CN101876645A - Electrochemical sensor for quickly detecting Sudan I in foods and preparation method thereof - Google Patents
Electrochemical sensor for quickly detecting Sudan I in foods and preparation method thereof Download PDFInfo
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- CN101876645A CN101876645A CN 201010192193 CN201010192193A CN101876645A CN 101876645 A CN101876645 A CN 101876645A CN 201010192193 CN201010192193 CN 201010192193 CN 201010192193 A CN201010192193 A CN 201010192193A CN 101876645 A CN101876645 A CN 101876645A
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Abstract
The invention discloses an electrochemical sensor for quickly detecting Sudan I in foods and a preparation method thereof. The preparation method of the sensor comprises the following steps of: uniformly mixing montmorillonite, conductive carbon powder and adhesive at a certain percentage to form a sensitive material; filling the sensitive material in a cavity on the front end of an insulating column and enabling the sensitive material contact with the end of a metal conductor inserted and fixed at the centre of the insulating column. The electrochemical sensor of the invention has the advantages of high sensitivity, low detection limitation, capability of realizing quick detection to the Sudan I in foods, simple and convenient operation, environment-friendliness, wide raw material sources and low cost; moreover, the preparation method is simple.
Description
Technical field
The present invention relates to electrochemical sensor of a kind of fast detecting Sudan I in foods and preparation method thereof, belong to the analytical chemistry field, also belong to the food security field.
Background technology
In food processing process, for improving the organoleptic properties, make it more tempting, usually add some pigments.The pigment that adds can be divided into natural colouring matter and synthetic food color two big classes at present.Natural colouring matter derives from natural products, and is little to the harm of human body.Synthetic food color then is the organic pigment that synthesizes by chemical method, compares with natural colouring matter, and synthetic food color is not only bright in colour, strong coloring force, and stable in properties, cheap, thereby is widely used in food service industry.It is very serious to the harm of human body that yet modern medicine study confirms many synthetic food colors, must strict its consumption of control even ban use of.Sudan red 1 is a kind of azo class pigment of synthetic, is widely used as the especially pigment adjuvant of chilli products of food at present.Yet a large amount of laboratory datas shows Sudan red 1 and may cause cancer that based on this, international cancer research institution belongs to the 3rd class carcinogen with it.China also prohibites the use tonyred in " food additives hygienic standard " in 1996.But many producers still add Sudan red 1 in violation of rules and regulations under the ordering about of interests.This shows that the detection of strengthening Sudan I in foods is very necessary.
The detection method of Sudan red 1 mainly contains chromatography, chromatograph-mass spectrometer coupling method and spectroscopic methodology at present.Chromatography and though the chromatograph-mass spectrometer coupling method is highly sensitive, selectivity good, analysis time is long, needs the operating personnel of large complicated instrument and equipment and specialty, is difficult to realize fast detecting, is not easy to generally promote.Though the required instrument of spectrophotometric method is simple, and is easy and simple to handle, a kind of method for quick of can yet be regarded as, low, the poor selectivity of its sensitivity is not suitable for trace analysis.Different with it is, that electrochemical sensing detects is not only highly sensitive, selectivity is good, and easy and simple to handle, analysis speed is fast, sample pretreatment is simple, required instrument is easy to be portable, thereby is fit to very much the fast detecting of trace components.Contain electroactive azo group in the molecular structure of Sudan red 1, under certain condition can be by electrochemical reduction.Based on this, developed the sensor that multiple electrochemical reduction is measured Sudan red 1.But the most sampling of these sensors mercury is sensitive material, and is not only big to human body harm, and can cause environmental pollution.In addition, these electrochemical sensors are the interference of avoiding the dissolved oxygen DO recovering signal, need logical high purity inert gas (as nitrogen, argon gas etc.) to remove oxygen in the solution before the mensuration, thereby complicated operation, and cause whole analysis time long (about 15～20min).Therefore, violate a ban in fast and convenient, the high sensitivity measuring food of the research environmentally friendly electrochemical sensor of Sudan red 1 still is full of challenge and novelty.
Summary of the invention
The objective of the invention is to remedy the deficiency of above-mentioned technology, electrochemical sensor of a kind of high sensitivity, fast detecting Sudan I in foods easy and simple to handle, eco-friendly and preparation method thereof is provided.
The objective of the invention is to be achieved by the following technical programs:
A kind of electrochemical sensor of fast detecting Sudan I in foods, comprise insulated column and intert and be fixed on the metallic conductor at insulated column center, one end of metallic conductor is positioned at the outside, rear end of insulated column, the front end of insulated column is provided with cavity, sensitive material is filled in this cavity, and contacts with the other end of metallic conductor; Described sensitive material is for comprising the potpourri of polynite, conductive carbon powder and bonding agent at least, and polynite and the conductive carbon powder quality percentage composition in this potpourri is respectively 5%～20% and 60%～90%, and all the other are bonding agent.
The present invention also provides the preparation method of the electrochemical sensor of above-mentioned fast detecting Sudan I in foods, may further comprise the steps: by the quality percentage composition of contained each component in the above-mentioned sensitive material, polynite, conductive carbon powder and bonding agent are mixed, obtain sensitive material, then this sensitive material is filled in the cavity that the insulated column front end is provided with, and makes sensitive material and intert the end of the metallic conductor that is fixed in the insulated column center and contact.
The particle diameter of the above polynite is 50nm～500nm; Conductive carbon powder is dag, acetylene black powder or activated carbon powder, and its particle diameter is 50nm～500nm; Bonding agent is a paraffin oil.
The above cavity is cylindrical, and it highly is 0.5～3mm, and diameter is 1～6mm.
The diameter of the above insulated column is 3～15mm, and used insulating material is teflon, poly-trifluoro-ethylene or polyether-ether-ketone resin.
The above metallic conductor is copper rod, aluminium bar or platinum rod, and its diameter is 0.25～3mm.
Compared with prior art, advantage of the present invention is as follows:
(1) electrochemical sensor of the present invention has high sensitivity
The present invention is with the polynite of the layer structure sensitive material as electrochemical sensor, by its strong accumulation ability, can significantly improve the surface concentration and the electrochemical oxidation signal of Sudan red 1, realizes high sensitivity measuring, detects and is limited to 0.01mg L
-1(be 10ppb, 4.03 * 10
-8Mol L
-1).
(2) electrochemical sensor of the present invention can be realized fast detecting
Polynite has significant enhancement effect to the oxidation of Sudan red 1, and is highly sensitive, thereby need not long-time enrichment when using electrochemical sensor of the present invention to measure Sudan red 1, satisfies fast detecting and requires (minute is lower than 2min).
It is easy and simple to handle when (3) electrochemical sensor of the present invention uses
Based on the electrochemical oxidation signal of Sudan red 1, dissolved oxygen DO is noiseless during mensuration, therefore, does not need long-time deoxygenation before the mensuration, operates very easy.In addition, sensor be all solid state, volume is little, be easy to carry.
(4) electrochemical sensor of the present invention is environmentally friendly
The used sensitive material of the present invention mainly is made of polynite, graphite etc., can not cause environmental pollution, and is to the healthy nothing influence of operator, environmentally friendly.
(5) preparation method of the present invention is simple, and raw material sources are extensive, and cost is low.
Description of drawings
Fig. 1 is the structural representation of the electrochemical sensor of fast detecting Sudan I in foods of the present invention, 1: insulated column, 2: metallic conductor, 3: cavity, 4: sensitive material;
Fig. 2 is 0.5mg L
-1Sudan red 1 at the cyclic voltammetry curve figure of 0.3V～1.0V, curve a for the polynite gained sensor that do not mix to the cyclic voltammetry curve of Sudan red 1, curve b is the cyclic voltammetry curve of the electrochemical sensor of embodiment 2 to Sudan red 1.
Fig. 3 be on the electrochemical sensor of the present invention to the differentiated pulse volt-ampere curve figure of low concentration Sudan red 1, a:0mgL
-1, b:0.05mg L
-1, c:0.1mg L
-1, d:0.2mg L
-1
Embodiment
The present invention is further illustrated below by specific embodiment, but protection scope of the present invention is not limited to following examples.
Embodiment 1:
As shown in Figure 1, electrochemical sensor of the present invention mainly is made up of insulated column 1, metallic conductor 2, cavity 3 and sensitive material 4, the diameter that insulated column 1 adopts usually is 3～15mm, can adopt teflon as insulating material, also can adopt poly-trifluoro-ethylene or polyether-ether-ketone resin; Metallic conductor 2 interts and is fixed in the center of insulated column 1, and the one end is positioned at the outside, rear end of insulated column 1.Metallic conductor can adopt copper rod, aluminium bar or platinum rod, and the diameter that adopts is 0.25～3mm usually.Front end at insulated column 1 is provided with a cavity 3, and cavity 3 is generally cylindrical, and it highly is 0.5～3mm, and diameter is 1～6mm.Sensitive material 4 is the potpourri of polynite, conduction powdered carbon and bonding agent, and polynite and the conductive carbon powder quality percentage composition in this potpourri is respectively 5%～20% and 60%～90%, and all the other are bonding agent; Usually adopting particle diameter is the polynite of 50nm～500nm, the conduction powdered carbon can adopt dag, acetylene black powder or activated carbon powder, particle diameter is generally 50nm～500nm, and bonding agent can adopt paraffin oil, and dag, acetylene black powder, activated carbon powder and paraffin oil adopt the commercially available prod to get final product.Sensitive material 4 is filled in the cavity 3, and contacts with the end of metallic conductor 2.
Embodiment 2:
With particle diameter is that the polynite of 100nm, dag and the paraffin oil that particle diameter is 300nm mix, polynite and the dag quality percentage composition in the gained potpourri is respectively 15% and 73%, all the other are paraffin oil, obtain sensitive material, then sensitive material is filled in the cylindrical cavity of diameter 3mm, high 1mm of embodiment 1 described teflon post front end, this teflon column length 5cm, diameter 6mm, its center is interted and is fixed with the copper rod of diameter 1mm, and sensitive material is contacted with the end of copper rod.On pan paper, polish polishing then, promptly obtain the electrochemical sensor of fast detecting Sudan I in foods.
Embodiment 3:
With particle diameter is that the polynite of 100nm, dag and the paraffin oil that particle diameter is 300nm mix, polynite and the dag quality percentage composition in the gained potpourri is respectively 10% and 75%, all the other are paraffin oil, obtain sensitive material, then sensitive material is filled in the cylindrical cavity of diameter 3mm, high 1mm of embodiment 1 described teflon post front end, this teflon column length 5cm, diameter 6mm, its center is interted and is fixed with the copper rod of diameter 1mm, and sensitive material is contacted with the end of copper rod.On pan paper, polish polishing then, promptly obtain the electrochemical sensor of fast detecting Sudan I in foods.
Embodiment 4:
With particle diameter is that the polynite of 300nm, acetylene black powder and the paraffin oil that particle diameter is 200nm mix, polynite and the acetylene black powder quality percentage composition in the gained potpourri is respectively 12.5% and 65%, all the other are paraffin oil, obtain sensitive material, then sensitive material is filled in the cylindrical cavity of diameter 2mm, high 1.5mm of embodiment 1 described polyether-ether-ketone resin post front end, this polyether-ether-ketone resin column length 5cm, diameter 4mm, its center is interted and is fixed with the aluminium bar of diameter 0.5mm, and sensitive material is contacted with the end of aluminium bar.On pan paper, polish polishing then, promptly obtain the electrochemical sensor of fast detecting Sudan I in foods.
Embodiment 5:
With particle diameter is that the polynite of 100nm, activated carbon powder and the paraffin oil that particle diameter is 100nm～350nm mix, polynite and the activated carbon powder quality percentage composition in the gained potpourri is respectively 14% and 70%, all the other are paraffin oil, obtain sensitive material, then sensitive material is filled in the cylindrical cavity of diameter 3mm, high 1mm of embodiment 1 described poly-trifluoro-ethylene post front end, should gather trifluoro-ethylene column length 5cm, diameter 6mm, its center is interted and is fixed with the platinum rod of diameter 1mm, and sensitive material is contacted with the end of platinum rod.On pan paper, polish polishing then, promptly obtain the electrochemical sensor of fast detecting Sudan I in foods.
Embodiment 6:
With embodiment 2 gained electrochemical sensors to 0.5mg L
-1Sudan red 1 carry out cyclic voltammetry scan at 0.3V～1.0V, potential scanning speed is 100mV s
-1, supporting electrolyte is the phosphate buffered solution of pH=7, and with the method that adopts embodiment 2 but the made sensor of the polynite of not mixing compare, the gained cyclic voltammetry curve is seen Fig. 1.As can be observed from Figure, curve b has a tangible oxidation peak and a very weak reduction peak in the sweep limit of 0.3V～1.0V, illustrate that the oxidation signal sensitivity that detects Sudan red 1 is higher, a compares with curve, the oxidation peak signal of curve b significantly improves, show that polynite has significant enhancement effect to the oxidation of Sudan red 1, the electrochemical sensor that the doping polynite is made can obviously improve the sensitivity of measuring Sudan red 1.
Adopt the electrochemical oxidation behavior of differentiated pulse voltammetry research low concentration Sudan red 1 on electrochemical sensor of the present invention, used electrolyte is the phosphate buffered solution of pH=7, pulse-response amplitude: 50mV, pulse width: 40ms, sweep velocity: 40mV s
-1, enrichment time: 2min, electric potential scanning interval: 0.3V～0.9V, gained differentiated pulse volt-ampere curve is seen Fig. 3.As can be seen from the figure, the concentration when Sudan red 1 is increased to 0.2mg L gradually from 0
-1The time, its oxidation peak current is linear to be increased, and shows that the concentration of this oxidation signal and Sudan red 1 has good linear relationship, can be used as the analyzing and testing signal.
Adopt the Sudan red 1 in electrochemical sensor mensuration chilli powder of the present invention, catsup, the Tabasco sample, testing result such as following table:
The relative standard deviation that each sample replicate determination is 5 times is lower than 5%, and precision was good when electrochemical sensor practical measurement of the present invention was described.In addition, recovery of standard addition illustrates that this sensor has very high accuracy and practicality between 90.7%～93.2%.Detectability (LOD)=3 σ/S, σ are the standard deviation of blank replicate determination 10 times, and S is the slope of typical curve.At this, σ=0.046, S=13.81L mg
-1, calculate detection and be limited to 0.01mg L
-1Show that electrochemical sensor of the present invention can realize the high sensitivity measuring to Sudan I in foods.
Claims (10)
1. the electrochemical sensor of a fast detecting Sudan I in foods, comprise insulated column and intert and be fixed on the metallic conductor at insulated column center, one end of metallic conductor is positioned at the outside, rear end of insulated column, it is characterized in that: the front end of insulated column is provided with cavity, sensitive material is filled in this cavity, and contacts with the other end of metallic conductor; Described sensitive material is for comprising the potpourri of polynite, conductive carbon powder and bonding agent at least, and polynite and the conductive carbon powder quality percentage composition in this potpourri is respectively 5%～20% and 60%～90%, and all the other are bonding agent.
2. according to the electrochemical sensor of the described fast detecting Sudan I in foods of claim 1, it is characterized in that: the particle diameter of described polynite is 50nm～500nm; Conductive carbon powder is dag, acetylene black powder or activated carbon powder, and its particle diameter is 50nm～500nm; Bonding agent is a paraffin oil.
3. according to the electrochemical sensor of the described fast detecting Sudan I in foods of claim 1, it is characterized in that: described cavity is cylindrical, and it highly is 0.5～3mm, and diameter is 1～6mm.
4. according to the electrochemical sensor of the described fast detecting Sudan I in foods of claim 1, it is characterized in that: the diameter of described insulated column is 3～15mm, and used insulating material is teflon, poly-trifluoro-ethylene or polyether-ether-ketone resin.
5. according to the electrochemical sensor of the described fast detecting Sudan I in foods of claim 1, it is characterized in that: described metallic conductor is copper rod, aluminium bar or platinum rod, and its diameter is 0.25～3mm.
6. the preparation method of the electrochemical sensor of the described fast detecting Sudan I in foods of claim 1, it is characterized in that: by the quality percentage composition of contained each component in the described sensitive material of claim 1, polynite, conductive carbon powder and bonding agent are mixed, obtain sensitive material, then this sensitive material is filled in the cavity that the insulated column front end is provided with, and makes sensitive material and intert the end of the metallic conductor that is fixed in the insulated column center and contact.
7. according to the preparation method of the electrochemical sensor of the described fast detecting Sudan I in foods of claim 6, it is characterized in that: the particle diameter of described polynite is 50nm～500nm; Conductive carbon powder is dag, acetylene black powder or activated carbon powder, and its particle diameter is 50nm～500nm; Bonding agent is a paraffin oil.
8. according to the preparation method of the electrochemical sensor of the described fast detecting Sudan I in foods of claim 6, it is characterized in that: described cavity is cylindrical, and it highly is 0.5～3mm, and diameter is 1～6mm.
9. according to the preparation method of the electrochemical sensor of the described fast detecting Sudan I in foods of claim 6, it is characterized in that: the diameter of described insulated column is 3～15mm, and used insulating material is teflon, poly-trifluoro-ethylene or polyether-ether-ketone resin.
10. according to the preparation method of the electrochemical sensor of the described fast detecting Sudan I in foods of claim 6, it is characterized in that: described metallic conductor is copper rod, aluminium bar or platinum rod, and its diameter is 0.25～3mm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102419345A (en) * | 2011-09-07 | 2012-04-18 | 苏州科技学院 | Graphene-starch electrochemical sensor, and preparation method and application thereof |
| CN102749380A (en) * | 2012-07-16 | 2012-10-24 | 常州大学 | Electrochemical method for detecting Sudan red I |
| CN104034766A (en) * | 2014-06-20 | 2014-09-10 | 遵义师范学院 | Preparation method and application of electrochemical transducer for fast detecting Sudan red in food |
| CN107402246A (en) * | 2017-07-13 | 2017-11-28 | 信阳师范学院 | Electrode based on nanogold/nanometer acetylene black modification and its preparation method and application |
| CN112881504A (en) * | 2021-01-19 | 2021-06-01 | 武汉工程大学 | Montmorillonite-based electrochemical sensor and preparation method and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102419345A (en) * | 2011-09-07 | 2012-04-18 | 苏州科技学院 | Graphene-starch electrochemical sensor, and preparation method and application thereof |
| CN102419345B (en) * | 2011-09-07 | 2014-08-06 | 苏州科技学院 | Graphene-starch electrochemical sensor, and preparation method and application thereof |
| CN102749380A (en) * | 2012-07-16 | 2012-10-24 | 常州大学 | Electrochemical method for detecting Sudan red I |
| CN102749380B (en) * | 2012-07-16 | 2014-05-21 | 常州大学 | Electrochemical method for detecting Sudan red I |
| CN104034766A (en) * | 2014-06-20 | 2014-09-10 | 遵义师范学院 | Preparation method and application of electrochemical transducer for fast detecting Sudan red in food |
| CN107402246A (en) * | 2017-07-13 | 2017-11-28 | 信阳师范学院 | Electrode based on nanogold/nanometer acetylene black modification and its preparation method and application |
| CN107402246B (en) * | 2017-07-13 | 2019-11-05 | 信阳师范学院 | Based on nanogold/nanometer acetylene black modification electrode and its preparation method and application |
| CN112881504A (en) * | 2021-01-19 | 2021-06-01 | 武汉工程大学 | Montmorillonite-based electrochemical sensor and preparation method and application thereof |
| CN112881504B (en) * | 2021-01-19 | 2022-08-02 | 武汉工程大学 | Montmorillonite-based electrochemical sensor and preparation method and application thereof |
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Application publication date: 20101103 |