CN111650264A - Method for detecting artificially synthesized pigment by derivative voltammetry - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000004832 voltammetry Methods 0.000 title claims abstract description 35
- IINNWAYUJNWZRM-UHFFFAOYSA-L erythrosin B Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(I)C(=O)C(I)=C2OC2=C(I)C([O-])=C(I)C=C21 IINNWAYUJNWZRM-UHFFFAOYSA-L 0.000 claims abstract description 11
- 235000012732 erythrosine Nutrition 0.000 claims abstract description 11
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- 229940011411 erythrosine Drugs 0.000 claims abstract description 11
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- 240000001592 Amaranthus caudatus Species 0.000 claims abstract description 9
- 235000005979 Citrus limon Nutrition 0.000 claims abstract description 9
- 244000131522 Citrus pyriformis Species 0.000 claims abstract description 9
- 235000012735 amaranth Nutrition 0.000 claims abstract description 9
- 239000004178 amaranth Substances 0.000 claims abstract description 9
- 235000012730 carminic acid Nutrition 0.000 claims abstract description 9
- 239000007853 buffer solution Substances 0.000 claims description 12
- 239000007836 KH2PO4 Substances 0.000 claims description 9
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 9
- 239000008151 electrolyte solution Substances 0.000 claims description 7
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 5
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
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- 229910000397 disodium phosphate Inorganic materials 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 23
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- 239000003086 colorant Substances 0.000 abstract description 9
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000000840 electrochemical analysis Methods 0.000 abstract description 5
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- 239000011734 sodium Substances 0.000 description 8
- 230000009467 reduction Effects 0.000 description 7
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 5
- 229910052753 mercury Inorganic materials 0.000 description 5
- 230000035945 sensitivity Effects 0.000 description 5
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000005375 photometry Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
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- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- 238000012569 chemometric method Methods 0.000 description 2
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- NPOYJZOTOXKWCU-UHFFFAOYSA-N 1-amino-2h-naphthalen-1-ol Chemical compound C1=CC=C2C(N)(O)CC=CC2=C1 NPOYJZOTOXKWCU-UHFFFAOYSA-N 0.000 description 1
- JBIJLHTVPXGSAM-UHFFFAOYSA-N 2-naphthylamine Chemical compound C1=CC=CC2=CC(N)=CC=C21 JBIJLHTVPXGSAM-UHFFFAOYSA-N 0.000 description 1
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 231100000315 carcinogenic Toxicity 0.000 description 1
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- CEZCCHQBSQPRMU-UHFFFAOYSA-L chembl174821 Chemical compound [Na+].[Na+].COC1=CC(S([O-])(=O)=O)=C(C)C=C1N=NC1=C(O)C=CC2=CC(S([O-])(=O)=O)=CC=C12 CEZCCHQBSQPRMU-UHFFFAOYSA-L 0.000 description 1
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- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
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- 230000001988 toxicity Effects 0.000 description 1
- 238000001075 voltammogram Methods 0.000 description 1
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- 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
- G01N27/416—Systems
- G01N27/48—Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
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Abstract
The invention provides a method for detecting artificially synthesized pigment by using derivative voltammetry. The invention establishes a differential voltammetry for simultaneously measuring five mixed artificially synthesized pigments on the basis of an electrochemical analysis method. The method can simply, conveniently and quickly detect the multi-component colorant mixture, and has good anti-interference performance and lower detection limit. The detectable synthetic pigment amaranth has a detection limit of 0.03 mu g/mL, sunset yellow of 0.005 mu g/mL, lemon yellow of 0.005 mu g/mL, carmine of 0.05 mu g/mL, and erythrosine of 0.05 mu g/mL.
Description
Technical Field
The invention belongs to the field of electrochemical detection, and relates to a method for detecting artificially synthesized pigment by using a derivative voltammetry method.
Background
The food colorant is divided into natural pigment and synthetic pigment, and the synthetic pigment has the advantages of bright color, strong tinting strength, stable property, difficult fading, low consumption, free color matching and low price. However, the synthetic pigment is mainly synthesized by taking benzene, toluene, naphthalene and the like as raw materials through chemical synthesis, and mainly belongs to aniline pigments. On one hand, the synthetic pigments have certain toxicity due to the mixed intermediate products, and on the other hand, some pigments can form carcinogenic substances beta-naphthylamine and alpha-amino naphthol in human bodies. Therefore, the application range, the application type and the usage amount are strictly controlled in various countries. China permits the use of 10 pigments, such as sunset yellow, lemon yellow, brilliant blue, indigo, carmine, amaranth, erythrosine, allura red, new red, acid red and the like. The method is used for accurately, qualitatively and quantitatively detecting the artificially synthesized coloring agent in the food, which is very important for the health of consumers.
At present, the analysis of the synthetic food pigment is mainly performed by HPLC, thin layer chromatography, photometry and polarography or voltammetry, and for the analysis of a multi-component colorant mixture, when the components are more, the chromatography is the first analysis method. For mixtures of no more than four component colorants, the use of photometry in combination with some chemometric methods gives better results. In this regard, some laboratory workers may have difficulty in performing specific procedures if simultaneous detection of multiple components is considered, and photometry requires the combination of some chemometric methods to process the results. Mass spectrometry technology is applied to the field, and the resolution capability and the detection limit are greatly improved, but the high cost of instruments is the fatal weakness of the popularization of the technology. In addition, chromatography, mass spectrometry or photometry requires a certain step of pretreatment when analyzing an actual sample, which may be troublesome and time-consuming for the actual analysis work. Capillary electrophoresis techniques also have application in this regard. Compared with the method, the application of polarography or voltammetry to the determination of the coloring agent has the characteristics of cheap instrument and simple and quick operation.
The electrochemical analysis method can make more choices for detection objects according to the diversity of the method, the change and the combination of an electrode system and a measurement system; on the other hand, different substances have different voltammetric responses on different electrode materials and in different base solutions, and have potential capability of simultaneously detecting multiple components. Most of the synthetic dyes have conditions for establishing electrochemical analysis methods because they contain an electrically active group such as azo or hydroxy in their structure. In the process of consulting literature, the differential voltammetry is applied to the detection of the coloring agent, most of the detection is carried out on a single component, and the detection is carried out on two components, so that simultaneous measurement reports of multi-component mixtures are rare. Since the coloring agent in food is basically composed of more than one variety, the importance of establishing a multi-component simultaneous detection technology, either in improving the analysis detection level or in actual work, is obvious.
The application of the electroanalytical chemistry method to the analysis and detection of the multi-component colorant mixture not only can expand the application range of the electroanalytical chemistry, but also more importantly provides a cheap, simple, convenient, rapid and accurate detection method in daily analysis so as to adapt to the requirement of the daily analysis.
Disclosure of Invention
The invention aims to provide a method for detecting artificially synthesized pigments by using derivative voltammetry.
The method specifically adopted by the invention comprises the following steps: a three-electrode system is adopted, a suspended mercury electrode is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, and the mixed pigment is subjected to experimental condition optimization selection and qualitative and quantitative analysis by adopting a linear scanning differential voltammetry method for 1.5 times.
The invention selects NaAc-Hac and Na2HPO4-KH2PO4And NH3-NH4Three kinds of buffer solutions of Cl are taken as research objects, the separation and measurement results of the mixed pigments in neutral, acidic and alkaline are respectively observed, and the results show that Na is used as the Na2HPO4-KH2PO4When the buffer solution (PBS) is used as a base solution, the reduction peaks of various pigments are moderate in size, the images are clear, the separated potentials are large, and the separation and the measurement are easy. PBS was therefore chosen as the base solution.
Further, Na is used2HPO4-KH2PO4The buffer solution is an electrolyte solution.
The differential voltammetry test is carried out by selecting buffer solutions with different concentrations under the same condition, and the result shows that the peak shape in a scanning graph using 0.1mol/L PBS solution as base solution is most acute and regular, and the sensitivity is higher.
The influence of the pH value of the buffer solution on the scanning graph is large, when the pH value is small, the peak shape becomes irregular, the sensitivity is low, when the pH value is large, although the sensitivity is high and the peak shape is sharp, the mixed pigment is difficult to separate and detect, so that the optimal pH value is obtained by selecting the buffer solutions with different pH values in a certain range to detect under the same condition and comparing.
Further, said Na2HPO4-KH2PO4The concentration of the buffer solution is 0.08-0.15mol/L, preferably 0.10 mol/L; the pH is 5.8-7.4, preferably 6.6.
As the adsorption of the pigment on the mercury-suspended electrode belongs to neutral adsorption, a method of enriching for a period of time at a certain potential can be adopted to enrich trace pigment in a solution to be detected on the surface of the electrode, and then linear scanning is carried out to ensure that the pigment is subjected to reduction reaction on the surface of the electrode, thereby improving the sensitivity of the experiment and reducing the detection limit. The optimum adsorption potential of the mercury electrode to the mixed pigment is in the range of 0 to-0.4V, so the enrichment potential should be selected in this region. The invention selects different enrichment potentials to test under the same condition, and finally selects the optimal enrichment potential to be-0.15V.
Further, the enrichment potential of the differential voltammetry was-0.15V.
The rest time can influence the detection result, and because different pigments have different adsorption strengths on the surface of the electrode, competitive adsorption exists, namely the pigment with strong adsorption squeezes the pigment with weak adsorption, so that the peak current of certain pigments with weak adsorption is reduced on the contrary along with the increase of the enrichment time, and the optimal rest time is selected to be 120 seconds in order to simultaneously detect five synthetic pigments.
Further, the resting time of the differential voltammetry was 120 seconds.
Further, the scanning speed of the differential voltammetry is 0.05V/s.
Further, the mixed pigments are respectively: the content of amaranth is as follows,
the color of the lemon is yellow,
the color of the carmine is shown in the formula,
the color of the sun is yellow,
the preparation of the erythrosine is prepared from the raw materials of erythrosine,
the structural formulas of five pigments of amaranth, sunset yellow, lemon yellow, carmine and erythrosine all contain reducible azo, and the electrode reactions are inferred to be all caused by reduction of azo groups according to the electrode behaviors, and the specific reaction mechanism is as follows:
Ar-N＝N-Ar′→[Ar-N＝N-Ar′]ads(formula 1)
[Ar-N＝N-Ar′]ads+2e+2H2O→Ar-NH-NH-Ar′+2OH-(formula 2)
And (3) performing cyclic voltammetry detection on the five pigments, and displaying that only a reduction peak of the pigments appears at a corresponding potential without an oxidation peak, wherein the reduction peak is gradually reduced after multiple scans, which indicates that the electrode reaction belongs to an irreversible reduction reaction.
Through the influence of an electrocapillary curve and static time before scanning, the relation between the peak height and the mercury column height, the influence of a surfactant (sodium dodecyl sulfate), a cyclic voltammogram and other mechanism tests, the reduction waves of the five pigments are absorption reduction waves and are caused by hydrogenation reduction of azo groups in the structure.
As shown in fig. 1, in order to detect the differential voltammetry curve of the five mixed pigments of the invention, a three-electrode system is specifically adopted, and a polar spectrogram obtained by scanning amaranth, sunset yellow, lemon yellow, carmine and erythrosine mixed pigments is obtained by adopting a Linear Scanning (LSV) differential voltammetry method for 1.5 times. As can be seen from the figure, the detected mixed pigments were characterized according to different peak potentials: amaranth is-0.41V, sunset yellow is-0.46V, lemon yellow is-0.52V, carmine is-0.64V, and erythrosine is-0.78V. The peak potential in different sample solutions is possible to generate positive shift or negative shift, and the method can adopt the standard addition, thereby proving that the method designed by the invention can simultaneously detect five mixed artificial pigments.
As shown in fig. 2, for the standard curve chart of the detection of the synthetic pigments (a) amaranth, (b) sunset yellow, (c) lemon yellow, (d) carmine and (e) erythrosine according to the present invention, the linear analysis of the five mixed pigments can be performed, and the linear range and detection limit data of the five pigments are calculated as follows:
after data processing, the method provided by the invention can be proved to be capable of accurately detecting five mixed artificial pigments.
FIG. 3 is a graph showing the electric capillary curve of the present invention for detecting blank base solution and five synthetic pigments. As can be seen, the electrocapillary curve positions of the various pigments are lower than those of the blank base solution (0.1mol/LPBS, pH 6.6). The bulges with sharp drop at corresponding potential indicate that the five pigments have stronger adsorbability on the mercury electrode and belong to neutral adsorption. Therefore, in the experiment, a certain potential is applied to the electrode to enrich the pigment in the solution, so that the analysis sensitivity can be improved and the detection limit can be reduced.
The invention establishes a differential voltammetry for simultaneously measuring five mixed artificially synthesized pigments on the basis of an electrochemical analysis method. The method can simply, conveniently and quickly detect the multi-component colorant mixture, and has good anti-interference performance and lower detection limit.
The invention has the beneficial effects that:
(1) the invention establishes a differential voltammetry method for simultaneously measuring five mixed artificially synthesized pigments on the basis of an electrochemical analysis method, has simple detection method, can be matched with a common electrode for detection, and has good anti-interference performance and lower detection limit.
(2) The preparation method is simple and feasible, has low cost, and does not need special environment and large instruments.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is a differential voltammogram of the present invention for detecting five mixed pigments;
FIG. 2 is a graph showing standard tests for the detection of the synthetic pigments (a) amaranth, (b) sunset yellow, (c) lemon yellow, (d) carmine, and (e) erythrosine according to the present invention;
FIG. 3 is a graph of an electrocapillary tube for detecting a blank base solution and five synthetic pigments according to the present invention.
Detailed Description
In order that the objects, aspects and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the following detailed description and the accompanying drawings.
Example 1
Detecting the artificially synthesized pigment by using derivative voltammetry:
a three-electrode system is adopted, a mercury-suspended electrode is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, and the mixed pigment is subjected to qualitative and quantitative analysis by adopting a linear scanning differential voltammetry method for 1.5 times. Specifically, 0.10mol/L of Na is adopted2HPO4-KH2PO4The buffer solution is an electrolyte solution, the pH of the electrolyte solution is 6.6, the enrichment potential is set to be-0.15V, the rest time is 120 seconds, and the scanning speed is 0.05V/s.
Example 2
Detecting the artificially synthesized pigment by using derivative voltammetry:
a three-electrode system is adopted, a mercury-suspended electrode is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, and the mixed pigment is subjected to qualitative and quantitative analysis by adopting a linear scanning differential voltammetry method for 1.5 times. Specifically, 0.15mol/L of Na is adopted2HPO4- KH2PO4The buffer solution is an electrolyte solution, the pH of the electrolyte solution is 6.6, the enrichment potential is set to be-0.15V, the rest time is 120 seconds, and the scanning speed is 0.05V/s.
Example 3
Detecting the artificially synthesized pigment by using derivative voltammetry:
adopts a three-electrode system, uses a suspended mercury electrode as a working electrode and an Ag/AgCl electrode as a reference electrodeThe electrode and the platinum wire electrode are counter electrodes, and the mixed pigment is qualitatively and quantitatively analyzed by adopting a linear scanning differential voltammetry method for 1.5 times. Specifically, 0.10mol/L of Na is adopted2HPO4- KH2PO4The buffer solution is electrolyte solution with pH of 7.4, set enrichment potential of-0.15V, rest time of 120 s, and scanning speed of 0.05V/baseds。
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single technical solution, and such description is for clarity only, and those skilled in the art should take the description as a whole, and the technical solutions in the embodiments may be combined appropriately to form other embodiments that those skilled in the art can understand. The technical details not described in detail in the present invention can be implemented by any of the prior arts in the field. In particular, all technical features of the invention which are not described in detail can be achieved by any prior art.
Claims (7)
1. A method for detecting artificially synthesized pigment by using a derivative voltammetry method is characterized in that a three-electrode system is adopted, a mercury-suspended electrode is used as a working electrode, an Ag/AgCl electrode is used as a reference electrode, a platinum wire electrode is used as a counter electrode, and the mixed pigment is qualitatively and quantitatively analyzed by adopting the differential voltammetry method of linear scanning for 1.5 times.
2. The method for detecting artificially synthesized pigments by using derivative voltammetry as claimed in claim 1, wherein the method comprisesWith Na2HPO4 -KH2PO4The buffer solution is an electrolyte solution.
3. The method for detecting artificially synthesized pigment by using derivative voltammetry as claimed in claim 2, wherein the Na is2HPO4 -KH2PO4The concentration of the buffer solution is 0.08-0.15mol/L, preferably 0.10 mol/L; the pH is 5.8-7.4, preferably 6.6.
4. The method for detecting artificially synthesized pigments by using derivative voltammetry, according to claim 1, wherein the enrichment potential of the differential voltammetry is-0.15V.
5. The method for detecting artificially synthesized pigments by using derivative voltammetry as claimed in claim 1, wherein the resting time of the differential voltammetry is 120 seconds.
6. The method for detecting artificial pigment by derivative voltammetry as claimed in claim 1, wherein the sweep rate of said differential voltammetry is 0.05V/s.
7. The method for detecting the artificially synthesized pigment by the derivative voltammetry according to claim 1, wherein the mixed pigments are respectively: the content of amaranth is as follows,
the color of the lemon is yellow,
the color of the carmine is shown in the formula,
the color of the sun is yellow,
the preparation of the erythrosine is prepared from the raw materials of erythrosine,
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| 罗利军等: "导数伏安法同时测定5种混合人工合成色素", 《分析试验室》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114894878A (en) * | 2022-05-24 | 2022-08-12 | 福州大学 | Method for measuring concentration of inhibitor in acidic copper plating solution |
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