Removal of chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin residues from citrus by using ozonated water
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Keywords
Abstract
Citrus fruits—oranges, lemons, and grapefruits—are produced and consumed in huge proportions around the globe which contain 91% water and the reason why they are regarded as the most hydrating fruits. Citrus fruits are a vital part of the human diet by providing the essential vitamins, minerals, and antioxidants to the body, but the process of citrus fruits production frequently utilizes the application of pesticides to deal with pests and diseases. Pesticide residues, including chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin, in the fruit can still have an effect on consumers’ health. In this study, the process of ozonation was used to remove pesticide residues from citrus fruits such as in oranges, lemons, and grapefruits. Ozonated water helped in the detection and removal of pesticides residues chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin from citrus fruits. The mean resid-ual level of chlorpyrifos was 0.015 ± 0.004 in oranges, 0.014 ± 0.004 in lemons, and 0.022 ± 0.001 in grapefruits; the bifenthrin level was 0.055 ± 0.004 in oranges, 0.055 ± 0.004 in lemons, and 0.054 ± 0.005 in grapefruits; the lambda-cyhalothrin level was 1.104 ± 0.174 in oranges, 1.056 ± 0.210 in lemons, and 1.208 ± 0.172 in grapefruits; and the carbofuran level was 0.625 ± 0.050 in oranges, 0.616 ± 0.046 in lemons, and 0.616 ± 0.050 in grapefruits. Furthermore, residual percentages of chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin were detected in all citrus fruits, with the results showing that maximum levels of pesticide residues were efficiently removed from citrus fruits at 10 ppm (parts per million) ozonation without any poisoning and deterioration of fruits.
Riferimenti bibliografici
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Islam SU, Ahmed MB, Ahsan H, Lee YS. Recent molecular mechanisms and beneficial effects of phytochemicals and plant-based whole foods in reducing LDL-C and preventing cardiovascular disease. Antioxidants. 2021;10(5):1–10. https://doi.org/10.3390/antiox10050784
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Kowalska G, Pankiewicz U, Kowalski R. Assessment of pesticide content in apples and selected citrus fruits subjected to simple culinary processing. Appl Sci. 2022;12(3):1417. https://doi.org/10.3390/app12031417
Lemic D, Zorić B, Novak A, Ivić D, Galešić MA, Viric Gasparic H. The effectiveness of ozone technology application in extending the shelf life of berry fruit. Appl Fruit Sci. 2025;67(1):1–10. https://doi.org/10.1007/s10341-025-01278-x
Li X, Liu C, Liu F, Zhang X, Chen X, Peng Q, et al. Zhao, Z. Substantial removal of four pesticide residues in three fruits with ozone microbubbles. Food Chem. 22024;441:138293. https://doi.org/10.1016/j.foodchem.2023.138293
Liang Z, Xu X, Cao R, Wan Q, Xu H, Wang J, et al. Synergistic effect of ozone and chlorine on inactivating fungal spores: Influencing factors and mechanisms. J Hazard Mater. 2021;420:126–30. https://doi.org/10.1016/j.jhazmat.2021.126610
Osman KA, Mohamed HHE, Salama MS. Ozone treatment as a green technology for removing chlorpyrifos residues from vegetables and its impact on the quality of vegetables. Ozone Sci Eng. 2024;46(6):558–72. https://doi.org/10.1080/01919512.2024.2404060
Özen T, Koyuncu MA, Erbaş D. Effect of ozone treatments on the removal of pesticide residues and postharvest quality in green pepper. J Food Sci Technol. 2021;58(6):2186–96. https://doi.org/10.1007/s13197-020-04729-3
Pandiselvam R, Kaavya R, Jayanath Y, Veenuttranon K, Lueprasitsakul P, Divya V, et al. Ozone as a novel emerging technology for the dissipation of pesticide residues in foods: A review. Trends Food Sci Technol. 2020;97:38–54. https://doi.org/10.1016/j.tifs.2019.12.017
Pal P, Kioka A. Micro and nanobubbles enhanced ozonation technology: A synergistic approach for pesticides removal. Compr Rev Food Sci Food Saf. 2025;24(2):e70133. https://doi.org/10.1111/1541-4337.70133
Pandiselvam R, Kaavya R, Khanashyam AC, Divya V, Abdullah SK, Aurum FS, et al. Research trends and emerging physical processing technologies in mitigation of pesticide residues on various food products. ESPR. 2022;29(30):45131–49. https://doi.org/10.1007/s11356-022-20338-3
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Saeid A, Ahmed M. (2021). Citrus fruits: Nutritive value and value-added products. Citrus Res Dev Biotechnol. 2021;16:1–10.
Shakouri A, Yazdanpanah H, Shojaee MH. Kobarfard F. Method development for simultaneous determination of 41 pesticides in rice using LC-MS/MS technique and its application for the analysis of 60 rice samples collected from Tehran market. Iran J Pharm Res. 2014;13:27–30.
Siddique Z, Malik AU, Asi MR, Inam-ur-Raheem M, Abdullah M. Impact of sonolytic ozonation (O3/US) on degradation of pesticide residues in fresh vegetables and fruits: Case study of Faisalabad, Pakistan. Ultrason Sonochem. 2021;79:105799. https://doi.org/10.1016/j.ultsonch.2021.105799
Sun D, Zhu Y, Pang J, Zhou Z, Jiao B. (2016). Residue level, persistence and safety of spirodiclofen–pyridaben mixture in citrus fruits. Food Chem. 2016;194:805–10. https://doi.org/10.1016/j.foodchem.2015.08.044
Swami S, Kumar B, Singh SB. Effect of ozone application on the removal of pesticides from grapes and green bell peppers and changes in their nutraceutical quality. J Environ Sci Health B. 2021;56(8):722–30. https://doi.org/10.1080/03601234.2021.1940660
Syed JH, Alamdar A, Mohammad A, Ahad K, Shabir Z, Ahmed H, et al. Pesticide residues in fruits and vegetables from Pakistan: A review of the occurrence and associated human health risks. ESPR. 2014;21:13367–93. https://doi.org/10.1007/s11356-014-3117-z
USDA. Citrus: World Markets and Trade. (2022). 1–13.
Vuthijumnonk J, Shimbhanao W. Removal of cyfluthrin by fine bubble technology in oranges (Citrus reticulata Blanco). IOP Conf Ser: Earth Environ Sci. 2019;16:30–4. https://doi.org/10.1088/1755-1315/346/1/012036
Wang LK, Wang MHS. Ozone residual determination or total oxidant determination by iodometric titration-assisted spectrophotometry. Environ. Sci Technol Eng Math. 2022;56:1–56.
Wu Y, An Q, Li D, Wu J, Pan C. Comparison of different home/commercial washing strategies for ten typical pesticide residue removal effects in kumquat, spinach and cucumber. Int J Environ Res Public Health. 2019;16:1–15. https://doi.org/10.3390/ijerph16030472
Yahia EM, García-Solís P, Celis MEM. Contribution of fruits and vegetables to human nutrition and health. In: Postharvest physiology and biochemistry of fruits and vegetables. Amsterdam: Elsevier; 2019. 19–45 pp. https://doi.org/10.1016/B978-0-12-813278-4.00002-6
Zhang AA, Sutar PP, Bian Q, Fang XM, Ni JB, Xiao HW. Pesticide residue elimination for fruits and vegetables: The mechanisms, applications, and future trends of thermal and non-thermal technologies. J Future Foods. 2022;2(3):223–40. https://doi.org/10.1016/j.jfutfo.2022.06.004
Zhong G, Nicolosi E. Citrus origin, diffusion, and economic importance. Citrus Genome. 2020;5:5–21. https://doi.org/10.1007/978-3-030-15308-3_2
Albuquerque TG, Nunes MA, Bessada SM, Costa HS, Oliveira MBP. Biologically active and health promoting food components of nuts, oilseeds, fruits, vegetables, cereals, and legumes. J Food Chem. 2020;12:609–56. https://doi.org/10.1016/B978-0-12-813266-1.00014-0
Ben Hsouna A, Sadaka C, Generalic Mekinic I, Garzoli S, Svarc-Gajic J, Rodrigues F, et al. The chemical variability, nutraceutical value, and food-industry and cosmetic applications of citrus plants: A critical review. Antioxidants. 2023;12(2):481. https://doi.org/10.3390/antiox12020481
Botondi R, Barone M, Grasso C. A review into the effectiveness of ozone technology for improving the safety and preserving the quality of fresh-cut fruits and vegetables. Foods. 2021;10(4):748. https://doi.org/10.3390/foods10040748
Dhankhar J, Mehla R, Kundu P. Assessment of Pesticide Residues in Milk and Milk Products. In: The Chemistry of Milk and Milk Products. Point Pleasant, NJ, USA: Apple Academic Press; 2023. 331–59 pp. https://doi.org/10.1201/9781003340706-20
Díaz-López M, Siles JA, Ros C, Bastida F, Nicolás E. The effects of ozone treatments on the agro-physiological parameters of tomato plants and the soil microbial community. Sci Total Environ. 2022;812:151429. https://doi.org/10.1016/j.scitotenv.2021.151429
Dubey P, Singh A, Yousuf O. (2022). Ozonation: An evolving disinfectant technology for the food industry. Food Bioprocess Technol. 2022;15(9):2102–13. https://doi.org/10.1007/s11947-022-02876-3
Foong SY, Ma NL, Lam SS, Peng W, Low F, Lee BH, et al. A recent global review of hazardous chlorpyrifos pesticide in fruit and vegetables: Prevalence, remediation and actions needed. J Hazard Mater. 2020;400:1–10. https://doi.org/10.1016/j.jhazmat.2020.123006
Gonçalves-Magalhães C, D’Antonino Faroni LR, Cecon PR, de Alencar ER, Silva MVDA, Aparecida Zinato Rodrigues A. Potential of ozonated mist for microbiological disinfection and preservation of the physicochemical quality of strawberries. Ozone Sci Eng. 2025:1–15. https://doi.org/10.1080/01919512.2025.2454934
Gonzalez-Curbelo MA, Varela-Martínez DA, Riano-Herrera DA. Pesticide-residue analysis in soils by the QuEChERS method: A review. Molecules. 2022;27(13):20–30. https://doi.org/10.3390/molecules27134323
Hamid S, Sharma K, Kumar K, Thakur A. Types and Cultivation of Citrus Fruits. Citrus Fruits and Juice: Processing and Quality Profiling. Singapore: Springer; 2024. 17–43 pp. https://doi.org/10.1007/978-981-99-8699-6_2
Islam SU, Ahmed MB, Ahsan H, Lee YS. Recent molecular mechanisms and beneficial effects of phytochemicals and plant-based whole foods in reducing LDL-C and preventing cardiovascular disease. Antioxidants. 2021;10(5):1–10. https://doi.org/10.3390/antiox10050784
Jiang Y, China C. Economic perspectives of major food crops of Pakistan: An econometric analysis. JASA. 2016;11:18–23.
Kaparapu J, Pragada PM, Geddada MNR. (2020). Fruits and vegetables and its nutritional benefits. In: Egbuna C, Tupas GD, editors. Functional Foods and Nutraceuticals Bioactive Components, Formulations and Innovations. 1st ed. Switzerland: Springer; 2020. 241–60 pp. https://doi.org/10.1007/978-3-030-42319-3_14
Kaur K, Pandiselvam R, Kothakota A, Ishwarya SP, Zalpouri R, Mahanti NK. Impact of ozone treatment on food polyphenols–A comprehensive review. Food Control. 2022;142:109207. https://doi.org/10.1016/j.foodcont.2022.109207
Khalid W, Arshad MS, Ranjha MMAN, Rozanska MB, Irfan S, Shafique B, et al. Functional constituents of plant-based foods boost immunity against acute and chronic disorders. Open Life Sci. 2022;17(1):1075–93. https://doi.org/10.1515/biol-2022-0104
Kowalska G, Pankiewicz U, Kowalski R. Assessment of pesticide content in apples and selected citrus fruits subjected to simple culinary processing. Appl Sci. 2022;12(3):1417. https://doi.org/10.3390/app12031417
Lemic D, Zorić B, Novak A, Ivić D, Galešić MA, Viric Gasparic H. The effectiveness of ozone technology application in extending the shelf life of berry fruit. Appl Fruit Sci. 2025;67(1):1–10. https://doi.org/10.1007/s10341-025-01278-x
Li X, Liu C, Liu F, Zhang X, Chen X, Peng Q, et al. Zhao, Z. Substantial removal of four pesticide residues in three fruits with ozone microbubbles. Food Chem. 22024;441:138293. https://doi.org/10.1016/j.foodchem.2023.138293
Liang Z, Xu X, Cao R, Wan Q, Xu H, Wang J, et al. Synergistic effect of ozone and chlorine on inactivating fungal spores: Influencing factors and mechanisms. J Hazard Mater. 2021;420:126–30. https://doi.org/10.1016/j.jhazmat.2021.126610
Osman KA, Mohamed HHE, Salama MS. Ozone treatment as a green technology for removing chlorpyrifos residues from vegetables and its impact on the quality of vegetables. Ozone Sci Eng. 2024;46(6):558–72. https://doi.org/10.1080/01919512.2024.2404060
Özen T, Koyuncu MA, Erbaş D. Effect of ozone treatments on the removal of pesticide residues and postharvest quality in green pepper. J Food Sci Technol. 2021;58(6):2186–96. https://doi.org/10.1007/s13197-020-04729-3
Pandiselvam R, Kaavya R, Jayanath Y, Veenuttranon K, Lueprasitsakul P, Divya V, et al. Ozone as a novel emerging technology for the dissipation of pesticide residues in foods: A review. Trends Food Sci Technol. 2020;97:38–54. https://doi.org/10.1016/j.tifs.2019.12.017
Pal P, Kioka A. Micro and nanobubbles enhanced ozonation technology: A synergistic approach for pesticides removal. Compr Rev Food Sci Food Saf. 2025;24(2):e70133. https://doi.org/10.1111/1541-4337.70133
Pandiselvam R, Kaavya R, Khanashyam AC, Divya V, Abdullah SK, Aurum FS, et al. Research trends and emerging physical processing technologies in mitigation of pesticide residues on various food products. ESPR. 2022;29(30):45131–49. https://doi.org/10.1007/s11356-022-20338-3
Costat Version 2.0 (1986). Costat Statistical Package for Analysis of Variance, Version 2. Minneapolis, MN, USA: Cohort Software.
Raza SA, Ali Y, Mehboob F. Role of agriculture in economic growth of Pakistan. 2012;24:1–10.
Saeid A, Ahmed M. (2021). Citrus fruits: Nutritive value and value-added products. Citrus Res Dev Biotechnol. 2021;16:1–10.
Shakouri A, Yazdanpanah H, Shojaee MH. Kobarfard F. Method development for simultaneous determination of 41 pesticides in rice using LC-MS/MS technique and its application for the analysis of 60 rice samples collected from Tehran market. Iran J Pharm Res. 2014;13:27–30.
Siddique Z, Malik AU, Asi MR, Inam-ur-Raheem M, Abdullah M. Impact of sonolytic ozonation (O3/US) on degradation of pesticide residues in fresh vegetables and fruits: Case study of Faisalabad, Pakistan. Ultrason Sonochem. 2021;79:105799. https://doi.org/10.1016/j.ultsonch.2021.105799
Sun D, Zhu Y, Pang J, Zhou Z, Jiao B. (2016). Residue level, persistence and safety of spirodiclofen–pyridaben mixture in citrus fruits. Food Chem. 2016;194:805–10. https://doi.org/10.1016/j.foodchem.2015.08.044
Swami S, Kumar B, Singh SB. Effect of ozone application on the removal of pesticides from grapes and green bell peppers and changes in their nutraceutical quality. J Environ Sci Health B. 2021;56(8):722–30. https://doi.org/10.1080/03601234.2021.1940660
Syed JH, Alamdar A, Mohammad A, Ahad K, Shabir Z, Ahmed H, et al. Pesticide residues in fruits and vegetables from Pakistan: A review of the occurrence and associated human health risks. ESPR. 2014;21:13367–93. https://doi.org/10.1007/s11356-014-3117-z
USDA. Citrus: World Markets and Trade. (2022). 1–13.
Vuthijumnonk J, Shimbhanao W. Removal of cyfluthrin by fine bubble technology in oranges (Citrus reticulata Blanco). IOP Conf Ser: Earth Environ Sci. 2019;16:30–4. https://doi.org/10.1088/1755-1315/346/1/012036
Wang LK, Wang MHS. Ozone residual determination or total oxidant determination by iodometric titration-assisted spectrophotometry. Environ. Sci Technol Eng Math. 2022;56:1–56.
Wu Y, An Q, Li D, Wu J, Pan C. Comparison of different home/commercial washing strategies for ten typical pesticide residue removal effects in kumquat, spinach and cucumber. Int J Environ Res Public Health. 2019;16:1–15. https://doi.org/10.3390/ijerph16030472
Yahia EM, García-Solís P, Celis MEM. Contribution of fruits and vegetables to human nutrition and health. In: Postharvest physiology and biochemistry of fruits and vegetables. Amsterdam: Elsevier; 2019. 19–45 pp. https://doi.org/10.1016/B978-0-12-813278-4.00002-6
Zhang AA, Sutar PP, Bian Q, Fang XM, Ni JB, Xiao HW. Pesticide residue elimination for fruits and vegetables: The mechanisms, applications, and future trends of thermal and non-thermal technologies. J Future Foods. 2022;2(3):223–40. https://doi.org/10.1016/j.jfutfo.2022.06.004
Zhong G, Nicolosi E. Citrus origin, diffusion, and economic importance. Citrus Genome. 2020;5:5–21. https://doi.org/10.1007/978-3-030-15308-3_2
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Amjad, A. ., Saeed, . M. K., Mehboob, R., Rehman, M., Zafar, S. ., Ullah, N., Sarwar, A., Aziz, T., Al-Hoshani, N., Meslet Alsebaii, N., Alsaggaf, W. T., & Al-Joufi, F. A. (2025). Removal of chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin residues from citrus by using ozonated water. Italian Journal of Food Science, 37(3), 389-401. https://doi.org/10.15586/ijfs.v37i3.2909
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Amjad, A. ., Saeed, . M. K., Mehboob, R., Rehman, M., Zafar, S. ., Ullah, N., Sarwar, A., Aziz, T., Al-Hoshani, N., Meslet Alsebaii, N., Alsaggaf, W. T., & Al-Joufi, F. A. (2025). Removal of chlorpyrifos, carbofuran, cyhalothrin, and bifenthrin residues from citrus by using ozonated water. Italian Journal of Food Science, 37(3), 389-401. https://doi.org/10.15586/ijfs.v37i3.2909