Skip to main content

Determination of 57 pesticide residues in fishery products by GC tandem mass spectrometry combined with QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction


An analytical method using GC–MS/MS combined with quick, easy, cheap, effective, rugged, and safe extraction was developed to determine 57 pesticides in fishery products. The limits of detection and quantification (LOD and LOQ, respectively) of the analytical method ranged between 0.91 and 2.12 ng/g wet mass and 3 and 7 ng/g wet mass, respectively. Moreover, the linearity of the calibration curves was acceptable (R2 > 0.99). The relative pesticide recoveries ranged between 53.87 and 127.2%, and reproducibility ranged between 0.25 and 10.87%. The pesticide residues in brown seaweed, eel, flatfish, shrimp, and abalone samples were analyzed using the developed analytical method, and the results indicate that most samples were not contaminated by the 57 target pesticides, except low levels (< 10 ng/g) of 1,1-dichloro-2,2-bis(4-chlorophenyl)ethene, alachlor, ametryn, isoprothiolane, and prometryn in several samples.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2


  • Ambrus Á, Yang YZ. Global Harmonization of maximum residue limits for pesticides. Journal of Agricultural and Food Chemistry. 64: 30-35 (2016)

    Article  CAS  PubMed  Google Scholar 

  • Baker LW, Fitzell DL, Seiber JN, Parker TR, Shibamoto T, Poore MW, Longley KE, Tomlin RP, Propper R, Duncan DW. Ambient air concentrations of pesticides in California. Environmental Science and Technology 30: 1365-1368 (1996)

    Article  CAS  Google Scholar 

  • Caldas SS, Bolzan CM, de Menezes EJ, Escarrone ALV, de Martinez Caspar Martins C, Bianchini A, Primel EG. A vortex-assisted MSPD method for the extraction of pesticide residues from fish liver and crab hepatopancreas with determination by GC-MS. Talanta. 112: 63-68 (2013)

    Article  CAS  Google Scholar 

  • Codex. Guidelines on good laboratory practice in pesticide residue analysis CAC/GL 40–1993. Revision 2003. Available from : Accessed Nov 2022 (2003)

  • Cruzeiro C, Rodriques-Oliveira N, Velhote S, Pardal MÂ, Rocha E, Rocha MJ. Development and application of a QuEChERS-based extraction method for the analysis of 55 pesticides in the bivalve Scrobicularia plana by GC-MS/MS. Analytical and Bioanalytical Chemistry. 408: 3681-3698 (2016)

    Article  CAS  PubMed  Google Scholar 

  • de Oliveira LG, Kurz MHS, Guimarães MCM, Martins ML, Prestes OD, Zanella R, da Silva Ribeiro JN, Gonçalves FF. Development and validation of a method for the analysis of pyrethroid residues in fish using GC-MS. Food Chemistry. 297: 124944 (2019)

    Article  CAS  PubMed  Google Scholar 

  • Duan Y, Guan N, Li P, Li J, Luo J. Monitoring and dietary exposure assessment of pesticide residues in cowpea (Vigna unguiculata L. Walp) in Hainan, China. Food Control. 59: 250-255 (2016)

    Article  CAS  Google Scholar 

  • Elgueta S, Moyano S, Sepúlveda P, Quiroz C, Correa A. Pesticide residues in leafy vegetables and human health risk assessment in North Central agricultural areas of Chile. Food Additives and Contaminants: Part B. 10: 105-112 (2017)

    Article  CAS  Google Scholar 

  • Hong J, Kim HY, Kim DG, Seo J, Kim KJ. Rapid determination of chlorinated pesticides in fish by freezing-lipid filtration, solid-phase extraction and gas chromatography-mass spectrometry. Journal of Chromatography A. 1038: 27-35 (2004)

    Article  CAS  PubMed  Google Scholar 

  • Kawahara J, Horikoshi R, Yamaguchi T, Kumagai K, Yanagisawa Y. Air pollution and young children’s inhalation exposure to organophosphorus pesticide in an agricultural community in Japan. Environment International. 31: 1123-1132 (2005)

    Article  CAS  PubMed  Google Scholar 

  • Lehotay SK. Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. Journal of AOAC International. 90: 485-520 (2007)

    Article  CAS  PubMed  Google Scholar 

  • Li W, Liu D, Li J, Gao J, Zhang C, Wang P, Zhou Z. Matrix solid-phase dispersion combined with GC-MS/MS for the determination of organochlorine pesticides and polychlorinated biphenyls in marketed seafood. Chromatographia. 80: 813-824 (2017)

    Article  CAS  Google Scholar 

  • Mac Loughlin TM, Peluso ML, Etchegoyen MA, Alonso LL, de Castro MC, Percudani MC, Marino DJG. Pesticide residues in fruits and vegetables of the Argentine domestic market: Occurrence and quality. Food Control. 93: 129-138 (2018)

    Article  CAS  Google Scholar 

  • Mingo V, Lötters S, Wagner N. The impact of land use intensity and associated pesticide applications on fitness and enzymatic activity in reptiles – a field study. Sci. Total Envion. 590: 114-124 (2017)

    Article  Google Scholar 

  • Ministry of Food and Drug safety (MFDS). Food Code (N. 2021–54). Available from: Accessed 3. 1st, 2023. (2021)

  • Ministry of Food and Drug Safety (MFDS). Food nutrient composition database. Available from : Accessed Nov. 01, 2022. (2022)

  • Miraglia M, Marvin HJP, Kleter GA, Battilani P, Brera C, Coni E, Cubadda F, Croci L, Santis BD, Dekkers S, Filippi L, Hutjes RWA, Noordam MY, Pisante M, Piva G, Prandini A, Toti L, van den Born GJ, Vespermann A. Climate change and food safety: an emerging issue with special focus on Europe. Food and Chemical Toxicology. 47: 1009-1021 (2009)

    Article  CAS  PubMed  Google Scholar 

  • Park DW, Yang YS, Lee YU, Han SJ, Kim HJ, Kim SH, Kim JP, Cho SJ, Lee D, Song N, Han Y, Kim HH, Cho BS, Chung JK, Kim AG. Pesticide residues and risk assessment from monitoring programs in the largest production area of leafy vegetables in South Korea: A 15-year study. Foods. 10: 425 (2021)

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Peng XT, Jiang L, Gong Y, Hu XZ, Peng LJ, Feng YQ. Preparation of mesoporous ZrO2-coated magnetic microsphere and its application in the multi-residue analysis of pesticides and PCBs in fish by GC-MS/MS. Talanta. 132: 118-125 (2015)

    Article  CAS  PubMed  Google Scholar 

  • Santhi VA, Hairin T, Mustafa AM. Simultaneous determination of organochlorine pesticides and bisphenol A in edible marine biota by GC-MS. Chemosphere. 86: 1066-1071 (2012)

    Article  CAS  PubMed  Google Scholar 

  • Sharma KK, Tripathy V, Sharma K, Gupta R, Yadav R, Devi S, Walia S. Long-term monitoring of 155 multi-class pesticide residues in Indian vegetables and their risk assessment for consumer safety. Food Chemistry. 373: 131518 (2022)

    Article  CAS  PubMed  Google Scholar 

  • Shrivas K, Wu HF. Ultrasonicatio followed by single-drop microextraction combined with GC/MS for rapid determination of organochlorine pesticides from fish. Journal of Separation Science. 31: 380-386 (2008)

    Article  CAS  PubMed  Google Scholar 

  • Stöckelhuber M, Müller C, Vetter F, Mingo V, Lötters S, Wagner N, Bracher F. Determination of pesticides adsorbed on arthropods and gastropods by a micro-QuEChERS approach and GC-MS/MS. Chromatographia. 80: 825-829 (2017)

    Article  Google Scholar 

  • Taverniers, I., Loose, M.D., & Bocksaele, E.V. Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance. Trends in Analytical Chemistry. 23: 535-552. (2004)

    Article  CAS  Google Scholar 

  • Tudi M, Ruan HD, Wang L, Lyu J, Sadler R, Connell D, Chu C, Phung DT. Agriculture development, pesticide application and its impact on the environment. Environmental Research and Public Health. 18: 1112 (2021)

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  • Tuncel SG, Oztas NB, Erduran MS. Air and groundwater pollution in an agriculture region of the Turkish mediterranean coast. Journal of the Air and Waste Management Association. 58: 1240-1249 (2008)

    Article  CAS  PubMed  Google Scholar 

  • Venkateswarlu P, Mohan KR, Kumar CR, Seshaiah K. Monitoring of multi-class pesticide residues in fresh grape samples using liquid chromatography with electrospray tandem mass spectrometry. Food Chemistry. 105: 1760-1766 (2007)

    Article  CAS  Google Scholar 

  • Wilkowska AM, Biziuk M. Rapid method for the determination of organochlorine pesticides and PCBs in fish muscle samples by microwave-assested extraction and analysis of extracts by GC-ECD. Journal of AOAC International. 93: 1987-1994 (2010)

    Article  CAS  PubMed  Google Scholar 

  • Xu F, Liu L, Wei W, Xu R. Determination of five endosulfan pesticides in the fish pond water by dispersive liquid-liquid microextraction combined with GC-MS. Forensic Sciences Research. 2: 40-45 (2017)

    Article  PubMed  PubMed Central  Google Scholar 

  • Yang SW, Yun CI, Moon JY, Lee JG, Kim YJ. Analytical method development and risk characterization of anthraquinone in various types of tea. Food Control. 137: 108923 (2022)

    Article  CAS  Google Scholar 

  • Zikankuba VL, Mwanyika G, Ntwenya JE, James A, Yildiz F. Pesticide regulations and their malpractice implications on food and environment safety. Cogent Food & Agriculture. 5: 1601544 (2019)

    Article  Google Scholar 

Download references


This research was supported by the National Istitute of Fisheries Science, Minisrty of Oceans and Fisheries, Korea (R2023054).

Author information

Authors and Affiliations


Corresponding authors

Correspondence to Joon-Goo Lee or Moo-Hyeog Im.

Ethics declarations

Conflict interest

The authors declare that they have no conflict of interest.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Springer Nature or its licensor (e.g. a society or other partner) holds exclusive rights to this article under a publishing agreement with the author(s) or other rightsholder(s); author self-archiving of the accepted manuscript version of this article is solely governed by the terms of such publishing agreement and applicable law.

Reprints and Permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Lee, H., Kim, M., Park, M. et al. Determination of 57 pesticide residues in fishery products by GC tandem mass spectrometry combined with QuEChERS (quick, easy, cheap, effective, rugged, and safe) extraction. Food Sci Biotechnol (2023).

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • DOI: