Environmental Science and Pollution Research

, Volume 26, Issue 4, pp 3465–3472 | Cite as

Residue behavior and risk assessment of cymoxanil in grape under field conditions and survey of market samples in Guangzhou

  • Jianxiang Huang
  • Qian Ye
  • Kai Wan
  • Fuhua WangEmail author
Research Article


A simple and fast method based on liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for cymoxanil residue analysis in grape. Sample preparation based on solid-liquid extraction was optimized without using adsorbent for purification. Recoveries were 79.8–109.5% with relative standard deviations (RSDs) of 2.5–9.4% at fortified levels from 0.001 to 0.50 mg/kg. The limit of detection (LOD) was 0.3 μg/kg. Field trials were conducted to explore the dissipation and terminal residue behavior of cymoxanil in grape. Results showed that the half-lives of cymoxanil were from 0.5 to 0.7 days. Terminal residues were from below the limit of quantification (LOQ) to 0.363 mg/kg. Dietary exposure risk assessment revealed that the risk quotients (RQs) were much less than 1. It was concluded that cymoxanil in grape raised negligible concerns to human health under field conditions. Sixty grape samples from Guangzhou market were found to be free of cymoxanil. The proposed study would provide reference for appropriate use of cymoxanil in grape planting in China.


Cymoxanil Grape Residue Risk assessment Survey Guangzhou 



This research was financially supported by the National Natural Science Foundation of China (no. 21305019) and National Program for Quality and Safety Risk Assessment of Agricultural Products of China (nos. GJFP2014001, GJFP2015001, and GJFP2016002).

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

11356_2018_3890_MOESM1_ESM.docx (16 kb)
ESM 1 (DOCX 15 kb)


  1. Ahammed Shabeer TP, Banerjee K, Jadhav M, Girame R, Utture S, Hingmire S, Oulkar D (2015) Residue dissipation and processing factor for dimethomorph, famoxadone and cymoxanil during raisin preparation. Food Chem 170:180–185CrossRefGoogle Scholar
  2. Arias LA, Bojacá CR, Ahumada DA, Schrevens E (2014) Monitoring of pesticide residues in tomato marketed in Bogota. Colombia Food Control 35:213–217CrossRefGoogle Scholar
  3. Arias-Estévez M, López-Periago E, Martínez-Carballo E, Simal-Gándara J, Mejuto JC, García-Río L (2008) The mobility and degradation of pesticides in soils and the pollution of groundwater resources. Agric Ecosyst Environ 123:247–260CrossRefGoogle Scholar
  4. Bavol D, Zima J, Barek J, Dejmkova H (2016) Voltammetric determination of cymoxanil and famoxadone at different types of carbon electrodes. Electroanalysis 28:1029–1034CrossRefGoogle Scholar
  5. Castro G, Pérez-Mayán L, Rodríguez-Cabo T, Rodríguez I, Ramil M, Cela R (2018) Multianalyte, high-throughput liquid chromatography tandem mass spectrometry method for the sensitive determination of fungicides and insecticides in wine. Anal Bioanal Chem 410:1139–1150CrossRefGoogle Scholar
  6. Chinese Nutrition Society (2016) Dietary guidelines for Chinese population (2016). People’s Medical Publishing House Co., Ltd, Beijing, p 56 (in Chinese)Google Scholar
  7. Esturk O, Yakar Y, Ayhan Z (2014) Pesticide residue analysis in parsley, lettuce and spinach by LC-MS/MS. J Food Sci Technol 51:458–466CrossRefGoogle Scholar
  8. European Commission Directorate-General for Health and Food Safety (2015) Document SANTE/11945/2015: guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed. Accessed 30 Sep 2018
  9. European Commission. Commission Regulation (EU) 2016/1785. (2016) Accessed 30 Sep 2018
  10. Fayette J, Roberts PD, Pernezny KL, Jones JB (2012) The role of cymoxanil and famoxadone in the management of bacterial spot on tomato and pepper and bacterial leaf spot on lettuce. Crop Prot 31:107–112CrossRefGoogle Scholar
  11. GB 2763-2014 (2014) National Standard of the People’s Republic of China: National Food Safety Standard-maximum residue limits for pesticides in food. Stands Press of China, Beijing (in Chinese)Google Scholar
  12. González Álvarez M, Noguerol-Pato R, González-Barreiro C, Cancho-Grande B, Simal-Gándara J (2012) Changes of the sensorial attributes of white wines with the application of new anti-mildew fungicides under critical agricultural practices. Food Chem 130:139–146CrossRefGoogle Scholar
  13. González-Rodríguez RM, Cancho-Grande B, Simal-Gándara J (2011) Decay of fungicide residues during vinification of white grapes harvested after the application of some new active substances against downy mildew. Food Chem 125:549–560CrossRefGoogle Scholar
  14. He LL, Xu YM, Sun YG, Huang YC, Pei RR, Zheng SY (2007) Residue dynamics of cymoxanil in mixed formulation in potatoes and soil. Journal of Agro-Environment. Science 26:322–325Google Scholar
  15. Hollosi L, Mittendorf K, Senyuva HZ (2012) Coupled turbulent flow chromatography: LC-MS/MS method for the analysis of pesticide residues in grapes, baby food and wheat flour matrices. Chromatographia 75:1377–1393CrossRefGoogle Scholar
  16. Hong SH, She YX, Zhang C, Cao XL, Zheng LF, Wang SS, Jin MJ, Shao H, Jin F, Lao SB, Yan FY, Wang J (2018) Simultaneous detection and degradation of pyraclostrobin and cymoxanil in cucumber and soil. Food Sci 39:262–266 (in Chinese)Google Scholar
  17. Huang JX, Liu CY, Lu DH, Chen JJ, Deng YC, Wang FH (2015) Residue behavior and risk assessment of mixed formulation of imidacloprid and chlorfenapyr in chieh-qua under field conditions. Environ Monit Assess 187:650. CrossRefGoogle Scholar
  18. Japanese Positive List System for Agricultural Chemical Residues in Foods (2016) Maximum residue limits (MRLs) of agricultural chemicals in foods. Accessed 30 Sep 2018
  19. Kemmerich M, Bernardi G, Prestes OD, Adaime MB, Zanella R (2018) Comprehensive method validation for the determination of 170 pesticide residues in pear employing modified QuEChERS without clean-up and ultra-high performance liquid chromatography coupled to tandem mass spectrometry. Food Anal Methods 11:556–577CrossRefGoogle Scholar
  20. Liu MY (2009) Study on the residue behavior and effect of cymoxanil and its mixture in grapery. Master Thesis, Hunan Agricultural University. Changsha, China, pp 21–26 (in Chinese)Google Scholar
  21. Liu XY, Yang Y, Cui Y, Zhu HJ, Li X, Li ZN, Zhang KK, Hu DY (2014) Dissipation and residue of metalaxyl and cymoxanil in pepper and soil. Environ Monit Assess 186:5307–5313CrossRefGoogle Scholar
  22. Liu J, Rashid M, Qi JW, Hu MY, Zhong GH (2016) Dissipation and metabolism of tebufenozide in cabbage and soil under open field conditions in South China. Ecotoxicol Environ Saf 134:204–212CrossRefGoogle Scholar
  23. López DR, Ahumada DA, Díaz AC, Guerrero JA (2014) Evaluation of pesticide residues in honey from different geographic regions of Colombia. Food Control 37:33–40CrossRefGoogle Scholar
  24. Luo YT, Meng YJ, Zhao JJ, Han XY, Ma ZQ, Wang WQ, Zhang XF (2016) Sensitivity to fungicides of Phytophthora infestans and controlling efficacy of corresponding fungicides against potato late blight. Agrochemicals 55:134–137 (in Chinese)Google Scholar
  25. MOA (Ministry of Agriculture of the People’s Republic of China) (2017) China agriculture yearbook of 2016. China Agriculture Press, Beijing, pp 222–225 (in Chinese)Google Scholar
  26. Mol HGJ, Rooseboom A, Dam RV, Roding M, Arondeus K, Sunarto S (2007) Modification and re-validation of the ethyl acetate-based multi-residue method for pesticides in produce. Anal Bioanal Chem 389:1715–1754CrossRefGoogle Scholar
  27. Moreno-González D, Huertas-Pérez JF, Gámiz-Gracia L, García-Campaña AM (2015) High-throughput methodology for the determination of 33 carbamates in herbal products by UHPLC-MS/MS. Food Anal Methods 8:2059–2068CrossRefGoogle Scholar
  28. Muñoz NC, Floriano L, Souza MPD, Bandeira NMG, Prestes OD, Zanella R (2017) Determination of pesticide residues in golden berry (Physalis peruviana L.) by modified QuEChERS method and ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry. Food Anal Methods 10:320–329CrossRefGoogle Scholar
  29. Nantia EA, Moreno-González D, García-Campaña AM, Gámiz-Gracia L (2017) High-throughput methodology for the determination of carbamates in food supplements by UHPLC-MS/MS. Chromatographia 80:63–70CrossRefGoogle Scholar
  30. NHFPC (National Health and Family Planning Commission of the People’s Republic of China) (2015) Report of nutrition and chronic disease status of the Chinese people. People’s Medical Publishing House Co., Ltd, Beijing, Beijing, p 13 (in Chinese)Google Scholar
  31. NY/T 788-2004 (2004) Agricultural Standard of the People’s Republic of China: guideline for pesticide residue testing. Agriculture Press of China, Beijing (in Chinese)Google Scholar
  32. Rodrigues AM, Ferreira V, Cardoso VV, Ferreira E, Benoliel MJ (2007) Determination of several pesticides in water by solid-phase extraction, liquid chromatography and electrospray tandem mass spectrometry. J Chromatogr A 1150:267–278CrossRefGoogle Scholar
  33. Sabando OLD, Balugera ZGD, Goicolea MA, Rodríguez E, Sampedro MC, Barrio RJ (2002) Determination of simazine and cymoxanil in soils by microwave-assisted solvent extraction and HPLC with reductive amperometrical detection. Chromatographia 55:667–671CrossRefGoogle Scholar
  34. Sun DL, Zhu YM, Pang JX, Zhou ZQ, Jiao BN (2016) Residue level, persistence and safety of spirodiclofen-pyridaben mixture in citrus fruits. Food Chem 194:805–810CrossRefGoogle Scholar
  35. Wang YH, Hou ZG, Mi DL, Zhao XF, Wang XH, Lu ZB (2014) Simultaneous determination of cymoxanil and azoxystrobin in potato and soil by high performance liquid chromatography. Agrochemicals 53:815–817 (in Chinese)Google Scholar
  36. Yan JQ, Wang R, Xu YC, Sun GG, Lu BH, Wang Y, Gao J (2016) The residual dynamics and final residue of cymoxanil in ginseng with the application of cymoxanil·mancozeb 72% WP. Agrochemicals 55:275–277 (in Chinese)Google Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Jianxiang Huang
    • 1
    • 2
    • 3
  • Qian Ye
    • 1
    • 2
    • 3
  • Kai Wan
    • 1
    • 2
    • 3
  • Fuhua Wang
    • 1
    • 2
    • 3
    Email author
  1. 1.Public Monitoring Center for Agro-productGuangdong Academy of Agricultural SciencesGuangzhouChina
  2. 2.Key Laboratory of Testing and Evaluation for Agro-product Quality and SafetyMinistry of Agriculture and Rural Affairs, People’s Republic of ChinaGuangzhouChina
  3. 3.Laboratory of Quality and Safety Risk Assessment for Agro-product (Guangzhou)Ministry of Agriculture and Rural Affairs, People’s Republic of ChinaGuangzhouChina

Personalised recommendations