A sensitive sensor based on graphitic carbon nitride/1-butyl-3-methylimidazolium hexafluorophosphate ionic liquids modified carbon paste electrode for sensing of carmoisine dye in food samples: https://dx.doi.org/10.5599/jese.1396 1143 J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152; https://dx.doi.org/10.5599/jese.1396 Open Access : : ISSN 1847-9286 www.jESE-online.org Original scientific paper A sensitive sensor based on graphitic carbon nitride/1-butyl-3-me- thylimidazolium hexafluorophosphate ionic liquids modified car- bon paste electrode for sensing of carmoisine dye in food samples Sayed Zia Mohammadi1 and Farideh Mousazadeh2, 1Department of Chemistry, Payame Nour University, Tehran, Iran 2School of Medicine, Bam University of Medical Sciences, Bam, Iran Corresponding author: faridehmousazadeh1398@gmail.com Received: June 4, 2022; Accepted: June 20, 2022; Published: August 26, 2022 Abstract The electrochemical sensors for carmoisine detection were explored and applied in the field of food safety because of the striking merits of fast detection speed, high sensitivity and easy operation. Herein, we developed a high-performance electrochemical carmoisine sensor based on g-C3N4 and ionic liquids (ILs), prepared by a one-pot hydrothermal synthesis method. Most importantly, the sensing performances of electrochemical carmoisine sensors based on g-C3N4 (graphitic carbon nitride)/IL (1-butyl-3-methylimidazolium hexafluorophosphate) are better than the bare carbon paste electrode (CPE) sensors. The detection limit of this sensor (g-C3N4/ILs/CPE) determined via differential pulse voltammetry was 0.1 µM over a wide linear range of 0.4–125.0 µM. Keywords Electrochemical sensors; differential pulse voltammetry; food analysis; chemically modified electrodes Introduction Color additives were used by the ancient Egyptians. Historians estimated that colored food appeared by 1500 B.C. Now, food manufacturers deem color as a vital criterion for food choice; thus, synthetic colorants are now being widely used due to their coloring properties, uniformity, stability, low cost, and availability in many hues, which overall increase the esthetic quality (Mpountoukas Below the acceptable daily intake (ADI) limit, the intake of artificial colorants seems to be safe. However, consumption of high concentrations of these artificial colorants may result in many ailments, especially in children, due to their low body weights. Children are the major consumers of colored food in developing countries, and thus, they are at high risk because they often exceed prescribed ADIs [1,2]. Carmoisine dye is a synthetic azo food dye broadly used in food industries to get on red color products. Because this dye is not carcinogenic and toxic, it is utilized as a coloring agent in https://dx.doi.org/10.5599/jese.1396 https://dx.doi.org/10.5599/jese.1396 http://www.jese-online.org/ mailto:faridehmousazadeh1398@gmail.com J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 SENSOR BASED ON g-C3N4/IONIC LIQUIDS MODIFIED CPE 1144 confectionery, ice cream, gelatin desserts drinks, medicine and cosmetics. However, at high doses of carmoisine, the vital organs in the human body, such as the liver and kidneys, can be damaged and the gens can be changed from the mediated reaction of this dye with DNA. In Europe, carmoisine is authorized for use in certain foods and beverages, such as cheeses, dried fruit, and some alcoholic beverages, and is permitted for use as an excipient in medications. Therefore, the determination of this type of food additive is very important in food products [3-5]. Until now, different methods such as chromatography, spectroscopy and liquid-liquid microex- traction have been reported for the determination of carmoisine dye [6-10]. In addition, volta- mmetry was also used to determine carmoisine dye based on its electrochemical activity [11,12]. Electrochemical sensors showed many advantages for the analysis of food compounds due to their fast response. High oxidation/reduction over-potential and low sensitivity of electroactive compounds at the surface of unmodified electrodes are major problems for trace level analysis [13- 20]. Therefore, modified electrodes were suggested as highly powerful tools for trace-level analysis of electroactive compounds. According to the previously published papers, room temperature ionic liquids and nanomaterials can improve the sensitivity of electrochemical sensors for the analysis of electroactive materials [21-35]. Room temperature ionic liquids (RTILs) are an exciting class of solvent, receiving much attention in recent years as a replacement for conventional solvents in many applications. As their name suggests, ionic liquids are salts that melt below 100 °C and room temperature ionic liquids exist in the liquid state at room temperature (25 °C). They are typically comprised of a bulky organic cation (e.g., imidazolium, tetraalkylammonium or pyrrolidinium) paired with an inorganic/organic anion (e.g., tetrafluoroborate, hexafluorophosphate, bis(triflurormethylsulfonyl)imide). RTILs possess several archetypal properties such as low volatility, high physical and chemical stability, wide electrochemical windows, intrinsic conductivity, wide liquid range, high polarity and the ability to dissolve a wide range of compounds. In addition to the use of RTILs in applications such as catalysis, ‘green’ chemistry, organic reactivity, analytical methods, biocatalysis and enzymes and applications in the chemical industry, they have also become recognized as ideal alternative electrolytes for use in many electrochemical devices, such as actuators, capacitors, batteries, fuel cells, solar cells and sensors [36-38]. Nanomaterials have become the most popular material due to their unique properties of low cost, large surface area, good biocompatibility and distinct catalytic activity [39]. Many researchers have been studying nanomaterials for electrochemical sensors [40-47]. Intensive research on g-C3N4 has been conducted since its appearance. With amazing properties of high chemical and thermal stability, medium energy gap (2.7 eV), ideal electronic structure, non-toxic, low density and high conductivity, g- C3N4 has become one of the hottest materials for modifying electrochemical sensors [48-50]. Therefore, in the present study, we fabricated a highly sensitive voltammetric sensor based on a carbon paste electrode modified with g-C3N4 and ionic liquids for the analysis of carmoisine in food samples. The fabricated sensor showed good electrical conductivity compared to the unmodified electrode and improved the quality of the carbon paste electrode for analysis of carmoisine in food samples. Experimental Apparatus and chemicals All the electrochemical measurements were carried out on a PGSTAT302N potentiostat/gal- vanostat Autolab consisting of a traditional three-electrode system: a bare or modified CPE as the S. Z. Mohammadi and F. Mousazadeh J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 http://dx.doi.org/10.5599/jese.1396 1145 working electrode, an Ag/AgCl as the reference electrode and a Pt wire as a counter electrode. Solution pH values were determined using a 713 pH meter combined with a glass electrode (Metrohm, Switzerland). Carmoisine and other chemicals used were analytical grade and were purchased from Merck. Ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was purchased from Sigma Aldrich co. Graphitic carbon nitride nanostructures were synthesized in our laboratory and a typical SEM is shown in Figure 1. Figure 1. FE-SEM image of g-C3N4 Preparation of g-C3N4/ILs/CPE g-C3N4/ILs/CPE was prepared by mixing 0.04 g of g-C3N4 with 0.96 g graphite powder and approximately 0.8 mL of ionic liquids with a mortar and pestle. The paste was then packed into the end of a glass tube (3.4 mm internal diameter and 15 cm long). A copper wire inserted into the carbon paste provided the electrical contact. For comparison, ionic liquids/carbon paste electrode (IL/CPE) in the absence of g-C3N4, (g-C3N4/CPE) consistent with g-C3N4 powder and paraffin oil, and bare carbon paste electrode consisting of graphite powder and paraffin oil were also prepared in the same way. The surface area of g-C3N4/ILs/CPE and the bare CPE were obtained by CV using 1 mM K3Fe(CN)6 at different scan rates. Using the Randles-Sevcik formula for g-C3N4/ILs/CPE, the electrode surface was found 0.288 cm2 which was about 3.2 times greater than bare CPE. Results and discussion Electrochemical behavior of carmoisine at the surface of various electrodes The effect of the electrolyte pH on the oxidation of 35.0 μM carmoisine was investigated at g-C3N4/ILs/CPE using differential pulse voltammetry (DPV) measurements in the phosphate- buffered solution (PBS) in the pH range from 2.0 to 9.0. According to the results, the oxidation peak current of carmoisine depends on the pH value and increases with increasing pH until it reaches the maximum at pH 7.0, and then decreases with higher pH values. The optimized pH corresponding to http://dx.doi.org/10.5599/jese.1396 J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 SENSOR BASED ON g-C3N4/IONIC LIQUIDS MODIFIED CPE 1146 the higher peak current was 7.0, indicating that protons are involved in the reaction of carmoisine oxidation. The electrochemical behavior of carmoisine was investigated by differential pulse voltammetry. The differential pulse voltammograms obtained using the bare CPE (curve d), ILs/CPE (curve c), g-C3N4/CPE (curve b) and g-C3N4/ILs/CPE (curve a) in 0.1 M PBS (pH 7.0) in the presence of 60.0 μM carmoisine are shown in Figure 2. On a bare CPE, an irreversible signal with a low oxidation current of 2.5 μA was obtained with a peak potential of 740 mV. After modifying the electrode with ILs/CPE, and g-C3N4/CPE, the peak current increased up to 6.06 and 8.93 μA, respectively. In contrast, g-C3N4/ILs/CPE exhibited an enhanced sharp anodic peak current (Ipa = 12.0 μA) at a much lower overpotential Ep = 450 mV. These results confirmed that the g-C3N4/ILs improved the sensitivity of the modified electrode by enhancing peak current and decreasing the overpotential of the oxidation of carmoisine. E / mV vs. Ag/AgCl/KCl Figure 2. Differential pulse voltammograms of (a) g-C3N4/ILs/CPE, (b) g-C3N4 /CPE, (c) ILs/CPE and (d) bare CPE in 0.1 M PBS (pH 7.0) in the presence of 60.0 μM carmoisine at the scan rate 50 mV s-1 Effect of scan rate on the determination of carmoisine at g-C3N4/ILs/CPE The influence of the scan rate () on the peak currents (Ipa) of carmoisine at g-C3N4/ILs/CPE was investigated by linear sweep voltammetry (LSV). Figure 3 shows the voltammetric response of 35.0 μM carmoisine at g-C3N4/ILs/CPE at different scan rates in the range of 5 to 400 mV s-1. The oxidation peak current of carmoisine increases linearly with increasing scan rate. A linear regression equation was obtained from the plot Ipa and vs. 1/2 (square root of scan rate) as follows; Ipa = 1.5769 ½ – 1.4736 (R2 = 0.9995) for the oxidation process, which indicates that the reaction of carmoisine at g- C3N4/ILs/CPE is diffusion controlled. S. Z. Mohammadi and F. Mousazadeh J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 http://dx.doi.org/10.5599/jese.1396 1147 E / mV vs. Ag/AgCl/KCl Figure 3. Linear sweep voltammograms of g-C3N4/ILs/CPE in 0.1 M PBS (pH 7.0) containing 35.0 μM carmoisine at various scan rates; 1-8 correspond to 5, 15, 45, 75, 100, 200, 300 and 400 mV s-1, respectively. Inset: variation of anodic peak current vs. ν1/2 In addition, the plot of log I vs. E (Tafel plot) is linear, having the following regression equation: log I = 0.1743E + 0.3498 (R2=0.9945) (Figure 4). Assuming that nα=1, the value of α was calculated as 0.71. E / mV vs. Ag/AgCl/KCl Figure 4. Tafel plot for g-C3N4/ILs/CPE in 0.1 M PBS (pH 7.0) in the presence of 35.0 µM carmoisine and scan rate 10 mV s−1 http://dx.doi.org/10.5599/jese.1396 J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 SENSOR BASED ON g-C3N4/IONIC LIQUIDS MODIFIED CPE 1148 Chronoamperometric analysis The analysis of chronoamperometry for carmoisine samples was performed using g-C3N4/ILs/ /CPE vs. Ag/AgCl/KCl (3.0 M) at 0.5 V. The chronoamperometric results of different concentrations of carmoisine in PBS (pH 7.0) are demonstrated in Figure 5. Figure 5. Chronoamperograms obtained at g-C3N4/ILs/CPE in 0.1 M PBS (pH 7.0) for different concentration of carmoisine. The 1-4 correspond to 0.1, 0.3, 0.6 and 1.0 mM of carmoisine. Insets: (A) Plots of I vs. t-1/2 obtained from chronoamperograms 1-4. (B) A plot of the slope of the straight lines against carmoisine concentration The Cottrell equation for chronoamperemetric analysis of electroactive moieties under mass transfer limited conditions is as in equation (1): I = nFAD1/2Cbπ-1/2t-1/2 (1) where D represents the diffusion coefficient (cm2 s-1), and Cb is the applied bulk concentration (mol cm-3). Experimental results of I vs. t-1/2 were plotted in Figure 5A, with the best fits for different concentrations of carmoisine. The resulting slopes corresponding to straight lines in Figure 5A, were then plotted against the concentration of carmoisine (Figure 5B). The mean value of D was determined to be 7.2×10-5 cm2/s according to the resulting slope and Cottrell equation. Calibration curve Because DPV commonly has a higher sensitivity than cyclic voltammetry technology, the DPV technique was applied for the quantitative detection of carmoisine. Figure 6 shows the differential pulse voltammograms of carmoisine at various concentrations using g-C3N4/ILs/CPE. As seen, the oxidation peak currents of carmoisine enhance gradually by increasing its concentrati- on. The oxidation peak currents (Ipa) show a good linear relationship with the concentrations of car- moisine ranging from 0.4 M to 125.0 μM. The linear equation is Ipa = 0.1914CCarmoisine + 0.8746 (R = 0.9992) (Fig. 6 (inset)). Also, the detection limit, Cm, of carmoisine was obtained using the equation (2): Cm = 3sb / m (2) S. Z. Mohammadi and F. Mousazadeh J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 http://dx.doi.org/10.5599/jese.1396 1149 E / mV vs. Ag/AgCl/KCl Figure 6. DPVs of g-C3N4/ILs/CPE in 0.1 M (pH 7.0) containing different concentrations of carmoisine. Numbers 1–10 correspond to 0.4, 2.5, 7.5, 15.0, 25.0, 40.0, 60.0, 80.0, 100.0 and 125.0 µM of carmoisine. Inset: plot of the electrocatalytic peak current as a function of carmoisine concentration in the range of 0.4-125.0 µM In the above equation, m is the slope of the calibration plot (0.1914 μA.μM-1) and sb is the standard deviation of the blank response obtained from 20 replicate measurements of the blank solution. The detection limit is 0.1 μM. Stability, repeatability, and reproducibility The long-term stability test of the g-C3N4/ILs/CPE using DPV was performed at room temperature. The results exhibited that the peak current of 50.0 μM carmoisine at the g-C3N4/ILs/CPE stayed at 93.7 % of its primary current after 7 days, 92.9 % after 14 days, and 89.1 % after 21 days, indicating the superior long-term stability of the proposed sensor. The oxidation of carmoisine (50.0 μM) on the same g-C3N4/ILs/CPE electrode was performed by ten repeated voltammetric measurements, the results of which confirmed the superior repeatability of a fabricated sensor with the relative standard deviation of 3.2 %. Similar conditions were provided for the carmoisine of the response currents of carmoisine (50.0 μM) on five g-C3N4/ILs/CPE, the results of which confirmed the excellent reproducibility of a fabricated sensor with the RSD of value 3.8 %. Analysis of real samples The real samples for the analysis were prepared and quantified by the DPV method. The developed sensor was applied to detect carmoisine in lemon juice and powdered juice samples. The results are summarized in Table 1. Each measurement was repeated three times. The recovery and http://dx.doi.org/10.5599/jese.1396 J. Electrochem. Sci. Eng. 12(6) (2022) 1143-1152 SENSOR BASED ON g-C3N4/IONIC LIQUIDS MODIFIED CPE 1150 relative standard deviation (RSD) values confirmed that the g-C3N4/ILs/CPE sensor has a great potential for analytical application. Table 1. The application of g-C3N4/ILs/CPE for determination of carmoisine in real samples (n=3) Sample Concentretion, μM Recovery, % RSD, % Spiked Found Lemon juice 5.0 4.9 98.0 3.1 7.0 7.2 102.9 1.9 Powdered juice 5.5 5.6 101.8 2.2 7.5 7.3 97.3 3.0 Conclusion A facile electrochemical sensor for carmoisine detection was designed and constructed by using g- C3N4/ILs modified carbon paste electrode. The electrochemical sensor possessed excellent performance with wide linear range (0.4-125.0 μM) and a low limit of detection (0.1 μM), which is due to the good rich accessible active sites. Additionally, the as-prepared electrochemical sensor has good selectivity, reproducibility, repeatability, stability, and potential application in real samples. References [1] C. 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This article is an open-access article distributed under the terms and conditions of the Creative Commons Attribution license (https://creativecommons.org/licenses/by/4.0/) https://doi.org/10.5599/jese.956 https://doi.org/10.5599/jese.1112 https://doi.org/10.1016/j.aca.2007.12.011 https://doi.org/10.1016/j.bios.2010.08.064 https://doi.org/10.1016/j.foodchem.2019.01.143 https://doi.org/10.5599/admet.1172 https://doi.org/10.22034/chemm.2020.113388 https://doi.org/10.1016/j.bios.2016.07.086 https://doi.org/10.22034/chemm.2021.118774 https://doi.org/10.1016/j.molliq.2019.01.081 https://doi.org/10.22034/chemm.2021.125035 https://doi.org/10.1039/C8NJ05581E https://doi.org/10.1016/j.jelechem.2018.01.034 https://doi.org/10.22034/chemm.2020.113657 https://doi.org/10.1016/j.carbon.2018.01.008 https://doi.org/10.1016/j.apt.2020.06.024 https://doi.org/10.1016/j.fct.2022.112907 https://creativecommons.org/licenses/by/4.0/) @Article{ZiaMohammadi2022, author = {{Zia Mohammadi}, Sayed and Mousazadeh, Farideh}, journal = {Journal of Electrochemical Science and Engineering}, title = {{A sensitive sensor based on graphitic carbon nitride/1-butyl-3-methylimidazolium hexafluorophosphate ionic liquids modified carbon paste electrode for sensing of carmoisine dye in food samples:}}, year = {2022}, issn = {1847-9286}, month = {aug}, number = {6}, pages = {1143--1152}, volume = {12}, abstract = {The electrochemical sensors for carmoisine detection were explored and applied in the field of food safety because of the striking merits of fast detection speed, high sensitivity and easy operation. Herein, we de­veloped a high-performance electrochemical carmoisine sensor based on g-C3N4 and ionic liquids (ILs), prepared by a one-pot hydrothermal synthesis method. Most importantly, the sensing per­formances of electrochemical carmoisine sensors based on g-C3N4 (graphitic carbon nitride)/IL (1-butyl-3-methylimidazolium hexafluorophosphate) are better than the bare carbon paste electrode (CPE) sensors. The detection limit of this sensor (g-C3N4/ILs/CPE) de­ter­mined via differential pulse voltammetry was 0.1 µM over a wide linear range of 0.4–125.0 µM.}, doi = {10.5599/JESE.1396}, file = {:D\:/OneDrive/Mendeley Desktop/Zia Mohammadi, Mousazadeh - 2022 - A sensitive sensor based on graphitic carbon nitride1-butyl-3-methylimidazolium hexafluorophosphate i.pdf:pdf;:08_jESE_1396_1143-1152.docx:Word_NEW;:www/jESE_V12_No6_1143-1152.pdf:PDF;:www/jESE_V12_No6_1143-1152.pdf:PDF}, keywords = {Electrochemical sensors, chemically modified electrodes, differential pulse voltammetry, food analysis}, publisher = {International Association of Physical Chemists (IAPC)}, url = {https://pub.iapchem.org/ojs/index.php/JESE/article/view/1396}, }