Residue distribution, safety evaluation, processing factor and dissipation kinetics of bifenthrin and ethion in date fruits

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O.I. Abdallah
S.S. Alamer
A.M. Alrasheed
A.A. Almundarij


risk assessment, method validation, QuEChERS, date fruits, ethion, bifenthrin


Gas chromatography with ion trap mass spectrometry was used to simultaneously analyses bifenthrin and ethion residues in date fruits after acetonitrile extraction and dispersive solid phase extraction for clean-up. The method was validated in line with the SANTE/11813/2017 guideline with performance criteria including the linearity range, repeatability, intermediate reproducibility, matrix effect, recovery, and limit of quantitation. Attractive advances results include: (1) lower quantitation limit of 6.9 and 5.8 ?g/kg; (2) the recoveries were between 91.61 and 98.84%, and the corresponding relative standard deviations (RSDs) were lower than 11.7%; (3) excellent repeatability RSDr of lower than 10.3 ?g/kg, and intermediate reproducibility RSDR of lower than 15.6 ?g/kg, Furthermore, the method is fast and simple. After validation, the developed method was successfully applied for the determination of the dissipation kinetics of the bifenthrin and ethion in date fruits over 45 days under field conditions of Saudi Arabia. The results showed that the dissipation kinetics of bifenthrin and ethion can be described by a first-order kinetics model with a half-life (t0.5) of 1.92 and 2.43 days for bifenthrin and 2.2 and 2.59 days for ethion, at the low and high recommended application rates, respectively. For safe consumption of dates, waiting periods of 12 and 28 days for bifenthrin and 18 and 38 days for ethion are suggested. A total of 600 date samples were collected from the largest market in the world in Qassim Province, Buraydah City, in 2017-2018. A risk assessment of the residues was performed by calculating the risk quotients for children and adults in Saudi Arabia. The high consumption of dates by children may have hazards. The processing factors for washing with tap water, and washing plus boiling (date syrup production) showed that washing had little effect on residue reduction compared with washing plus boiling.

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Abdallah, O.I., Alamer, S.S. and Alrasheed, A.M., 2018. Monitoring pesticide residues in dates marketed in Al-Qassim, Saudi Arabia using a QuEChERS methodology and liquid chromatography-tandem mass spectrometry. Biomedical Chromatography 32(6): e4199.
Abdallah, O.I., Hanafi, A., Abdel Ghani, S.B., Ghisoni, S. and Lucini, L., 2017. Pesticides contamination in Egyptian honey samples. Journal of Consumer Protection and Food Safety 12: 317-327.
Abdel-Gawad, H., Mahdy, F., Hashad, A. and Elgemeie, G.H., 2014. Fate of 14C-ethion insecticide in the presence of deltamethrin and dimilin pesticides in cotton seeds and oils, removal of ethion residues in oils, and bioavailability of its bound residues to experimental animals. Journal of Agricultural and Food Chemistry 62: 12287-12293.
Al-Farsi, M., Alasalvar, C., Morris, A., Baron, M. and Shahidi, F., 2005. Comparison of antioxidant activity, anthocyanins, carotenoids, and phenolics of three native fresh and sun-dried date (Phoenix dactylifera L.) varieties grown in Oman. Journal of Agricultural and Food Chemistry 53: 7592-7599.
Al-Taher, F., Chen, Y., Wylie, P. and Cappozzo, J., 2013. Reduction of pesticide residues in tomatoes and other produce. Journal of Food Protection 76: 510.
Ashraf, Z. and Hamidi-Esfahani, Z., 2011. Date and date processing: a review. Food Reviews International 27: 101-133.
Baloch, M.K., Saleem, S.A., Baloch, A.K. and Baloch, W.A., 2006. Impact of controlled atmosphere on the stability of Dhakki dates. LWT – Food Science and Technology 39: 671-676.
Claeys, W.L., De Voghel, S., Schmit, J.-F., Vromman, V. and Pussemier, L., 2008. Exposure assessment of the Belgian population to pesticide residues through fruit and vegetable consumption. Food Additives and Contaminants 25: 851-863.
Clementi, M., Tiboni, G.M., Causin, R., La Rocca, C., Maranghi, F., Raffagnato, F. and Tenconi, R., 2008. Pesticides and fertility: an epidemiological study in Northeast Italy and review of the literature. Reproductive Toxicology 26: 13-18.
Damalas, C.A. and Eleftherohorinos, I.G., 2011. Pesticide exposure, safety issues, and risk assessment indicators. International Journal of Environmental Research and Public Health 8: 1402-1419.
El-Sharnouby, G.A., Aleid, S.M. and Al-Otaibi, M.M., 2014. Liquid sugar extraction from date palm (Phoenix dactylifera L.) fruits. Journal of Food Processing and Technology 5: 402.
EU Reference Laboratories for Residues of Pesticides, 2017. SANTE/11813/2017. Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed. Available at:
European Commission (EC), 2002. Commission Directive 2002/63/EC of 11 July 2002 establishing community methods of sampling for the official control of pesticide residues in and on products of plant and animal origin and repealing Directive 79/700/EEC. Official Journal of the European Communities L 187: 30-43.
European Commission (EC), 2005. Regulation (EC) No 396/2005. Available at:
European Food Safety Authority (EFSA), 2011. Conclusion on the peer review of the pesticide risk assessment of the active substance bifenthrin. EFSA Journal 9: 2159.
Fenoll, J., Ruiz, E., Hellín, P., Lacasa, A. and Flores, P., 2009. Dissipation rates of insecticides and fungicides in peppers grown in greenhouse and under cold storage conditions. Food Chemistry 113: 727-732.
Ferrer, C., Lozano, A., Agüera, A., Girón, A.J. and Fernández-Alba, A., 2011. Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables. Journal of Chromatography A 1218: 7634-7639.
Food and Agriculture Organisation / World Health Organisation (FAO/WHO), 2008. Pesticide residues in food – 2006 evaluations. Part II – Toxicological. FAO/WHO, Rome, Italy.
Gale, F. and Buzby, J.C., 2009. Imports from China and food safety issues. Diane Publishing, Collingdale, PA, USA.
Ganbi, H., 2012. Production of nutritious high quality date (Phoenix dactylifera) fruits syrup (Dibs) by using some novel technological approaches. Journal of Applied Sciences Research 8(3): 1524-1538.
Ghani, S.B.A. and Abdallah, O.I., 2016. Method validation and dissipation dynamics of chlorfenapyr in squash and okra. Food Chemistry 194: 516-521.
Ghani, S.B.A., Alhewairini, S.S. and Hrouzková, S., 2018. A fast and easy QuEChERS-DLLME method combined with GC-MS for ethion and bifenthrin residues determination and study of their dissipation dynamics in palm dates. Food Analytical Methods 11(12): 3542-3550.
Gohari-Ardebili, A., 2004. Survey on effects of replacement of sugar with date syrup on Physico-chemical ccharacteristics of soft ice cream. MSc-thesis, Ferdowsi University, Mashhad, Iran.
Gupta, S., Sharma, R., Gupta, R., Sinha, S., Singh, R. and Gajbhiye, V., 2009. Persistence of new insecticides and their efficacy against insect pests of okra. Bulletin of Environmental Contamination and Toxicology 82: 243-247.
Kumari, S., Chauhan, R. and Kumari, B., 2013. Persistence and decontamination of bifenthrin residues in okra fruits. African Journal of Agricultural Research 8: 4833-4838.
Liang, H., Li, L., Li, W., Wu, Y., Zhou, Z. and Liu, F., 2011. Dissipation and residue of dimethomorph in pepper and soil under field conditions. Ecotoxicology and Environmental Safety 74: 1331-1335.
Lucini, L. and Molinari, G.P., 2011. Performance and matrix effect observed in QuEChERS extraction and tandem mass spectrometry analyses of pesticide residues in different target crops. Journal of Chromatographic Science 49: 709-714.
MacNeil, J.D. and Hikichi, M., 1976. Degradation of endosulfan and ethion on pears and pear and grape foliage. Journal of Agricultural and Food Chemistry 24: 608-611.
Mnif, W., Hassine, A.I.H., Bouaziz, A., Bartegi, A., Thomas, O. and Roig, B., 2011. Effect of endocrine disruptor pesticides: a review. International Journal of Environmental Research and Public Health 8: 2265-2303.
Parmar, K., Korat, D., Shah, P. and Singh, S., 2012. Dissipation and decontamination of some pesticides in/on okra. Pesticide Research Journal 24: 42-46.
Patyal, S., Dubey, J., Sharma, I. and Divender, G., 2010. Persistence of bifenthrin residues on apple (Malus domestica) fruit and soil. Pesticide Research Journal 22: 116-119.
Priyadarshini G, V.S., Reddy, C.N. and Swarupa, S., 2017. Dissipation pattern of ethion and profenophos in curry leaf. Journal of Global Bioscience 1: 4661-4665.
Ramarao, G. and Goud, R.C., 2016. Dissipation pattern and accumulation of bifenthrin in tomato. Journal of Entomological Research 40: 275-277.
Reddy, D.J. and Rao, B.N., 2002. Efficacy of selected insecticides against pests of grapevine. Pesticide Research Journal 14: 92-99.
Reddy, S.S., Reddy, C.N., Srinivas, C., Rao, A.M. and Reddy, S.N., 2017. Dissipation pattern of bifenthrin on dolichos bean. International Journal of Current Microbiology and Applied Sciences 6: 675-680.
Seenivasan, S. and Muraleedharan, N., 2015. Persistence of bifenthrin in tea and its transfer from black tea to tea brew. Journal of Tea Science Research 5: 1-7.
Sharma, B. and Parihar, N., 2013. Dissipation and persistence of dimethoate and ethion residues in/on chilli, Capsicum annuum(L.). Pesticide Research Journal 25: 80-82.
Sidhu, J.S., Al-Saqer, J.M., Al-Hooti, S.N. and Al-Othman, A., 2003. Quality of pan bread made by replacing sucrose with date syrup produced by using pectinase/cellulase enzymes. Plant Foods for Human Nutrition 58: 1-8.
Son, H.-K., Kim, S.-A., Kang, J.-H., Chang, Y.-S., Park, S.-K., Lee, S.-K., Jacobs Jr., D. and Lee, D.-H., 2010. Strong associations between low-dose organochlorine pesticides and type 2 diabetes in Korea. Environment International 36: 410-414.
Tewary, D.K., Kumar, V., Ravindranath, S. and Shanker, A., 2005. Dissipation behavior of bifenthrin residues in tea and its brew. Food Control 16: 231-237.
Tomlin, C.D.S., 2009. The pesticide manual: a world compendium. British Crop Production Council, Alton, UK, 1457 pp.
Varghese, T.S., Mathew, T.B., George, T., Beevi, S.N. and Xavier, G., 2011. Dissipation study of dimethoate, ethion and oxydemeton methyl in chilli. Pesticide Research Journal 23: 68-73.
World Health Organisation (WHO), 1995. GEMS/Food-EURO second workshop on reliable evaluation of low-level contamination of food. Report of a workshop in the frame of GEMS. May 26-27, 1995. Kulmbach, Germany.
World Health Organisation (WHO), 2003. Global environment monitoring system/food contamination monitoring and assessment program regional per capita consumption of raw and semi processed agricultural commodities. WHO, Geneva, Switzerland. Available at:
Yang, A., Park, J.-H., El-Aty, A.A., Choi, J.-H., Oh, J.-H., Do, J.-A., Kwon, K., Shim, K.-H., Choi, O.-J. and Shim, J.-H., 2012. Synergistic effect of washing and cooking on the removal of multi-classes of pesticides from various food samples. Food Control 28: 99-105.
You, X., Jiang, N., Liu, F., Liu, C. and Wang, S., 2013. Dissipation and residue of bifenthrin in wheat under field conditions. Bulletin of Environmental Contamination and Toxicology 90: 238-241.
Zhao, B., Shen, H., Liu, F., Liu, S., Niu, J., Guo, F. and Sun, X., 2012. Exposure to organochlorine pesticides is an independent risk factor of hepatocellular carcinoma: a case-control study. Journal of Exposure Science and Environmental Epidemiology 22: 541.