CN102384933A - L-serine/chitosan modified acetaminophen electrochemical sensor and application thereof - Google Patents
L-serine/chitosan modified acetaminophen electrochemical sensor and application thereof Download PDFInfo
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- CN102384933A CN102384933A CN2010102778160A CN201010277816A CN102384933A CN 102384933 A CN102384933 A CN 102384933A CN 2010102778160 A CN2010102778160 A CN 2010102778160A CN 201010277816 A CN201010277816 A CN 201010277816A CN 102384933 A CN102384933 A CN 102384933A
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Abstract
The invention discloses an L-serine/chitosan modified acetaminophen electrochemical sensor and application thereof, relating to an L-serine/chitosan modified acetaminophen electrochemical sensor and application to measurement of acetaminophen by using the L-serine/chitosan modified acetaminophen electrochemical sensor. A glassy carbon electrode is used as a working electrode, and an L-serine/chitosan composite film is coated on the surface of the glassy carbon electrode. The L-serine/chitosan modified acetaminophen electrochemical sensor has the advantages of high sensitivity and good selectivity.
Description
Technical field
The present invention relates to the electrochemical sensor of a kind of L-serine/chitosan-modified and come paracetamol to measure with this sensor.
Background technology
Paracetamol (ACOP) is commonly called as paracetamol, is acetophenone amine medicine; Can be through suppressing the synthetic of prostaglandin in the central nervous system, and the impulsion of blocking-up pain nerve tip and produce analgesic, analgesic effect, its pharmacological action is similar with aspirin; But its spinoff is much littler than aspirin; Can be used for irritated to aspirin, do not tolerate or be inappropriate for the case of using aspirin, like varicella, hemophilia, and peptic ulcer, gastritis etc.ACOP uses in chinese-western medicine preparation extensively, diseases such as heating, headache, arthralgia, rheumatalgia, skeletal muscle pain and the various neuralgia that being applicable to catches a cold causes, antimigraine, dysmenorrhoea.Can damage human body but too much take paracetamol, all influential to digestive system, urinary system, hematological system, respiratory system, also can suppress respiratory center when serious, damage the liver kidney.So control requires very strictly to the content of ACOP, and the research of ACOP assay method has also just been had significance.The current method that is used to detect ACOP has titrimetry method, AAS, chromatography, capillary electrophoresis, chemoluminescence method, thin layer chromatography scanning etc.The experiment condition and the operative technique of the requirement that has in these methods are higher, and the pre-treatment process that the needs that have are complicated is unfavorable for the fast detecting to ACOP.Therefore develop cheap, simple to operate, response rapidly, and the detection method of the higher ACOP of sensitivity has great practical significance.In recent years, the electrochemical sensing technology is simple to operate with it, and cost is low, and the sample that is equipped with detection need not pass through pre-service and can directly measure; Electrode response is fast, needs the short period; Selectivity, sensitivity are better; Stable and anti-interference strong, and have application promise in clinical practice.
The L-serine is a kind of aliphatics polarity alpha amino acid, also is a kind of important amino acid in the natural amino acid, contain simultaneously active-OH ,-NH
2With-COOH, have good electrochemical activity, thereby its Electrochemical characteriration is had crucial meaning.The absorption chelation can take place with some molecules, ion in the L-serine, makes L-serine modified electrode in chemical analysis and bioanalysis, have a good application prospect.
Shitosan is to be obtained through deacetylation by the chitin that nature extensively exists, and chemical name is polydextrose amine (1-4)-2-amino-B-D glucose, and is abundant at occurring in nature content, good film-forming property.Has abundant-NH in its molecule
2With-OH, thus make shitosan have effects such as ion-exchange, ion chelating, absorption to many ions, organism.Thereby in analysis field, be used widely the various modified electrodes that especially prepare, superior performance as active detection material.But discover, simple unsatisfactory with chitosan-modified electrode performance, lack good selectivity and sensitivity.
Summary of the invention
Shortcoming to existing detection technique the invention provides a kind of L-serine/chitosan-modified electrochemical sensor that can measure paracetamol content, advantage highly sensitive, that selectivity is good that this electrochemical sensor has.
In order to realize above-mentioned purpose of the present invention, the present invention adopts following technical scheme, and it is working electrode with the glass-carbon electrode, and the glass-carbon electrode surfaces coated is covered with L-serine/chitosan complex film;
The preparation method of L-serine/chitosan complex film is:
(1) glass-carbon electrode is polished successively, polished and cleans, obtain pretreated glassy carbon electrode;
(2) shitosan and L-serine are joined in the acetum, constantly stir and make it dissolving fully; Wherein, the mass and size concentration of shitosan is 0.005g/mL～0.007g/mL, and the mass and size concentration of L-serine is 0.003g/mL～0.005g/mL;
(3) pretreated glassy carbon electrode that step (1) is obtained immerses in the prepared mixed solution of step (2), leaves standstill under the room temperature 3-5 hour, promptly gets the crude product of the glass-carbon electrode that is coated with L-serine/chitosan complex film;
(4) crude product that makes in the step (3) is cleaned 2-3 time with redistilled water, remove unnecessary L-serine and shitosan, dry under the room temperature, promptly get and be coated with L-serine/chitosan complex film.
The mass concentration of the acetum in the step (1) is 1%～2%.
It can be used for measuring the content of paracetamol in the solution.
Use its method of measuring Paracetamol content in the solution to be:
(1) paracetamol standard water solution to be measured is added in acetate-sodium acetate buffer solution, with this as electrolytic solution;
(2) be working electrode with L-serine/chitosan-modified glass-carbon electrode, saturated calomel electrode is a contrast electrode, and platinum electrode is an auxiliary electrode, places the electrolytic solution described in the step (1), carries out electro-chemical test.
In the described electrolytic solution, acetaminophen solution concentration to be measured is 0～1.0 * 10
-3Mol/L, the pH value of acetate-sodium acetate buffer solution is 4.6～5.3.
PH value the best of described acetate-sodium acetate buffer solution is 4.9.
Beneficial effect of the present invention:
The present invention adopts L-serine and the shitosan preparation electrochemical sensor that combines, and it is adsorbed onto the glass-carbon electrode surface through noncovalent interaction with shitosan and L-serine, has made L-serine/chitosan-modified electrochemical sensor.This sensor had both overcome the not strong shortcoming of shitosan selective adsorption capacity; Amino acid instability, caducous inferior position have also been remedied; Given full play to the two advantage separately, strengthened the detectability of sensor, and given full play to the hydrogen bond adsorption technology and prepare easy, reliable and stable advantage; Made electrochemical sensor, had the advantage quick, sensitive, that antijamming capability is strong with higher sensitivity and stability.The present invention adopts self-assembly method with active detection material L-serine and chitosan-modified to electrode surface in addition, makes the preparation of electrochemical sensor easy, with low cost.
Description of drawings
Fig. 1 is the preparation process mechanism synoptic diagram of L-serine/chitosan-modified electrochemical sensor; From figure, can see; Made in the acetum on the glass-carbon electrode substrate surface band-COOH owing to being immersed in; Thereby make these-COOH can and L-serine, shitosan between hydrogen bond action takes place, and make L-serine and shitosan can be adsorbed on the electrode basement surface securely;
Fig. 2 is in acetate-sodium acetate buffer solution of different pH, 1.0 * 10
-3The reduction peak current of mol/L ACOP;
Fig. 3 is under the different modifying electrode, 1.0 * 10
-3The cyclic voltammetry curve of mol/L ACOP, wherein, end liquid is that pH is acetate-sodium acetate buffer solution of 4.9, a bare electrode, b glycan modified electrode, c L-serine modified electrode, d L-serine/chitosan-modified electrode;
Fig. 4 is the linear volt-ampere curve under the different ACOP concentration, and end liquid is that pH is acetate-sodium acetate buffer solution of 4.9, and little figure wherein is to be horizontal ordinate with concentration, and peak current is the typical curve that ordinate is done.
Embodiment
Below in conjunction with specific embodiment the present invention is further set forth.
Embodiment 1
The preparation method of electrochemical sensor is:
(1) with the burnishing powder glass-carbon electrode of polishing, makes its substrate surface smooth bright and clean, with absolute ethyl alcohol and distilled water the glass-carbon electrode substrate surface is cleaned successively then, obtain pretreated glassy carbon electrode;
(2) 0.5g shitosan and 0.3g L-serine being joined the 100ml volume fraction is in 1% the acetum, stirs they are fully dissolved;
(3) pretreated glassy carbon electrode is immersed in the prepared solution of step (2), left standstill under the room temperature 3 hours, shitosan and L-serine are adsorbed onto on the electrode basement surface, form L-serine/chitosan complex film;
(4) spend the glass-carbon electrode 2 times of redistilled water cleaning and dipping, remove unnecessary L-serine and shitosan, must be coated with L-serine/chitosan complex film;
(5) be working electrode with L-serine/chitosan-modified glass-carbon electrode, saturated calomel electrode is a contrast electrode, and platinum electrode is an auxiliary electrode, obtains L-serine/chitosan-modified electrochemical sensor.
Embodiment 2
The preparation method of electrochemical sensor is:
(1) with the burnishing powder glass-carbon electrode of polishing, makes its substrate surface smooth bright and clean, with absolute ethyl alcohol and distilled water the glass-carbon electrode substrate surface is cleaned successively then, obtain pretreated glassy carbon electrode;
(2) 0.7g shitosan and 0.5g L-serine being joined the 100ml volume fraction is in 2% the acetum, stirs they are fully dissolved;
(3) pretreated glassy carbon electrode is immersed in the prepared solution of step (2), left standstill under the room temperature 4 hours, shitosan and L-serine are dissolved be attached on the electrode basement surface, form L-serine/chitosan complex film;
(4) spend the glass-carbon electrode 3 times of redistilled water cleaning and dipping, remove unnecessary L-serine and shitosan, must be coated with L-serine/chitosan complex film;
(5) be working electrode with L-serine/chitosan-modified glass-carbon electrode, saturated calomel electrode is a contrast electrode, and platinum electrode is an auxiliary electrode, obtains L-serine/chitosan-modified electrochemical sensor.
Embodiment 3
The preparation method of electrochemical sensor is:
(1) with the burnishing powder glass-carbon electrode of polishing, makes its substrate surface smooth bright and clean, with absolute ethyl alcohol and distilled water the glass-carbon electrode substrate surface is cleaned successively then, obtain pretreated glassy carbon electrode;
(2) 0.6g shitosan and 0.4g L-serine being joined the 100ml volume fraction is in 1% the acetum, stirs they are fully dissolved;
(3) pretreated glassy carbon electrode is immersed in the prepared solution of step (2), left standstill under the room temperature 5 hours, shitosan and L-serine are adsorbed onto on the electrode basement surface, form L-serine/chitosan complex film;
(4) with the glass-carbon electrode of redistilled water cleaning and dipping 2 times, remove unnecessary L-serine and shitosan, must be coated with L-serine/chitosan complex film;
(5) be working electrode with L-serine/chitosan-modified glass-carbon electrode, saturated calomel electrode is a contrast electrode, and platinum electrode is an auxiliary electrode, obtains L-serine/chitosan-modified electrochemical sensor.
Embodiment 4
L-serine/chitosan-modified the electrochemical sensor that utilizes embodiment 1 to make is placed on the electrolytic solution of ACOP under the condition of different pH, measures reduction peak current; Condition determination is, electrolytic solution is the acetate-sodium acetate buffer solution (0.1mol/L) of different acidity, and ACOP concentration is 1.0 * 10
-3Mol/L, assay method are cyclic voltammetry, electric potential scanning scope-0.8～0.8V, and sweep velocity 100mV/s, the visible Fig. 2 of result can be found out by Fig. 2, is that the peak current response is best under 4.9 the condition at pH.
Embodiment 5
Respectively with a bare electrode, b glycan modified electrode, c L-serine modified electrode, the L-serine that d embodiment 1 makes/chitosan-modified electrode places the electrolytic solution of ACOP, measures reduction peak current; Condition determination is, electrolytic solution is acetate-sodium acetate buffer solution (0.1mol/L) of pH 4.9, and ACOP concentration is 1.0 * 10
-3Mol/L; Assay method is a cyclic voltammetry: electric potential scanning scope-0.8～0.8V, sweep velocity 100mV/s, the visible Fig. 3 of test result; Peak current by the glass-carbon electrode of the visible L-serine of Fig. 3/chitosan-modified is maximum; And peak current is minimum on the bare electrode, and the advantage that has had the two through the electrode behind the L-serine/chitosan-modified concurrently be described, can be better to ACOP generation electrochemical response.
Embodiment 6
L-serine/chitosan-modified the electrochemical sensor that utilizes embodiment 1 to make is placed in the ACOP electrolytic solution of variable concentrations, measures reduction peak current; Condition determination is that electrolytic solution is acetate-sodium acetate buffer solution (0.1mol/L) of pH4.9., and assay method is linear voltammetry: sweep limit-0.8～0.8V, sweep velocity 100mV/s.Can find out that peak current is 2.0 * 10 in ACOP concentration
-6～1.0 * 10
-3Become the good linear relation in the scope of mol/L, linear equation is I
p(μ A)=-3.015-0.33C (10
-5Mol/L), related coefficient is 0.99702.Testing result is seen Fig. 4, Fig. 4, and a 0mol/L, b 2.0 * 10
-6Mol/L, c 1.0 * 10
-5Mol/L, d 5 * 10
-5Mol/L, e 1.0 * 10
-4Mol/L, f2.0 * 10
-4Mol/L, g 5.0 * 10
-4Mol/L, h 8.0 * 10
-4Mol/L, i1.0 * 10
-3Mol/L; Detecting among Fig. 4 is limited to 8.3 * 10
-7Mol/L (CL=3Si c/X; CL is a detection limit, and si is the standard deviation of sample measurement reading, and c is the sample size value, and X is a sample measurement reading mean value.)
Claims (6)
1.L-serine/chitosan-modified paracetamol electrochemical sensor is characterized in that: it is working electrode with the glass-carbon electrode, and the glass-carbon electrode surfaces coated is covered with L-serine/chitosan complex film;
The preparation method of L-serine/chitosan complex film is:
(1) glass-carbon electrode is polished successively, polished and cleans, obtain pretreated glassy carbon electrode;
(2) shitosan and L-serine are joined in the acetum, constantly stir and make it dissolving fully; Wherein, the mass and size concentration of shitosan is 0.005～0.007g/mL, and the mass and size concentration of L-serine is 0.003～0.005g/mL;
(3) pretreated glassy carbon electrode that step (1) is obtained immerses in the prepared mixed solution of step (2), leaves standstill under the room temperature 3-5 hour, promptly gets the crude product of the glass-carbon electrode that is coated with L-serine/chitosan complex film;
(4) crude product that makes in the step (3) is cleaned 2-3 time with distilled water, remove unnecessary L-serine and shitosan, dry under the room temperature, promptly get the glass-carbon electrode that surfaces coated is covered with L-serine/chitosan complex film.
2. electrochemical sensor according to claim 1 is characterized in that: the mass concentration of the acetum in the step (1) is 1%～2%.
3. the application of L-serine/chitosan-modified paracetamol electrochemical sensor, it is characterized in that: it can be used for measuring the content of paracetamol in the solution.
4. the application of electrochemical sensor according to claim 3 is characterized in that: use its method of measuring Paracetamol content in the solution to be:
(1) acetaminophen solution to be measured is added in acetate-sodium acetate buffer solution, with this as electrolytic solution;
(2) be working electrode with L-serine/chitosan-modified glass-carbon electrode, saturated calomel electrode is a contrast electrode, and platinum electrode is an auxiliary electrode, places the electrolytic solution described in the step (1), carries out electro-chemical test.
5. the application of electrochemical sensor according to claim 4 is characterized in that, in the described electrolytic solution, acetaminophen solution concentration to be measured is 0～1.0 * 10
-3Mol/L, the pH value of acetate-sodium acetate buffer solution is 4.6～5.3.
6. the application of electrochemical sensor according to claim 5 is characterized in that, pH value the best of described acetate-sodium acetate buffer solution is 4.9.
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| CN103926303A (en) * | 2014-05-05 | 2014-07-16 | 济南大学 | Method for simultaneously determining aminophenol isomers |
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| CN101793862A (en) * | 2010-04-06 | 2010-08-04 | 济南大学 | L-cysteine/chitosan-modified electrochemical sensor and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103926303A (en) * | 2014-05-05 | 2014-07-16 | 济南大学 | Method for simultaneously determining aminophenol isomers |
| CN103926303B (en) * | 2014-05-05 | 2016-04-20 | 济南大学 | A kind of method for Simultaneously test amino phenol isomeride |
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Application publication date: 20120321 |