CN104132973A - Preparation method of electrochemical sensor based on graphene film modified electrode - Google Patents
Preparation method of electrochemical sensor based on graphene film modified electrode Download PDFInfo
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- CN104132973A CN104132973A CN201410366336.XA CN201410366336A CN104132973A CN 104132973 A CN104132973 A CN 104132973A CN 201410366336 A CN201410366336 A CN 201410366336A CN 104132973 A CN104132973 A CN 104132973A
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Abstract
According to the invention, an electrochemical sensor based on an electro reduction oxidation graphene film modified glass carbon electrode is prepared and is used for detecting a medicament sibutramine (SHM) for the treatment of obesity. The invention employs a drop coating and electrochemical reduction method, and uses oxidation graphene for modification on glass carbon electrode, so as to prepare a novel electrochemical sensor. The electrochemical sensor involved in the invention shows the characteristics of simpleness, rapidness and high sensitivity in the detection process of SHM in pure samples and biological samples, and can be successfully used for the detection of SHM in human plasma and urine.
Description
Technical field
The present invention relates to a kind of preparation of electrochemical sensor, relate in particular to a kind of preparation method based on electroreduction graphene oxide film modified glass carbon electrode.
Background technology
Sibutramine hydrochloride (SHM), chemistry N-{1-[1-(4-chlorphenyl)-epoxy butyl by name]-3-methyl butyl }-N, N dimethylamine hydrochloride monohydrate, is a kind of medicament that is used for the treatment of obesity.
In human body and pharmaceutical preparation, the quantitative detection of SHM generally adopts spectrophotometric method, high performance liquid chromatography and Using Flow Injection Analysis etc., and these methods have length analysis time, sampling or purification process complexity conventionally, sample need be in shortcomings such as line extractions.Recently a kind of suspension type mercury dropping that detects SHM in beverage and pharmaceutical preparation by voltammetry that had bibliographical information, but this method relates to the use of mercury electrode, and mercury is volatile and poisonous, harmful to environmental and human health impacts.
The method that quantitatively detects SHM is utilized the electrode of Graphene modification in addition, and Graphene is the cellular lattice material of a kind of two-dimentional single carbon atom layer, has very good property, as high specific surface area and significant electricity and heat conductivity etc.While being used as the electrode material of model electrochemical sensor, Graphene can significantly promote electronics to shift, and can be used as the detection of good electrode modification material for bioactive compound.Graphene is very important at the deposition process of electrode surface to fax sense and electro-catalysis application, but the graphene film modified electrode of preparing by electronation graphene oxide sheet has some intrinsic defects, control as bad in film thickness, can introduce toxic chemical etc.
Summary of the invention
For prior art shortcoming, the present invention adopts liquid phase suspending liquid to prepare graphene film by electrochemical reduction graphene oxide, specifically by electrode surface self assembly graphene oxide suspending liquid then the method for electrochemical reduction prepare graphene film.Prepared graphene film is used for modified glass carbon electrode, forms electrochemical sensor, sibutramine hydrochloride (SHM) is detected, and has overcome prior art in the shortcoming of preparing aspect graphene film modified electrode.
The present invention relates to a kind of preparation method of the electrochemical sensor based on electroreduction graphene oxide film modified glass carbon electrode, electrochemical sensor involved in the present invention can be used for sibutramine hydrochloride and detects.
Step of the present invention is as follows:
(1) preparation of graphene oxide: powdered graphite joins in the concentrated sulphuric acid under 0 DEG C of condition, under ice-water bath stirring condition, add potassium permanganate, the mass ratio of powdered graphite and potassium permanganate is 1:6～1:10, preferably 1:8, mass volume ratio (the w/v of powdered graphite and the concentrated sulphuric acid, g/mL) be 1:40～1:50, preferably 1:45.Potpourri stirs then dilute with water at 50 DEG C of 2～3h at 60～80 DEG C, dropwise add 30% hydrogen peroxide, after filtering, after hydrochloric acid solution washing with the above 1:10 of 100mL, wash again until the pH of solution reaches 6.3 grind into powder after 55～80 DEG C of vacuum drying 12～20h of yellow solid that obtain with water.
(2) preparation of electrochemical reduction graphene oxide modified glass carbon electrode (ERGO-GCE): graphene oxide is distributed in the water that microporous barrier leaches, ultrasonic concussion 3～8h forms stable suspending liquid, the graphene oxide suspending liquid of prepared 6～12 μ mol/L is deposited to behind the surface of glassy carbon electrode, dry with infrared lamp, under-1.7V～2.3V voltage, adopt cyclic voltammetry to obtain the graphene oxide of electrochemical reduction for 4～6 times.
The present invention carries out modification with graphene oxide to glassy carbon electrode, has prepared a kind of novel electrochemical sensor.Electrode (ERGO-GCE) after modification is used for the treatment of obesity medicament---the Electrochemical Detection of sibutramine hydrochloride (SHM), ERGO-GCE is the electro-oxidation process of catalysis SHM effectively, can be successfully for the detection of human plasma and urine SHM.The features such as simple, quick, sensitivity is high in the testing process of the electrochemical sensor the present invention relates to SHM in pure sample product and biological sample, are presented.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with implementing, the invention will be further described.
A preparation method for the electrochemical sensor based on electroreduction graphene oxide film modified glass carbon electrode detecting for sibutramine, its step is as follows:
(1) preparation of graphene oxide: 4g powdered graphite joins in the 180mL concentrated sulphuric acid under 0 DEG C of condition, under ice-water bath stirring condition, add 32g potassium permanganate, potpourri stirs 3h and then at 50 DEG C, dilutes with 800mL water at 75 DEG C, dropwise add the hydrogen peroxide of 50mL30%, after hydrochloric acid solution washing with 100mL1:10 after filtering, wash again until the pH of solution reaches 6.3 grind into powder after the 60 DEG C of vacuum drying 15h of yellow solid that obtain with water.
(2) preparation of electrochemical reduction graphene oxide modified glass carbon electrode (ERGO-GCE): graphene oxide is distributed to ultrasonic concussion 3h in the water that microporous barrier leaches and forms stable suspending liquid, the graphene oxide suspending liquid of prepared 6 μ mol/L is deposited to behind the surface of glassy carbon electrode, dry with infrared lamp, then under-1.7V～2.3V voltage, adopt cyclic voltammetry to obtain the graphene oxide of electrochemical reduction for 6 times.
Claims (6)
1. a preparation method for the electrochemical sensor based on graphene oxide film modified electrode, its step is as follows:
(1) preparation of graphene oxide: powdered graphite joins in the concentrated sulphuric acid under 0 DEG C of condition, under ice-water bath stirring condition, add potassium permanganate composition mixture, wherein, powdered graphite and potassium permanganate mass ratio are 1:6～1:10, the mass volume ratio (w/v, g/mL) of powdered graphite and the concentrated sulphuric acid is 1:40～1:50; Said mixture stirs after 2～3h at 60～80 DEG C, dilute with water at 50 DEG C, dropwise add 30% hydrogen peroxide, after hydrochloric acid solution washing with the above 1:10 of 100mL after potpourri filters, wash with water again, until the pH of solution reaches 6.3, grind into powder after 55～80 DEG C of vacuum drying 12～20h of yellow solid that obtain;
(2) preparation of electrochemical reduction graphene oxide modified glass carbon electrode (ERGO-GCE): graphene oxide is distributed in the water that microporous barrier leaches, ultrasonic concussion 3～8h forms stable graphene oxide suspending liquid, the graphene oxide suspending liquid of prepared 6～12 μ mol/L is deposited on the surface of glassy carbon electrode, dry with infrared lamp, under 1.7V～-2.3V voltage, adopt cyclic voltammetry to obtain the graphene oxide of electrochemical reduction for 4～6 times.
2. the preparation method of electrochemical sensor according to claim 1, is characterized in that: described in step (1), the mass ratio of powdered graphite and potassium permanganate is 1:8.
3. the preparation method of electrochemical sensor according to claim 1, is characterized in that: described in step (1), the mass volume ratio (w/v, g/mL) of powdered graphite and the concentrated sulphuric acid is 1:45.
4. the preparation method of electrochemical sensor according to claim 1, is characterized in that: yellow solid described in step (1) under 60 DEG C of conditions, vacuum drying 15h, then grind into powder.
5. the preparation method of electrochemical sensor according to claim 1, is characterized in that: in step (2), prepared graphene oxide suspension concentration is 6 μ mol/L.
6. the purposes of arbitrary electrochemical sensor of claim 1～5 preparation, is characterized in that: described electrochemical sensor is for the detection of sibutramine hydrochloride.
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| CN104477895A (en) * | 2014-12-11 | 2015-04-01 | 百顺松涛（天津）动力电池科技发展有限公司 | Preparation method of nitrogen-doped graphene for cathode of lithium ion battery |
| CN105136886A (en) * | 2015-10-14 | 2015-12-09 | 无锡百灵传感技术有限公司 | Electrode for detecting Sudan red rapidly and quantitatively |
| CN105153340A (en) * | 2015-07-14 | 2015-12-16 | 湘潭大学 | Preparation method of rigid chain liquid crystal polymer material for hydrogen peroxide sensors |
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| CN104477895A (en) * | 2014-12-11 | 2015-04-01 | 百顺松涛（天津）动力电池科技发展有限公司 | Preparation method of nitrogen-doped graphene for cathode of lithium ion battery |
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| CN105136886A (en) * | 2015-10-14 | 2015-12-09 | 无锡百灵传感技术有限公司 | Electrode for detecting Sudan red rapidly and quantitatively |
| CN105136886B (en) * | 2015-10-14 | 2018-05-01 | 广州智谱慧科技有限公司 | A kind of electrode of Quantitative detection tonyred |
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