CN105628777A - Preparation method of high-sensitivity functionalized gold nanoparticle-doped phenprobamate MIECS (Molecular Imprinting Electrochemical Sensor) - Google Patents
Preparation method of high-sensitivity functionalized gold nanoparticle-doped phenprobamate MIECS (Molecular Imprinting Electrochemical Sensor) Download PDFInfo
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- CN105628777A CN105628777A CN201610000381.2A CN201610000381A CN105628777A CN 105628777 A CN105628777 A CN 105628777A CN 201610000381 A CN201610000381 A CN 201610000381A CN 105628777 A CN105628777 A CN 105628777A
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- phenprobamate
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- G—PHYSICS
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- 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
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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
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/308—Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
Abstract
The invention discloses a preparation method of a high-sensitivity functionalized gold nanoparticle-doped phenprobamate MIECS (Molecular Imprinting Electrochemical Sensor). The preparation method is characterized by taking phenprobamate as a template molecule, aminotadalafil as a functional monomer, azodiisobutyronitrile as an initiator, dodecanethiol functionalized gold nanoparticles as a doping agent and hydrocortisone acetate as a coupling agent, thus preparing the high-sensitivity dodecanethiol functionalized gold nanoparticle-doped phenprobamate MIECS. An analysis method is simple and practical, and the disadvantages of complexity, expensive price of equipment and low sensitivity of a previous analysis method are overcome.
Description
Technical field
The present invention relates to molecular imprinting electrochemical sensor, the preparation method of the phenprobamate molecular imprinting electrochemical sensor of especially a kind of highly sensitive functionalized golden nanometer particle doping.
Background technology
The main function of phenprobamate is the pain for treating anxiety and the muscle epitonos such as muscle spasm, muscle rigidity causes, but owing to being excessively used that this type of medicine can cause drowsiness, dizzy, malaise, walking is unstable, feel sick, flatulence, stomachache, the side effect such as stomach upset sense and stomach dull pain.
The method measuring phenprobamate (Phenprobamate) has ultraviolet spectroscopy, Gradient Elution method, reversed-phase high-performance liquid chromatography-diode array etc. But these methods are owing to needing the instrument and equipment of costliness, there is cost length high, consuming time or the shortcoming such as sensitivity is not high; Therefore, study a kind of high sensibility, simplicity phenprobamate assay method to have very important significance.
Molecular imprinting is with target molecule to be measured for template molecule, be combined with template molecule by covalently or non-covalently key form monomer template molecular complex by having in structure complementary functional monomer, add cross-linking agent so as to carry out polyreaction with monomer to form template molecule polymer, by either physically or chemically removing template molecule after having reacted, obtain molecularly imprinted polymer, form complementary with former microsphere space structure and that there is Multiple recognition site hole in the polymer. Current method can not be properly matched with template molecule due to the function monomer chosen, and the rigidity cross-linked 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 phenprobamate molecular imprinting electrochemical sensor of easy a kind of highly sensitive functionalized golden nanometer particle doping.
For solving above-mentioned technical problem, the present invention adopt the following technical scheme that with phenprobamate be template molecule, amino tadalafil be function monomer, azodiisobutyronitrile be initiator, the functionalized golden nanometer particle of lauryl mercaptan for adulterant, prepare with hydrocortisone acetate for cross-linking agent.
The preparation method of the phenprobamate molecular imprinting electrochemical sensor of above-mentioned a kind of highly sensitive functionalized golden nanometer particle doping, with phenprobamate for template molecule, amino tadalafil is function monomer, azodiisobutyronitrile is initiator, with hydrocortisone acetate for cross-linking agent, the functionalized golden nanometer particle of lauryl mercaptan is adulterant, diameter 2mm glassy carbon electrode surface is formed a kind of functionalized golden nanometer particle phenprobamate molecular imprinting polymer membrane of hydridization lauryl mercaptan, then adopt the acetic acid of eluant mol ratio 1: 2 and isopropyl alcohol mixed solvent by template molecule elution, obtain.
The preparation method of the phenprobamate molecular imprinting electrochemical sensor of above-mentioned a kind of highly sensitive functionalized golden nanometer particle doping, comprises the following steps:
<1>in 10.0mL etoh solvent, it is sequentially added into the functionalized golden nanometer particle of lauryl mercaptan of 0.3mmol��0.6mmol template molecule phenprobamate, 1.0mmol��5.0mmol function monomer amino tadalafil, 5mmol cross-linking agent hydrocortisone acetate, 0.2mmol initiator azodiisobutyronitrile and 0.0250g��0.0450g, often adds a kind of chemical reagent ultrasound wave and dissolve 9 minutes;
<2>the mixture 8 �� L taking step<1>is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, after placing 5 hours, electrode after modifying is placed in the vacuum drying oven of 68 DEG C thermal polymerization 4.5 hours, then the acetic acid adopting eluant mol ratio to be 1: 2 and isopropyl alcohol mixed solvent, by template molecule elution, to obtain final product.
Research finds, with phenprobamate be template molecule, amino tadalafil be function monomer, azodiisobutyronitrile be initiator, the functionalized golden nanometer particle of lauryl mercaptan is for adulterant, with the phenprobamate molecular imprinting electrochemical sensor that hydrocortisone acetate is prepared for cross-linking agent, can be used for measuring the content of phenprobamate. The application present invention sets up the electrochemical analysis method measuring phenprobamate, has very outstanding sensitivity; The concentration of phenprobamate is 1.0 �� 10-8��2.1 �� 10-4Presenting good linear relationship (linearly dependent coefficient is R=0.9998) within the scope of mol/L, detection limit (S/N=3) is 1.5 �� 10-9Mol/L, therefore, the phenprobamate molecular imprinting electrochemical sensor of 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 of the preparation method of the phenprobamate molecular imprinting electrochemical sensor of a kind of highly sensitive functionalized golden nanometer particle doping in embodiment 1.
Detailed description of the invention
Embodiment 1
One, the process of glass-carbon electrode
Glass-carbon electrode is polished with the alumina powder of 1.0 ��m, 0.3 ��m and 0.05 ��m successively on polishing cloth, is then placed in ultrasonic 8min in the nitric acid that volume ratio is 1: 1, places into ultrasonic 8min in dehydrated alcohol, finally clean with pure water ultrasonic cleaning.
Two, the preparation of phenprobamate molecular imprinting electrochemical sensor
<1>in 10.0mL etoh solvent, it is sequentially added into the functionalized golden nanometer particle of lauryl mercaptan of 0.4mmol template molecule phenprobamate, 2.0mmol function monomer amino tadalafil, 5mmol cross-linking agent hydrocortisone acetate, 0.2mmol initiator azodiisobutyronitrile and 0.0350g, often adds a kind of chemical reagent ultrasound wave and dissolve 9 minutes;
<2>the mixture 8 �� L taking step<1>is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, after placing 5 hours, electrode after modifying is placed in the vacuum drying oven of 68 DEG C thermal polymerization 4.5 hours, then adopt eluant mol ratio 1: 2 acetic acid and isopropyl alcohol mixed solvent by template molecule elution, by magnetic agitation eluted template molecule, until eluent can't detect template molecule, wash away the solvent of trace electrode surface again with ultra-pure water, then trace electrode is stored in ultra-pure water stand-by.
Three, the mensuration of the drafting of working curve and detection limit
It is functionalized the experiment of the phenprobamate molecular engram electrode response characteristic of golden nanometer particle doping with differential pulse voltammetry, measures the range of linearity and detection limit. The phenprobamate molecular engram electrode that functionalized golden nanometer particle is adulterated respectively in the phenprobamate solution of variable concentrations cultivate within 7 minutes, (end liquid is 5.0mmol/LK3[Fe(CN)6] the phosphate buffered solution solution of-0.5mol/LpH=7.5), then carry out differential pulse voltammetry measurement. Phenprobamate solution concentration is 1.0 �� 10-8��2.1 �� 10-4Good linear relationship is presented within the scope of mol/L; Linear equation is Ip (�� A)=-0.0990c (��m ol/L)+23.14, and linearly dependent coefficient is R=0.9998, and detection limit (S/N=3) is 1.5 �� 10-9mol/L��
Therefore, the phenprobamate molecular engram sensor of this functionalized golden nanometer particle doping has high sensitivity.
Claims (1)
1. the preparation method of the phenprobamate molecular imprinting electrochemical sensor of a highly sensitive functionalized golden nanometer particle doping, it is characterized in that with the phenprobamate of 0.03mmol/mL��0.06mmol/ml for template molecule, the amino tadalafil of 0.1mmol/ml��0.5mmol/ml is function monomer, 0.02mmol/ml azodiisobutyronitrile is initiator, 0.5mmol/ml hydrocortisone acetate is cross-linking agent, the functionalized golden nanometer particle of 0.0025g/ml��0.0045g/ml lauryl mercaptan is adulterant, glassy carbon electrode surface is formed a kind of functionalized golden nanometer particle phenprobamate molecular imprinting polymer membrane of hydridization lauryl mercaptan, then adopt eluant acetic acid and isopropyl alcohol mixed solvent eluted template molecule and get final product,
Specifically undertaken by following operation:
<1>in 10.0mL etoh solvent, it is sequentially added into the functionalized golden nanometer particle of lauryl mercaptan of 0.3mmol��0.6mmol template molecule phenprobamate, 1.0mmol��5.0mmol function monomer amino tadalafil, 5mmol cross-linking agent hydrocortisone acetate, 0.2mmol initiator azodiisobutyronitrile and 0.0250g��0.0450g, often adds a kind of chemical reagent ultrasound wave and dissolve 9 minutes;
<2>the mixture 8 �� L taking step<1>is applied in the glassy carbon electrode surface that totally smooth diameter is 2mm, after placing 5 hours, electrode after modifying is placed in the vacuum drying oven of 68 DEG C thermal polymerization 4.5 hours, then the acetic acid adopting eluant mol ratio to be 1: 2 and isopropyl alcohol mixed solvent, by template molecule elution, to obtain final product.
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| CN108007987A (en) * | 2017-12-02 | 2018-05-08 | 广西民族大学 | A kind of preparation method of ethyldopa molecular imprinting electrochemical sensor |
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