (Meprobamate) has ultraviolet spectroscopy, high performance liquid chromatography 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 Meprobamate 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 Meprobamate molecular imprinting electrochemical sensor of easy a kind of highly sensitive functionalized golden nanometer particle doping.
For solving the problems of the technologies described above, the present invention adopts following technical scheme: taking Meprobamate as template molecule, amino tadalafil is function monomer, azoisobutyronitrile is initiating agent, the functionalized golden nanometer particle of lauryl mercaptan is adulterant, is prepared by crosslinking chemical with hydrocortisone acetate.
The preparation method of the Meprobamate molecular imprinting electrochemical sensor of above-mentioned a kind of highly sensitive functionalized golden nanometer particle doping, take Meprobamate as template molecule, amino tadalafil is function monomer, azoisobutyronitrile is initiating agent, take hydrocortisone acetate as crosslinking chemical, the functionalized golden nanometer particle of lauryl mercaptan is adulterant, diameter 2mm glassy carbon electrode surface is formed the Meprobamate hybrid molecule imprinted polymer films of a kind of functionalized golden nanometer particle doping, then adopt the acetic acid of eluant, eluent mol ratio 2: 3 and phenmethylol mixed solvent by template molecule elution, obtain.
The preparation method of the Meprobamate molecular imprinting electrochemical sensor of the highly sensitive functionalized golden nanometer particle doping of above-mentioned kind, comprises the following steps:
<1> is in 10.0mL etoh solvent, add the functionalized golden nanometer particle of lauryl mercaptan of 0.2mmol ~ 0.8mmol template molecule Meprobamate, 2.0mmol ~ 6.0mmol function monomer amino tadalafil, 3.8mmol crosslinking chemical hydrocortisone acetate, 0.1mmol initiating agent azoisobutyronitrile and 0.0200g ~ 0.0400g successively, often add a kind of chemical reagent ultrasound wave and dissolve 12 minutes;
The potpourri 6 μ L that <2> gets step <1> is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 6 hours, thermal polymerization 5.5 hours in the vacuum drying chamber that electrode after modifying is placed in 65 DEG C, then adopt eluant, eluent mol ratio be 2: 3 acetic acid and phenmethylol mixed solvent by template molecule elution, to obtain final product.
Research finds, take Meprobamate as template molecule, amino tadalafil is function monomer, azoisobutyronitrile is initiating agent, the functionalized golden nanometer particle of lauryl mercaptan is adulterant, the Meprobamate molecular imprinting electrochemical sensor prepared with hydrocortisone acetate, can be used for the content measuring Meprobamate.Application the present invention sets up the electrochemical analysis method measuring Meprobamate, has very outstanding sensitivity; The concentration of Meprobamate is 1.0 × 10
-8~ 2.0 × 10
-4present good linear relationship (linearly dependent coefficient is R=0.9994) within the scope of mol/L, detection limit (S/N=3) is 1.2 × 10
-9mol/L, therefore, the Meprobamate molecular imprinting electrochemical sensor of this lauryl mercaptan functionalized golden nanometer particle 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 in a kind of preparation method's embodiment 1 of Meprobamate molecular imprinting electrochemical sensor of highly sensitive functionalized golden nanometer particle doping.
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 Meprobamate molecular imprinting electrochemical sensor
<1> is in 10.0mL etoh solvent, add the functionalized golden nanometer particle of lauryl mercaptan of 0.5mmol template molecule Meprobamate, 5.0mmol function monomer amino tadalafil, 3.8mmol crosslinking chemical hydrocortisone acetate, 0.1mmol initiating agent azoisobutyronitrile and 0.0250g successively, often add a kind of chemical reagent ultrasound wave and dissolve 12 minutes;
The potpourri 6 μ L that <2> gets step <1> is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 6 hours, thermal polymerization 5.5 hours in the vacuum drying chamber that electrode after modifying is placed in 65 DEG C, then adopt eluant, eluent mol ratio 2: 3 acetic acid and phenmethylol 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 Meprobamate molecular engram electrode response characteristic of the functionalized golden nanometer particle doping of lauryl mercaptan with differential pulse voltammetry, measure the range of linearity and detection limit.The Meprobamate molecular engram electrode of functionalized for lauryl mercaptan golden nanometer particle doping is cultivated in the Meprobamate solution of variable concentrations respectively 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.Meprobamate solution concentration is 1.0 × 10
-8~ 2.0 × 10
-4good linear relationship is presented within the scope of mol/L; Linear equation is Ip (μ A)=-0.0903c (μm ol/L)+23.32, and linearly dependent coefficient is R=0.9994, and detection limit (S/N=3) is 1.2 × 10
-9mol/L.
Therefore, the Meprobamate molecular engram electrode of this lauryl mercaptan functionalized golden nanometer particle doping has high sensitivity.
Claims (1)
1. the preparation method of the Meprobamate molecular imprinting electrochemical sensor of a highly sensitive functionalized golden nanometer particle doping, it is characterized in that with the Meprobamate of 0.02mmol/mL ~ 0.08mmol/ml for template molecule, the amino tadalafil of 0.2mmol/ml ~ 0.6mmol/ml is function monomer, 0.01mmol/ml azoisobutyronitrile is initiating agent, with 0.38mmol/ml hydrocortisone acetate for crosslinking chemical, the functionalized golden nanometer particle of 0.0020g/ml ~ 0.0040g/ml lauryl mercaptan is adulterant, glassy carbon electrode surface is formed the Meprobamate molecular imprinting polymer membrane of the functionalized golden nanometer particle doping of a kind of lauryl mercaptan, then adopt eluant, eluent acetic acid and phenmethylol mixed solvent eluted template molecule and get final product,
Specifically undertaken by following operation:
<1> is in 10.0mL etoh solvent, add the functionalized golden nanometer particle of lauryl mercaptan of 0.2mmol ~ 0.8mmol template molecule Meprobamate, 2.0mmol ~ 6.0mmol function monomer amino tadalafil, 3.8mmol crosslinking chemical hydrocortisone acetate, 0.1mmol initiating agent azoisobutyronitrile and 0.0200g ~ 0.0400g successively, often add a kind of chemical reagent ultrasound wave and dissolve 12 minutes;
The potpourri 6 μ L that <2> gets step <1> is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, place after 6 hours, thermal polymerization 5.5 hours in the vacuum drying chamber that electrode after modifying is placed in 65 DEG C, then adopt eluant, eluent mol ratio be 2: 3 acetic acid and phenmethylol mixed solvent by template molecule elution, to obtain final product.
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| CN106770557A (en) * | 2017-01-09 | 2017-05-31 | 广西民族大学 | A kind of preparation method of highly sensitive Bezafibrate molecular imprinting electrochemical sensor |
| CN106770558A (en) * | 2017-01-09 | 2017-05-31 | 广西民族大学 | A kind of preparation method of highly sensitive pemoline molecular imprinting electrochemical sensor |
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| CN103926288A (en) * | 2014-04-25 | 2014-07-16 | 广西民族大学 | High-sensitivity nanometer cobalt oxide-doped amobarbital molecular imprinting electrochemical sensor and preparation method thereof |
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| CN106770558A (en) * | 2017-01-09 | 2017-05-31 | 广西民族大学 | A kind of preparation method of highly sensitive pemoline molecular imprinting electrochemical sensor |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
| CN107976479A (en) * | 2017-12-02 | 2018-05-01 | 广西民族大学 | A kind of preparation method of mysoline molecular imprinting electrochemical sensor |
| 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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