LC–MS/MS Analysis of Five Neonicotinoid Pesticides in Sheep and Cow Milk Samples Collected in Jordan Valley

  • Giorgio Fedrizzi
  • Alberto Altafini
  • Sara Armorini
  • Khaled Mefleh Al-Qudah
  • Paola RoncadaEmail author


The purpose of the present study was to evaluate the presence of five neonicotinoid pesticides, acetamiprid, imidacloprid, clothianidin, thiacloprid, and thiamethoxam, in sheep and cow milk samples collected from animals bred in the Jordan Valley. In this area, numerous citrus plantations are present, and these insecticides are commonly used to protect plants from pests and diseases. Thirty-seven sheep milk samples and 31 cow milk samples were analysed. The analytical method, based on a single cleanup extraction step with SPE cartridges packed with diatomaceous earth material, together with analysis by LC–MS/MS, has guaranteed average recoveries between 75.1% and 88.3%, limits of detection (LOD) and quantification (LOQ) of 0.5 and 1 µg/kg, respectively, for all the five neonicotinoids. LOQ was much lower than the codex maximum residues limits for these pesticides in milks. No residues of the five neonicotinoids were found in any sample at a concentration level above LOD.


Neonicotinoids Milk Jordan Valley Pesticide residues Environment LC–MS/MS 


Compliance with Ethical Standards

Conflict of interest

The authors declare that they have no conflict of interest.


  1. Ahmad R, Nida M, Salem NM, Estaitieh H (2010) Occurrence of organochlorine pesticide residues in eggs, chicken and meat in Jordan. Chemosphere 78:667–671CrossRefGoogle Scholar
  2. Al Antary TM, Alawi MA, Estityah H, Haddad N, Al-Antary ET (2015) Chlorinated pesticide residues in human breast milk collected from southern Jordan in 2012/2013. Toxin Rev 34(4):190–194CrossRefGoogle Scholar
  3. Alawi M, Al-Antary T, Hussein E, Al-Oqlah K (2012) Comparison study of pesticides residues in agricultural crops in Jordan for seven studies between 1993 and 2008. Fresen Environ Bull 21(4A):927–934Google Scholar
  4. Alawi MA, Al Antary TM, Estityah H, Haddad N (2016) Evaluation of chlorinated pesticides residues in foodstuff of animal origin from middle districts of Jordan in 2013–2014. Toxin Rev 36(2):94–100CrossRefGoogle Scholar
  5. Antary T, Alawi M, Hussein H, Al-Oqlah K (2012) Comparison study of chlorinated pesticides in animal products within fourteen years in Jordan. Fresenius Environ Bull 21(1):117–122Google Scholar
  6. Batarseh M, Tarawneh R (2013) Multiresidue analysis of pesticides in agriculture soil from Jordan valley. JJC 8(3):152–168CrossRefGoogle Scholar
  7. Bonmatin JM, Giorio C, Girolami V, Goulson D, Kreutzweiser DP et al (2015) Environmental fate and exposure; neonicotinoids and fipronil. Environ Sci Pollut Res 22:35–67CrossRefGoogle Scholar
  8. Codex Alimentarius (2018) Accessed 5 July 2018
  9. Codex Pesticides Residues in Food Online Database (2018) Accessed 5 July 2018
  10. Dagnac T, Garcia-Chao M, Pulleiro P, Garcia-Jares C, Llompart M (2009) Dispersive solid-phase extraction followed by liquid chromatography–tandem mass spectrometry for the multi-residue analysis of pesticides in raw bovine milk. J Chromatogr A 1216(18):3702–3709CrossRefGoogle Scholar
  11. De Belder T (2018) Implications of restricted use for neonics in the EU. USDA Foreign Agricultural Service (FAS) Washington, DC. Gain Report No.: E18030. Accessed 1 Oct 2018
  12. Elbert A, Haas M, Springer B, Thielert W, Naven R (2008) Applied aspects of neonicotinoid uses in crop protection. Pest Manag Sci 64:1099–1105CrossRefGoogle Scholar
  13. FAO (2006) Thiacloprid. FAO JMPR report, 230Google Scholar
  14. FAO (2008) Imidacloprid. FAO JMPR report, 217Google Scholar
  15. FAO (2010a) Clothianidin. FAO JMPR report, 107Google Scholar
  16. FAO (2010b) Thiamethoxam. FAO JMPR report, 313Google Scholar
  17. FAO (2011) Acetamiprid. FAO JMPR report, 23Google Scholar
  18. Jeschke P, Nauen R, Schindler M, Elbert A (2011) Overview of the status and global strategy for neonicotinoids. J Agric Food Chem 59(7):2897–2908CrossRefGoogle Scholar
  19. Jeschke P, Nauen R, Beck ME (2013) Nicotinic acetylcholine receptor agonists: a milestone for modern crop protection. Angew Chem Int Ed 52:9464–9485CrossRefGoogle Scholar
  20. Khraishy M (2017) Jordan—Food and Agricultural Import Regulations and Standards—Narrative. USDA Foreign Agricultural Service (FAS) Washington, DC. Gain Report No.: JO160015. Accessed 5 July 2018
  21. Lachat L, Glauser G (2018) Development and validation of an ultra-sensitive UHPLC–MS/MS method for neonicotinoid analysis in milk. J Agric Food Chem 66(32):8639–8646CrossRefGoogle Scholar
  22. Limay-Rios V, Forero LG, Xue Y, Smith J, Baute T, Schaafsma A (2016) Neonicotinoid insecticide residues in soil dust and associated parent soil in fields with a history of seed treatment use on crops southwestern Ontario. Environ Toxicol Chem 35(2):303–310CrossRefGoogle Scholar
  23. Liu S, Zheng Z, Wei F, Ren Y, Gui W, Wu H, Zhu G (2010) Simultaneous determination of seven neonicotinoid pesticide residues in food by ultraperformance liquid chromatography tandem mass spectrometry. J Agric Food Chem 58(6):3271–3278CrossRefGoogle Scholar
  24. Marei A, Salah N, Al-Rimawi F, Khayat S, Damiri B, Naser A (2017) Assessment of commonly used pesticides in the ground water of the shallow aquifer systems in Jericho and Jeftlik areas/lower Jordan valley, occupied Palestinian territories. Int J Environ Agric Res 3(2):53–59Google Scholar
  25. Nasir K, Yousif Y. Bilto YY, Al-Shuraiki Y (1998) Residues of chlorinated hydrocarbon insecticides in human milk of Jordanian women. Environ Pollut 99:141–148CrossRefGoogle Scholar
  26. Sait B, Levent A, Veli G, Muhsin K (2010) Organochlorine pesticide (OCP) residues in cow’s, buffalo’s, and sheep’s milk from Afyonkarahisar region, Turkey. Environ Monit Assess 181:555–562Google Scholar
  27. Salem NM, Ahmad R, Estaitieh H (2009) Organochlorine pesticide residues in dairy products in Jordan. Chemosphere 77:673–678CrossRefGoogle Scholar
  28. SANTE (European Commission, Directorate General for Health and Food Safety) (2017) Guidance document on analytical quality control and method validation procedures for pesticide residues and analysis in food and feed. SANTE/11813/2017Google Scholar
  29. Seccia S, Fidente P, Montesano D, Morrica P (2008) Determination of neonicotinoid insecticides residues in bovine milk samples by solid-phase extraction clean-up and liquid chromatography with diode-array detection. J Chromatogr A 1214:115–120CrossRefGoogle Scholar
  30. Simon-Delso N, Amaral-Rogers V, Belzunces LP, Bonmatin JM, Chagnon M et al (2015) Systemic insecticides (neonicotinoids and fipronil): trends, uses, mode of action and metabolites. Environ Sci Pollut Res 22:5–34CrossRefGoogle Scholar
  31. Tian H (2011) Determination of chloramphenicol, enrofloxacin and 29 pesticides residues in bovine milk by liquid chromatography–tandem mass spectrometry. Chemosphere 83(3):349–355CrossRefGoogle Scholar
  32. Van Timmeren S, Wise JC, Vandervoort C, Isaacs R (2011) Comparison of foliar and soil formulations of neonicotinoid insecticides for control of potato leafhopper, Empoasca fabae (Homoptera: Cicadellidae), in wine grapes. Pest Menag Sci 67:560–567CrossRefGoogle Scholar
  33. Venot JP, Molle F, Hassan Y (2007) Irrigated agriculture, water pricing and water savings in the Lower Jordan River Basin (in Jordan). Colombo (LK): International Water Management Institute (IWMI). Comprehensive Assessment of Water Management in Agriculture—Research Report 18. Accessed 17 July 2018
  34. Vo DT, Hsu WH, Abu-Basha EA, Martin RJ (2010) Insect nicotinic acetylcholine receptor agonists as flea adulticides in small animals. J Vet Pharmacol Ther 33:315–322Google Scholar
  35. Wood TJ, Goulson D (2017) The environmental risks of neonicotinoid pesticides: a review of the evidence post 2013. Environ Sci Pollut Res Int 24(21):17285–17325CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Reparto chimico degli alimentiIstituto Zooprofilattico Sperimentale della Lombardia e dell’Emilia Romagna “Bruno Ubertini”BolognaItaly
  2. 2.Department of Veterinary Medical SciencesUniversity of BolognaOzzano dell’Emilia (BO)Italy
  3. 3.Department of Veterinary Clinical SciencesJordan University of Science and TechnologyIrbidJordan

Personalised recommendations