CN113311041A - Electrochemical method for detecting Sudan red in food - Google Patents

Electrochemical method for detecting Sudan red in food Download PDF

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Publication number
CN113311041A
CN113311041A CN202110579539.7A CN202110579539A CN113311041A CN 113311041 A CN113311041 A CN 113311041A CN 202110579539 A CN202110579539 A CN 202110579539A CN 113311041 A CN113311041 A CN 113311041A
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sudan red
electrode
food
detecting
electrochemical method
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周海旭
苏同超
周浩宇
李波
高晗
朱明明
赵岩岩
白秀芝
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Henan Institute of Science and Technology
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Henan Institute of Science and Technology
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • G01N27/308Electrodes, e.g. test electrodes; Half-cells at least partially made of carbon
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/48Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
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Abstract

The invention discloses an electrochemical method for detecting Sudan red in food, which specifically comprises the following steps: (1) preparing an expanded graphite paste electrode; (2) preparing a Sudan red standard solution; (3) drawing a standard curve: taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a Sudan red standard solution, stirring, enriching and scanning to obtain a linear regression equation, and drawing a standard curve; (4) preparing a solution to be detected; (5) and (6) detecting. The three-electrode system disclosed by the invention is simple in structure, wide in detection range and low in detection limit, can be used for stably, quickly and accurately detecting the content of Sudan red in food, and can be repeatedly used for detecting the Sudan red.

Description

Electrochemical method for detecting Sudan red in food
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to an electrochemical method for detecting Sudan red in food.
Background
Sudan red is a chemical coloring agent, mainly used in petroleum, engine oil and other industrial solvents for coloring and brightening shoes, floors and the like. Its chemical composition contains a compound called naphthalene, said material possesses azo structure, and the property of said chemical structure can determine that it possesses carcinogenicity, and possesses obvious toxic action for liver and kidney organs of human body. Because the food dyed by the Sudan red is very bright in color and not easy to fade, people can have strong appetite, and some illegal food enterprises add the Sudan red into the food, such as chilli powder, chilli oil, red bean curd, red-yolk eggs and the like. If the food containing Sudan red is eaten for a long time, the structure of liver DNA can be changed, and liver diseases can be caused.
Common analysis and detection methods of Sudan red include polarography, solid-phase extraction-gas chromatography, thin-layer chromatography, molecular imprinting solid-phase extraction technology and the like, but the methods are not suitable for being widely used for daily food safety supervision and detection. In addition, based on the physicochemical properties of Sudan red, a sample needs to be pretreated, and pretreatment methods include normal-phase solid-phase extraction, liquid-phase micro-extraction, pressurized solvent extraction, ultrasonic-assisted extraction and the like. With the development of the technology, the electrochemical method has the advantages of high sensitivity, easy miniaturization, low cost and the like, and becomes an excellent method for on-site detection of Sudan red.
Therefore, how to develop a rapid, simple and low-cost sudan red detection method is a problem that needs to be solved urgently by those skilled in the art.
Disclosure of Invention
In view of the above, the present invention provides an electrochemical method for detecting sudan red in food, so as to solve the deficiencies in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an electrochemical method for detecting Sudan red in food specifically comprises the following steps:
(1) preparation of expanded graphite paste electrode
Heating and melting the expanded graphite and the solid paraffin, stirring and mixing, filling the mixture into one end of a glass tube after cooling, and inserting a metal rod into the other end of the glass tube to realize circuit connection to obtain an expanded graphite paste electrode for later use;
(2) preparation of standard solution of Sudan red
Firstly weighing a certain amount of Sudan red solid, then adding water to dissolve, diluting and fixing the volume to obtain a series of Sudan red standard solutions with different concentrations;
(3) drawing of standard curve
Taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into the Sudan red standard solution, stirring and enriching, finally scanning by using a differential pulse voltammetry method, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the Sudan red standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring and enriching, then scanning by using a differential pulse voltammetry method, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of Sudan red in the liquid to be detected.
The invention has the beneficial effects that the expanded graphite with a loose porous structure becomes an excellent electrode material due to the characteristics of large specific surface area, high electrochemical activity, low cost and the like, the invention creatively uses an expanded graphite paste electrode as a working electrode, a saturated calomel electrode as a reference electrode and a platinum wire electrode as a counter electrode to obtain a three-electrode system, and the system can effectively improve the current of the oxidation peak of Sudan red on the expanded graphite paste electrode, so that the system has good electrocatalytic performance and conductive performance on the redox reaction of the Sudan red, and the sensitivity of an analysis method is obviously improved.
Further, in the step (1), the mass ratio of the expanded graphite to the solid paraffin is (90-95) to (5-10); heating at 60-70 deg.C for 1-3 min; the metal bar is a copper bar, an iron bar or an aluminum bar.
The expanded graphite paste electrode prepared from the expanded graphite and the solid paraffin has good reproducibility and stability.
Further, in the step (2), the concentration of the Sudan red standard solution is 1-10 μ g/L.
Further, in the steps (3) and (5), the stirring and enriching speed is 100-200r/min, and the time is 6-10 min.
The method has the further beneficial effects that the oxidation peak current of the Sudan red in the standard solution and the solution to be detected on the expanded graphite paste electrode can be conveniently detected through stirring and enrichment, so that the detection accuracy is improved.
Further, in the steps (3) and (5), the scanning voltage is 0.3-0.5V, the potential amplification is 3-6mV, the pulse amplitude is 30-40mV, and the pulse frequency is 40-60 Hz.
The method has the further beneficial effects that through the setting of the parameters, the oxidation peak current values of the standard solution and the liquid to be detected can be efficiently and accurately measured by adopting the differential pulse voltammetry.
Further, in the step (4), the pore diameter of the microporous membrane is 100-1000 nm.
The food residue detection device has the further beneficial effects that residues in food to be detected can be removed through microporous membrane filtration, and the influence of impurities on the detection result of liquid to be detected is avoided.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
the three-electrode system disclosed by the invention is simple in structure, wide in detection range and low in detection limit, can be used for stably, quickly and accurately detecting the content of Sudan red in food, and can be repeatedly used for detecting the Sudan red.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The electrochemical method for detecting Sudan red in food specifically comprises the following steps:
(1) preparation of expanded graphite paste electrode
Heating 90g of expanded graphite and 10g of solid paraffin to 60 ℃ for melting for 3min, stirring and mixing, cooling, filling into one end of a glass tube, inserting a copper rod into the other end of the glass tube to realize circuit connection, and obtaining an expanded graphite paste electrode for later use;
(2) preparation of standard solution of Sudan red
Firstly weighing a certain amount of Sudan red solid, then adding water to dissolve, diluting and fixing the volume to obtain a series of Sudan red standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into a Sudan red standard solution, stirring at the speed of 100r/min for 10min to enrich, finally scanning by using a differential pulse voltammetry method, wherein the scanning voltage is 0.3V, the potential amplification is 3mV, the pulse amplitude is 30mV, the pulse frequency is 40Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the Sudan red standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the aperture of 100nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring at the speed of 100r/min for 10min for enrichment, then scanning by using a differential pulse voltammetry, wherein the scanning voltage is 0.3V, the potential amplification is 3mV, the pulse amplitude is 30mV, and the pulse frequency is 40Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of Sudan red in the liquid to be detected.
Example 2
The electrochemical method for detecting Sudan red in food specifically comprises the following steps:
(1) preparation of expanded graphite paste electrode
Heating 92g of expanded graphite and 8g of solid paraffin to 65 ℃ for melting for 2min, stirring and mixing, cooling, filling into one end of a glass tube, inserting an iron rod into the other end of the glass tube to realize circuit connection, and obtaining an expanded graphite paste electrode for later use;
(2) preparation of standard solution of Sudan red
Firstly weighing a certain amount of Sudan red solid, then adding water to dissolve, diluting and fixing the volume to obtain a series of Sudan red standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into Sudan red standard solution, stirring at the speed of 150r/min for 8min for enrichment, finally scanning by using a differential pulse voltammetry method, wherein the scanning voltage is 0.4V, the potential amplification is 5mV, the pulse amplitude is 35mV, the pulse frequency is 50Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the Sudan red standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the aperture of 500nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring at the speed of 150r/min for 8min for enrichment, then scanning by using a differential pulse voltammetry, wherein the scanning voltage is 0.4V, the potential amplification is 5mV, the pulse amplitude is 35mV, and the pulse frequency is 50Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of Sudan red in the liquid to be detected.
Example 3
The electrochemical method for detecting Sudan red in food specifically comprises the following steps:
(1) preparation of expanded graphite paste electrode
Heating 95g of expanded graphite and 5g of solid paraffin to 70 ℃ for melting for 1min, stirring and mixing, cooling, filling into one end of a glass tube, inserting an aluminum rod into the other end of the glass tube to realize circuit connection, and obtaining an expanded graphite paste electrode for later use;
(2) preparation of standard solution of Sudan red
Firstly weighing a certain amount of Sudan red solid, then adding water to dissolve, diluting and fixing the volume to obtain a series of Sudan red standard solutions with different concentrations (1 mug/L, 2 mug/L, 6 mug/L, 8 mug/L and 10 mug/L);
(3) drawing of standard curve
Taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into Sudan red standard solution, stirring at the speed of 200r/min for 6min for enrichment, finally scanning by using a differential pulse voltammetry method, wherein the scanning voltage is 0.5V, the potential amplification is 6mV, the pulse amplitude is 40mV, the pulse frequency is 60Hz, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the Sudan red standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane with the pore diameter of 1000nm to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring at the speed of 200r/min for 6min for enrichment, then scanning by using a differential pulse voltammetry, wherein the scanning voltage is 0.5V, the potential amplification is 6mV, the pulse amplitude is 40mV, and the pulse frequency is 60Hz, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of Sudan red in the liquid to be detected.
Performance testing
Preparing an expanded graphite paste electrode according to the method of example 2, preparing a sudan red standard solution, drawing a standard curve, sequentially performing ultrasonic extraction and anion solid phase extraction and small column purification on the commercially available chili sauce, dissolving the obtained extract with water, filtering the dissolved extract through a microporous membrane with the pore diameter of 500nm to obtain a solution to be detected, detecting the content of the sudan red in the solution to be detected, and comparing the content of the sudan red with the detection result of HPLC. In parallel with three experiments, the average value is taken, the content of the Sudan red in the chilli sauce detected by the method in example 2 is 0.82mg/L, and the content of the Sudan red in the chilli sauce detected by HPLC is also 0.82 mg/L.
The tests show that the three-electrode system disclosed by the invention is simple in structure, wide in detection range, low in detection limit, capable of stably, quickly and accurately detecting the content of Sudan red in food and capable of being repeatedly used for detecting the Sudan red.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (8)

1. An electrochemical method for detecting Sudan red in food is characterized by comprising the following steps:
(1) preparation of expanded graphite paste electrode
Heating and melting the expanded graphite and the solid paraffin, stirring and mixing, filling the mixture into one end of a glass tube after cooling, and inserting a metal rod into the other end of the glass tube to realize circuit connection to obtain an expanded graphite paste electrode for later use;
(2) preparation of standard solution of Sudan red
Firstly weighing a certain amount of Sudan red solid, then adding water to dissolve, diluting and fixing the volume to obtain a series of Sudan red standard solutions with different concentrations;
(3) drawing of standard curve
Taking an expanded graphite paste electrode as a working electrode, taking a saturated calomel electrode as a reference electrode, taking a platinum wire electrode as a counter electrode to obtain a three-electrode system, then inserting the three-electrode system into the Sudan red standard solution, stirring and enriching, finally scanning by using a differential pulse voltammetry method, obtaining a linear regression equation according to the linear relation between the oxidation peak current value and the concentration of the Sudan red standard solution, and drawing a standard curve;
(4) preparation of the test solution
Sequentially carrying out ultrasonic extraction and anion solid phase extraction and small column purification treatment on a food sample to be detected, dissolving the obtained extract with water, and filtering the dissolved extract through a microporous membrane to obtain a liquid to be detected;
(5) detection of
Inserting the three-electrode system into the liquid to be detected, stirring and enriching, then scanning by using a differential pulse voltammetry method, and calculating according to the oxidation peak current value and a linear regression equation to obtain the content of Sudan red in the liquid to be detected.
2. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein in step (1), the mass ratio of the expanded graphite to the paraffin wax is (90-95) to (5-10).
3. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein the heating temperature in step (1) is 60-70 ℃ for 1-3 min.
4. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein in step (1), the metal bar is a copper bar, an iron bar or an aluminum bar.
5. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein in step (2), the concentration of the Sudan red standard solution is 1-10 μ g/L.
6. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein in steps (3) and (5), the stirring enrichment speed is 100-200r/min, and the time is 6-10 min.
7. The electrochemical method for detecting Sudan red in food according to claim 1, wherein in steps (3) and (5), the scanning voltage is 0.3-0.5V, the potential amplification is 3-6mV, the pulse amplitude is 30-40mV, and the pulse frequency is 40-60 Hz.
8. The electrochemical method for detecting Sudan red in food as claimed in claim 1, wherein in step (4), the pore size of the microporous membrane is 100-1000 nm.
CN202110579539.7A 2021-05-26 2021-05-26 Electrochemical method for detecting Sudan red in food Pending CN113311041A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012134408A1 (en) * 2011-03-31 2012-10-04 Argricultural Research Development Agency Electrochemical detection of capsaicinoid compounds in a sample
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012134408A1 (en) * 2011-03-31 2012-10-04 Argricultural Research Development Agency Electrochemical detection of capsaicinoid compounds in a sample
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

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
中国食品药品检定研究院组织编写: "《食品检验操作技术规范 理化检验》", 31 August 2019, 中国医药科技出版社 *
刘航龙等: "离子液体/石墨烯修饰玻碳电极快速检测辣椒粉中苏丹红Ⅰ", 《广东农业科学》 *

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Application publication date: 20210827