The residues of bifenazate (sum of bifenazate and bifenazate-diazene) and etoxazole in whole citrus and pulp collected from twelve regions of China were monitored and their chronic dietary risk to consumer were also evaluated. The citrus samples were extracted by a QuEChERS (quick, easy, cheap, effective, rugged, and safe) method, and analyzed by high performance liquid chromatography-tandem mass spectrometry (HPLC–MS/MS). The average recoveries of target compounds were ranged from 83 to 100% with relative standard deviations (RSDs) of 0.59–11.8%. The limits of quantification (LOQs) for three analytes were 0.01 mg/kg. At the interval to harvest of 20 and 30 days, the residues of total bifenazate and etoxazole were from below 0.02 to 0.26 mg/kg and from below 0.01 to 0.30 mg/kg in citrus samples. The chronic risk quotients (RQs) were below 100%, indicating no unacceptable risk to consumers.
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Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. J AOAC Int 86(2):412–431. https://doi.org/10.1093/jaoac/86.2.412
Chen H, Li W, Guo L, Weng H, Wei Y, Guo Q (2019) Residue, dissipation, and safety evaluation of etoxazole and pyridaben in Goji berry under open-field conditions in the China’s Qinghai-Tibet Plateau. Environ Monit Assess 191(8):517. https://doi.org/10.1007/s10661-019-7671-1
CNS (2012) The chinese dietary guidelines. People’s Publishing House, Beijing
Dekeyser MA (2005) Acaricide mode of action. Pest Manag Sci 61(2):103–110. https://doi.org/10.1002/ps.994
European Food Safety, Authority (2012) Reasoned opinion on the review of the existing maximum residue levels (MRLs) for etoxazole according to Article 12 of Regulation (EC) No 396/2005. EFSA J. https://doi.org/10.2903/j.efsa.2012.2931
European Food Safety Authority, Anastassiadou M, Brancato A, Carrasco Cabrera L, Ferreira L, Greco L, Jarrah S, Kazocina A, Leuschner R, Magrans JO, Miron I, Nave S, Pedersen R, Reich H, Rojas A, Sacchi A, Santos M, Stanek A, Theobald A, Vagenende B, Verani A (2019) Modification of the existing maximum residue level for bifenazate in elderberries. EFSA J 17(11):e05878. https://doi.org/10.2903/j.efsa.2019.5878
European Food Safety Authority, Brancato A, Brocca D, De Lentdecker C, Erdos Z, Ferreira L, Greco L, Janossy J, Jarrah S, Kardassi D, Leuschner R, Lythgo C, Medina P, Miron I, Molnar T, Nougadere A, Pedersen R, Reich H, Sacchi A, Santos M, Stanek A, Sturma J, Tarazona J, Theobald A, Vagenende B, Verani A, Villamar-Bouza L (2017) Modification of the existing maximum residue level for bifenazate in soya bean. EFSA J 15(9):e04983. https://doi.org/10.2903/j.efsa.2017.4983
FAO. (2006a) Pesticide residues in food 2006. http://www.fao.org/fileadmin/templates/agphome/documents/Pests_Pesticides/JMPR/JMPRrepor2006.pdf. Accessed 12 October 2006
FAO. (2006b) Updating the principles and methods of risk assessment: MRLs for pesticides and veterinary drugs (Rome). http://www.fao.org/3/al932e/al932e.pdf. Accessed 23 January 2006
FAO. (2010a) BIFENAZATE (219). http://www.fao.org/fileadmin/templates/agphome/documents/Pests_Pesticides/JMPR/Report10/bifenazate.pdf. Accessed 09 July 2010
FAO. (2010b) ETOXAZOLE (241). http://www.fao.org/fileadmin/templates/agphome/documents/Pests_Pesticides/JMPR/Report10/bifenazate.pdf. Accessed 09 July 2010
Gómez-Almenar MC, García-Mesa JA (2015) Determination of pesticide residues in olives by liquid extraction surface analysis followed by liquid chromatography/tandem mass spectrometry. Grasas Aceites. https://doi.org/10.3989/gya.0828142
Ham J, You S, Lim W, Song G (2020) Etoxazole induces testicular malfunction in mice by dysregulating mitochondrial function and calcium homeostasis. Environ Pollut 263(Pt A):114573. https://doi.org/10.1016/j.envpol.2020.114573
Hayward DG, Wong JW, Park HY (2015) Determinations for pesticides on black, green, oolong, and white teas by gas chromatography triple-quadrupole mass spectrometry. J Agric Food Chem 63(37):8116–8124. https://doi.org/10.1021/acs.jafc.5b02860
Hiragaki S, Kobayashi T, Ochiai N, Toshima K, Dekeyser MA, Matsuda K, Takeda M (2012) A novel action of highly specific acaricide; bifenazate as a synergist for a GABA-gated chloride channel of Tetranychus urticae [Acari: Tetranychidae]. Neurotoxicology 33(3):307–313. https://doi.org/10.1016/j.neuro.2012.01.016
IUPAC. (2021) Pesticides properties database. https://sitem.herts.ac.uk/aeru/ppdb/en/Reports/76.htm. Accessed 28 April 2021
Lin H, Liu L, Zhang Y, Shao H, Li H, Li N, Zou P, Lu N, Guo Y (2020) Residue behavior and dietary risk assessment of spinetoram (XDE-175-J/L) and its two metabolites in cauliflower using QuEChERS method coupled with UPLC-MS/MS. Ecotoxicol Environ Saf 202:110942. https://doi.org/10.1016/j.ecoenv.2020.110942
Liu S, Kou H, Mu B, Wang J, Zhang Z (2019) Dietary risk evaluation of tetraconazole and bifenazate residues in fresh strawberry from protected field in North China. Regul Toxicol Pharmacol 106:1–6. https://doi.org/10.1016/j.yrtph.2019.04.008
Ma J, Huang Y, Peng Y, Xu Z, Wang Z, Chen X, Xie S, Jiang P, Zhong K, Lu H (2021) Bifenazate exposure induces cardiotoxicity in zebrafish embryos. Environ Pollut 274:116539. https://doi.org/10.1016/j.envpol.2021.116539
Malhat F, Hassan A (2011) Level and fate of etoxazole in green bean (Phaseolus vulgaris). Bull Environ Contam Toxicol 87(2):190–193. https://doi.org/10.1007/s00128-011-0336-6
Ochiai N, Mizuno M, Mimori N, Miyake T, Dekeyser M, Canlas LJ, Takeda M (2007) Toxicity of bifenazate and its principal active metabolite, diazene, to Tetranychus urticae and Panonychus citri and their relative toxicity to the predaceous mites, Phytoseiulus persimilis and Neoseiulus californicus. Exp Appl Acarol 43(3):181–197. https://doi.org/10.1007/s10493-007-9115-9
Park W, Lim W, Park S, Whang KY, Song G (2020) Exposure to etoxazole induces mitochondria-mediated apoptosis in porcine trophectoderm and uterine luminal epithelial cells. Environ Pollut 257:113480. https://doi.org/10.1016/j.envpol.2019.113480
Peng Y, Li M, Huang Y, Cheng B, Cao Z, Liao X, Xiong G, Liu F, Hu C, Lu H (2021) Bifenazate induces developmental and immunotoxicity in zebrafish. Chemosphere 271:129457. https://doi.org/10.1016/j.chemosphere.2020.129457
Perestrelo R, Silva P, Porto-Figueira P, Pereira JAM, Silva C, Medina S, Camara JS (2019) QuEChERS—fundamentals, relevant improvements, applications and future trends. Anal Chim Acta 1070:1–28. https://doi.org/10.1016/j.aca.2019.02.036
Rejczak T, Tuzimski T (2017) QuEChERS-based extraction with dispersive solid phase extraction clean-up using PSA and ZrO2-based sorbents for determination of pesticides in bovine milk samples by HPLC-DAD. Food Chem 217:225–233. https://doi.org/10.1016/j.foodchem.2016.08.095
Rencuzogullari E, Ila HB, Kayraldiz A, Arslan M, Diler SB, Topaktas M (2004) The genotoxic effect of the new acaricide etoxazole. Russ J Genet 40(11):1300–1304. https://doi.org/10.1023/B:RUGE.0000048674.00728.2f
Saber AN, Malhat F, Anagnostopoulos C, Kasiotis KM (2020) Evaluation of dissipation, unit–unit-variability and terminal residue of etoxazole residues in strawberries from two different parts in Egypt. Journal of Consumer Protection and Food Safety 15(3):229–236. https://doi.org/10.1007/s00003-019-01266-w
SANTE/11945/2015. (2015) Analytical quality control and method validation procedures for pesticide residues and analysis in food and feed. https://www.eurl-pesticides.eu/library/docs/allcrl/AqcGuidance_SANTE_2015_11945.pdf. Accessed 1 January 2016
Satheshkumar A, Senthurpandian VK, Shanmugaselvan VA (2014) Dissipation kinetics of bifenazate in tea under tropical conditions. Food Chem 145:1092–1096. https://doi.org/10.1016/j.foodchem.2013.09.042
Sharma KK, Tripathy V, Mohapatra S, Matadha NY, Pathan ARK, Sharma BN, Dubey JK, Katna S, George T, Tayade A, Sharma K, Gupta R, Walia S (2021) Dissipation kinetics and consumer risk assessment of novaluron + lambda-cyhalothrin co-formulation in cabbage. Ecotoxicol Environ Saf 208:111494. https://doi.org/10.1016/j.ecoenv.2020.111494
Sun D, Pang J, Fang Q, Zhou Z, Jiao B (2016) Stereoselective toxicity of etoxazole to MCF-7 cells and its dissipation behavior in citrus and soil. Environ Sci Pollut Res Int 23(24):24731–24738. https://doi.org/10.1007/s11356-016-7393-7
Thekkumpurath AS, Girame R, Hingmire S, Jadhav M, Jain P (2020) Residue dissipation, evaluation of processing factor and safety assessment of hexythiazox and bifenazate residues during drying of grape to raisin. Environ Sci Pollut Res Int 27(33):41816–41823. https://doi.org/10.1007/s11356-020-10169-5
Uner N, Oruc E, Sevgiler Y (2005) Oxidative stress-related and ATPase effects of etoxazole in different tissues of Oreochromisniloticus. Environ Toxicol Pharmacol 20(1):99–106. https://doi.org/10.1016/j.etap.2004.11.006
Wang Z, Pang J, Liao C, Zhang Q, Sun D (2020) Determination of etoxazole in different parts of citrus fruit and its potential dietary exposure risk assessment. Chemosphere. https://doi.org/10.1016/j.chemosphere.2020.128832
Yao Z, Li Z, Zhuang S, Li X, Xu M, Lin M, Wang Q, Zhang H (2015) Enantioselective determination of acaricide etoxazole in orange pulp, peel, and whole orange by chiral liquid chromatography with tandem mass spectrometry. J Sep Sci 38(4):599–604. https://doi.org/10.1002/jssc.201401065
Zheng X, Liu C, Hu J (2020) Residues and dietary risk assessments of 2,4-D Isooctyl ester, metribuzin, acetochlor, and 2-Ethyl-6-methylaniline in corn or soybean fields. J Agric Food Chem 68(15):4315–4324. https://doi.org/10.1021/acs.jafc.0c00193
This work was supported by financial support from National Natural Science Foundation of China (Project No. 21677009).
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Hou, H., Yu, X., Dong, B. et al. Residues and Safety Evaluation of Etoxazole, Bifenazate and Its Metabolite Bifenazate-diazene in Citrus Under Open-Field Conditions. Bull Environ Contam Toxicol 107, 281–288 (2021). https://doi.org/10.1007/s00128-021-03319-z
- Pesticide residue
- Risk assessment