CN105628777B - A kind of preparation method of the phenprobamate molecular imprinting electrochemical sensor of highly sensitive functionalization golden nanometer particle doping - Google Patents

A kind of preparation method of the phenprobamate molecular imprinting electrochemical sensor of highly sensitive functionalization golden nanometer particle doping Download PDF

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CN105628777B
CN105628777B CN201610000381.2A CN201610000381A CN105628777B CN 105628777 B CN105628777 B CN 105628777B CN 201610000381 A CN201610000381 A CN 201610000381A CN 105628777 B CN105628777 B CN 105628777B
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phenprobamate
golden nanometer
nanometer particle
ml
kind
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CN201610000381.2A
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CN105628777A (en
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韦贻春
余会成
李�浩
雷福厚
陈其锋
谭学才
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广西民族大学
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Abstract

The invention discloses a kind of preparation method of the phenprobamate molecular imprinting electrochemical sensor of highly sensitive functionalization golden nanometer particle doping, using phenprobamate as template molecule, amino tadalafil is function monomer, azodiisobutyronitrile is initiator, lauryl mercaptan functionalization golden nanometer particle is dopant, crosslinking agent is used as using hydrocortisone acetate, the phenprobamate molecular imprinting electrochemical sensor of highly sensitive lauryl mercaptan functionalization golden nanometer particle doping is prepared for accordingly, the analysis method is simple and practical, it is complicated to overcome conventional analysis method, equipment is expensive, the shortcomings that sensitivity is low.

Description

A kind of phenprobamate molecular engram of highly sensitive functionalization golden nanometer particle doping The preparation method of electrochemical sensor

Technical field

The present invention relates to molecular imprinting electrochemical sensor, especially a kind of highly sensitive functionalization golden nanometer particle is mixed The preparation method of miscellaneous phenprobamate molecular imprinting electrochemical sensor.

Background technology

The main function of phenprobamate is caused for treating the muscle epitonos such as anxiety and muscle cramp, muscle rigidity Pain, but due to be excessively used such medicine can cause drowsiness, dizzy, malaise, walking shakiness, nausea, gasteremphraxis, abdomen Bitterly, the side effect such as stomach upset sense and stomach dull pain.

Measure phenprobamate (Phenprobamate) method have ultraviolet spectroscopy, Gradient Elution method, RPLC-diode array etc..But there is cost in these methods due to needing expensive instrument and equipment High, the shortcomings of time-consuming or sensitivity is not high;Therefore, study a kind of high sensibility, easy phenprobamate assay method has Very 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 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, complementary and with Multiple recognition site the sky with former microsphere space structure is formed in the polymer Cave.Current method is because the function monomer of selection can not be properly matched with template molecule, and the rigidity being crosslinked 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 highly sensitive function Change the preparation method of the phenprobamate molecular imprinting electrochemical sensor of golden nanometer particle doping.

In order to solve the above technical problems, the present invention adopts the following technical scheme that:Using phenprobamate as template molecule, amino he Da Nafei is function monomer, azodiisobutyronitrile is initiator, lauryl mercaptan functionalization golden nanometer particle is dopant, with acetic acid Hydrocortisone is prepared for crosslinking agent.

A kind of phenprobamate molecular imprinting electrochemical sensor of above-mentioned highly sensitive functionalization golden nanometer particle doping Preparation method, using phenprobamate as template molecule, amino tadalafil be function monomer, azodiisobutyronitrile is initiator, It is dopant by crosslinking agent, lauryl mercaptan functionalization golden nanometer particle of hydrocortisone acetate, in diameter 2mm glass-carbon electrode tables A kind of hydridization lauryl mercaptan functionalization golden nanometer particle phenprobamate molecular imprinting polymer membrane is formed on face, then uses and washes The acetic acid and isopropyl alcohol mixed solvent of de- agent mol ratio 1: 2 produce template molecule elution.

A kind of phenprobamate molecular imprinting electrochemical sensor of above-mentioned highly sensitive functionalization golden nanometer particle doping Preparation method, comprise the following steps:

<1>Into 10.0mL etoh solvents, sequentially add 0.3mmol~0.6mmol template molecules phenprobamate, 1.0mmol~5.0mmol function monomer amino tadalafil, 5mmol crosslinking agents hydrocortisone acetate, 0.2mmol initiators The lauryl mercaptan functionalization golden nanometer particle of azodiisobutyronitrile and 0.0250g~0.0450g, often adds a kind of chemical reagent and surpasses Sound wave dissolves 9 minutes;

<2>Take step<1>The μ L of mixture 8 be applied in clean smooth a diameter of 2mm glassy carbon electrode surface, place 5 After hour, the electrode after modification is placed in thermal polymerization 4.5 hours in 68 DEG C of vacuum drying chamber, then using eluant, eluent mol ratio Acetic acid and isopropyl alcohol mixed solvent for 1: 2 produce template molecule elution.

Research finds, using phenprobamate as template molecule, amino tadalafil be function monomer, azodiisobutyronitrile is draws Hair agent, lauryl mercaptan functionalization golden nanometer particle are dopant, the phenprobamate prepared using hydrocortisone acetate as crosslinking agent Molecular imprinting electrochemical sensor, the content available for measure phenprobamate.The electricity for determining phenprobamate is established using the present invention Chemical analysis method, there is very outstanding sensitivity;The concentration of phenprobamate is 1.0 × 10-8~2.1 × 10-4Mol/L scopes Interior that good linear relationship (linearly dependent coefficient R=0.9998) is presented, detection limit (S/N=3) is 1.5 × 10-9Mol/L, Therefore, the phenprobamate molecular imprinting electrochemical sensor of functionalization golden nanometer particle doping has higher sensitivity, exceedes Current detection method, and equipment is simple, it is simple to make.

Brief description of the drawings

Fig. 1 is a kind of phenprobamate molecular engram electricity of highly sensitive functionalization golden nanometer particle doping in embodiment 1 The working curve diagram of the preparation method of chemical sensor.

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 Ultrasonic 8min in the nitric acid that volume ratio is 1: 1, ultrasonic 8min in absolute ethyl alcohol is placed into, be finally cleaned by ultrasonic with pure water clean.

2nd, the preparation of phenprobamate molecular imprinting electrochemical sensor

<1>Into 10.0mL etoh solvents, 0.4mmol template molecules phenprobamate, 2.0mmol function monomers are sequentially added Amino tadalafil, 5mmol crosslinking agents hydrocortisone acetate, the ten of 0.2mmol initiator azodiisobutyronitriles and 0.0350g Two thiol-functional golden nanometer particles, often add a kind of chemical reagent ultrasonic wave and dissolve 9 minutes;

<2>Take step<1>The μ L of mixture 8 be applied in clean smooth a diameter of 2mm glassy carbon electrode surface, place 5 After hour, the electrode after modification is placed in thermal polymerization 4.5 hours in 68 DEG C of vacuum drying chamber, then using eluant, eluent mol ratio 1: 2 acetic acid and isopropyl alcohol mixed solvent are by template molecule elution, by magnetic agitation eluted template molecule, until being examined in eluent Template molecule is not detected, then the solvent of trace electrode surface is washed away with ultra-pure water, then trace electrode is stored in ultra-pure water It is stand-by.

3rd, the measure of the drafting of working curve and detection limit

The phenprobamate molecular engram electrode response that golden nanometer particle doping is functionalized with differential pulse voltammetry is special Property experiment, determine the range of linearity and detection limit.The phenprobamate molecular engram electrode point that functionalization golden nanometer particle is adulterated 7 minutes are cultivated not in the phenprobamate solution of various concentrations, and (bottom liquid is 5.0mmol/L K3[Fe(CN)6]-0.5mol/L pH =7.5 phosphate buffer solution solution), then carry out differential pulse voltammetry measurement.Phenprobamate solution concentration 1.0 × 10-8~2.1 × 10-4Good linear relationship is presented in the range of mol/L;Linear equation is Ip (μ A)=- 0.0990c (μm ol/ L)+23.14, linearly dependent coefficient R=0.9998, detection limit (S/N=3) are 1.5 × 10-9mol/L。

Therefore, the phenprobamate molecular engram sensor of functionalization golden nanometer particle doping has high sensitivity.

Claims (1)

  1. A kind of 1. preparation of the phenprobamate molecular imprinting electrochemical sensor of highly sensitive functionalization golden nanometer particle doping Method, it is characterised in that using 0.03mmol/mL~0.06mmol/mL phenprobamate as template molecule, 0.1mmol/mL~ 0.5mmol/mL amino tadalafil is function monomer, 0.02mmol/mL azodiisobutyronitriles are initiator, 0.5mmol/mL Hydrocortisone acetate is crosslinking agent, 0.0025g/mL~0.0045g/mL lauryl mercaptan functionalization golden nanometer particles are doping Agent, a kind of hydridization lauryl mercaptan functionalization golden nanometer particle phenprobamate molecularly imprinted polymer is formed in glassy carbon electrode surface Film, then produced using eluant, eluent acetic acid and isopropyl alcohol mixed solvent eluted template molecule;
    Specifically carried out by following operation:
    <1>Into 10.0mL etoh solvents, sequentially add 0.3mmol~0.6mmol template molecules phenprobamate, 1.0mmol~ 5.0mmol function monomer amino tadalafil, 5mmol crosslinking agents hydrocortisone acetate, the isobutyl of 0.2mmol initiators azo two The lauryl mercaptan functionalization golden nanometer particle of nitrile and 0.0250g~0.0450g, often add a kind of chemical reagent ultrasonic wave dissolving 9 Minute;
    <2>Take step<1>The μ L of mixture 8 be applied in clean smooth a diameter of 2mm glassy carbon electrode surface, place 5 hours Afterwards, the electrode after modification is placed in thermal polymerization 4.5 hours in 68 DEG C of vacuum drying chamber, then uses eluant, eluent mol ratio as 1: 2 acetic acid and isopropyl alcohol mixed solvent produce template molecule elution.
CN201610000381.2A 2016-01-04 2016-01-04 A kind of preparation method of the phenprobamate molecular imprinting electrochemical sensor of highly sensitive functionalization golden nanometer particle doping CN105628777B (en)

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