Skip to main content
SpringerLink
Log in

Application of dispersive liquid–liquid microextraction followed by gas chromatography/mass spectrometry as effective tool for trace analysis of organochlorine pesticide residues in honey samples

  • Original Paper
  • Published:
Journal of the Iranian Chemical Society Aims and scope Submit manuscript

Abstract

A dispersive liquid–liquid microextraction (DLLME) method followed by gas chromatography/mass spectrometry (GC/MS) was applied for the trace determination of organochlorine pesticides in honey samples. The type and volume of organic extraction and disperser solvents, pH, effect of added salt content and centrifuging time and speed were optimized to find the appropriate extraction conditions. In DLLME, 30 µL of 1,2-dibromomethane (serving as extractant) and 1.5 mL of acetonitrile (serving as disperser) were applied. The limit of detection (3 s) and limit of quantification (10 s) for all the analytes of interest (organochlorine pesticides) varied from 0.004 to 0.07 and from 0.02 to 0.3 ng g−1, respectively. The extraction recovery ranged from 91 to 100 %, and the enrichment factors ranged from 171 to 199. The relative standard deviation was <6 % for intraday (n = 6) and <8 % interday (n = 4) measurements. The proposed DLLME–GC/MS method was confirmed to be fast, simple to perform, friendly to environment and suitable for analysis of organochlorine pesticide residues at trace levels in honey samples.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5

Similar content being viewed by others

References

  1. Y. Zhang, H.K. Lee, Determination of ultraviolet filters in water samples by vortex-assisted dispersive liquid–liquid microextraction followed by gas chromatography–mass spectrometry. J. Chromatogr. 1249, 25–31 (2012)

    Article  CAS  Google Scholar 

  2. D. Tsipi, M. Triantafyllou, A. Hiskia, Determination of organochlorine pesticide residues in honey, applying solid phase extraction with RP-C18 material†. Analyst 124(4), 473–475 (1999)

    Article  CAS  Google Scholar 

  3. M. Fontcuberta et al., Chlorinated organic pesticides in marketed food: Barcelona, 2001–06. Sci. Total Environ. 389(1), 52–57 (2008)

    Article  CAS  Google Scholar 

  4. D.Q. Hung, W. Thiemann, Contamination by selected chlorinated pesticides in surface waters in Hanoi, Vietnam. Chemosphere 47(4), 357–367 (2002)

    Article  CAS  Google Scholar 

  5. L. Guzzella, F. Pozzoni, G. Giuliano, Herbicide contamination of surficial groundwater in Northern Italy. Environ. Pollut. 142(2), 344–353 (2006)

    Article  CAS  Google Scholar 

  6. S. Meijer et al., Air-soil exchange of organochlorine pesticides in agricultural soils. 1. Field measurements using a novel in situ sampling device. Environ. Sci. Technol. 37(7), 1292–1299 (2003)

    Article  CAS  Google Scholar 

  7. M. Gonzalez et al., Occurrence and distribution of organochlorine pesticides (OCPs) in tomato (Lycopersicon esculentum) crops from organic production. J. Agric. Food Chem. 51(5), 1353–1359 (2003)

    Article  CAS  Google Scholar 

  8. C. Blasco et al., Assessment of pesticide residues in honey samples from Portugal and Spain. J. Agric. Food Chem. 51(27), 8132–8138 (2003)

    Article  CAS  Google Scholar 

  9. Ö. Erdoğrul, Levels of selected pesticides in honey samples from Kahramanmaraş, Turkey. Food Control 18(7), 866–871 (2007)

    Article  Google Scholar 

  10. S. Bogdanov, Contaminants of bee products. Apidologie 37, 1–18 (2006)

    Article  CAS  Google Scholar 

  11. M. Choi, I.-S. Lee, R.-H. Jung, Rapid determination of organochlorine pesticides in fish using selective pressurized liquid extraction and gas chromatography–mass spectrometry. Food Chem. 205, 1–8 (2016)

    Article  CAS  Google Scholar 

  12. Z. Cheng et al., Atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for simultaneous determination of fifteen organochlorine pesticides in soil and water. J. Chromatogr. A 1435, 115–124 (2016)

    Article  CAS  Google Scholar 

  13. J.A. Cai et al., Hollow fiber based liquid phase microextraction for the determination of organochlorine pesticides in ecological textiles by gas chromatography–mass spectrometry. Talanta 146, 375–380 (2016)

    Article  CAS  Google Scholar 

  14. F.M. Malhat et al., Residues of organochlorine and synthetic pyrethroid pesticides in honey, an indicator of ambient environment, a pilot study. Chemosphere 120, 457–461 (2015)

    Article  CAS  Google Scholar 

  15. G. Zheng et al., Multiresidue analysis of 30 organochlorine pesticides in milk and milk powder by gel permeation chromatography-solid phase extraction–gas chromatography–tandem mass spectrometry. J. Dairy Sci. 97(10), 6016–6026 (2014)

    Article  CAS  Google Scholar 

  16. X. Shi et al., Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in seawater samples by membrane-assisted solvent extraction combined with gas chromatography–electron capture detector and gas chromatography–tandem mass spectrometry. J. Chromatogr. B 972, 58–64 (2014)

    Article  CAS  Google Scholar 

  17. M. Kahle et al., Azole fungicides: occurrence and fate in wastewater and surface waters. Environ. Sci. Technol. 42(19), 7193–7200 (2008)

    Article  CAS  Google Scholar 

  18. M.B. Melwanki, M.-R. Fuh, Partitioned dispersive liquid–liquid microextraction: an approach for polar organic compounds extraction from aqueous samples. J. Chromatogr. 1207(1), 24–28 (2008)

    Article  CAS  Google Scholar 

  19. K.B. Borges et al., Simultaneous determination of multibenzodiazepines by HPLC/UV: investigation of liquid–liquid and solid-phase extractions in human plasma. Talanta 78(1), 233–241 (2009)

    Article  CAS  Google Scholar 

  20. A.L. Saber, On-line solid phase extraction coupled to capillary LC-ESI-MS for determination of fluoxetine in human blood plasma. Talanta 78(1), 295–299 (2009)

    Article  CAS  Google Scholar 

  21. S.R. Rissato et al., Supercritical fluid extraction for pesticide multiresidue analysis in honey: determination by gas chromatography with electron-capture and mass spectrometry detection. J. Chromatogr. 1048(2), 153–159 (2004)

    Article  CAS  Google Scholar 

  22. C. Sanchez-Brunete et al., Determination of insecticides in honey by matrix solid-phase dispersion and gas chromatography with nitrogen–phosphorus detection and mass spectrometric confirmation. J. AOAC Int. 85(1), 128–133 (2002)

    CAS  Google Scholar 

  23. Y. Wang et al., Determination of triazines in honey by dispersive liquid–liquid microextraction high-performance liquid chromatography. J. Chromatogr. 1217(26), 4241–4246 (2010)

    Article  CAS  Google Scholar 

  24. A.A. Barakat et al., Simple and rapid method of analysis for determination of pesticide residues in honey using dispersive solid phase extraction and GC determination. J. Food Agric. Environ. 5(2), 97 (2007)

    CAS  Google Scholar 

  25. N. Campillo et al., Solid-phase microextraction and gas chromatography with atomic emission detection for multiresidue determination of pesticides in honey. Anal. Chim. Acta 562(1), 9–15 (2006)

    Article  CAS  Google Scholar 

  26. M. Rezaee et al., Determination of organic compounds in water using dispersive liquid–liquid microextraction. J. Chromatogr. A 1116(1), 1–9 (2006)

    Article  CAS  Google Scholar 

  27. B. Ebrahimpour, Y. Yamini, M. Rezazadeh, A sensitive emulsification liquid phase microextraction coupled with on-line phase separation followed by HPLC for trace determination of sulfonamides in water samples. Environ. Monit. Assess. 187(1), 1–13 (2015)

    Article  CAS  Google Scholar 

  28. A.N. Anthemidis, K.-I.G. Ioannou, On-line sequential injection dispersive liquid–liquid microextraction system for flame atomic absorption spectrometric determination of copper and lead in water samples. Talanta 79(1), 86–91 (2009)

    Article  CAS  Google Scholar 

  29. H. Chen, R. Chen, S. Li, Low-density extraction solvent-based solvent terminated dispersive liquid–liquid microextraction combined with gas chromatography-tandem mass spectrometry for the determination of carbamate pesticides in water samples. J. Chromatogr. 1217(8), 1244–1248 (2010)

    Article  CAS  Google Scholar 

  30. W. Li et al., Development of on-line spectroscopic determination approach of dispersive liquid–liquid microextraction based on an effective device. Spectrochim. Acta Part A Mol. Biomol. Spectrosc. 124, 159–164 (2014)

    Article  CAS  Google Scholar 

  31. B. Horstkotte et al., In-syringe magnetic stirring assisted dispersive liquid–liquid micro-extraction with solvent washing for fully automated determination of cationic surfactants. Anal. Methods 6(24), 9601–9609 (2014)

    Article  CAS  Google Scholar 

  32. E. Ranjbari, M.R. Hadjmohammadi, Magnetic stirring-assisted dispersive liquid–liquid microextraction followed by high performance liquid chromatography for determination of phthalate esters in drinking and environmental water samples. Talanta 100, 447–453 (2012)

    Article  CAS  Google Scholar 

  33. J. Zhou et al., Multiresidue determination of tetracycline antibiotics in propolis by using HPLC-UV detection with ultrasonic-assisted extraction and two-step solid phase extraction. Food Chem. 115(3), 1074–1080 (2009)

    Article  CAS  Google Scholar 

  34. M. Alexovič et al., A single-valve sequential injection manifold (SV-SIA) for automation of air-assisted liquid-phase microextraction: stopped flow spectrophotometric determination of chromium (VI). Anal Methods 5(10), 2497–2502 (2013)

    Article  Google Scholar 

  35. P.-S. Chen, W.-Y. Haung, S.-D. Huang, Analysis of triazine herbicides using an up-and-down-shaker-assisted dispersive liquid–liquid microextraction coupled with gas chromatography–mass spectrometry. J. Chromatogr. B 955, 116–123 (2014)

    Article  Google Scholar 

  36. M. Alexovič et al., An automatic, vigorous-injection assisted dispersive liquid–liquid microextraction technique for stopped-flow spectrophotometric detection of boron. Talanta 133, 127–133 (2015)

    Article  Google Scholar 

  37. L. Rusnáková et al., A dispersive liquid–liquid microextraction procedure for determination of boron in water after ultrasound-assisted conversion to tetrafluoroborate. Talanta 85(1), 541–545 (2011)

    Article  Google Scholar 

  38. V.P. Jofré et al., Optimization of ultrasound assisted-emulsification-dispersive liquid–liquid microextraction by experimental design methodologies for the determination of sulfur compounds in wines by gas chromatography–mass spectrometry. Anal. Chim. Acta 683(1), 126–135 (2010)

    Article  Google Scholar 

  39. A. Bidari et al., Sample preparation method for the analysis of some organophosphorus pesticides residues in tomato by ultrasound-assisted solvent extraction followed by dispersive liquid–liquid microextraction. Food Chem. 126(4), 1840–1844 (2011)

    Article  CAS  Google Scholar 

  40. F. Javanmardi et al., Benzoic and sorbic acid in soft drink, milk, ketchup sauce and bread by dispersive liquid–liquid microextraction coupled with HPLC. Food Addit. Contam. Part B 8(1), 32–39 (2014)

    Article  Google Scholar 

  41. S. Zhang et al., Dispersive liquid–liquid microextraction combined with sweeping micellar electrokinetic chromatography for the determination of some neonicotinoid insecticides in cucumber samples. Food Chem. 133(2), 544–550 (2012)

    Article  CAS  Google Scholar 

  42. M.A. Farajzadeh et al., Determination of some synthetic phenolic antioxidants and bisphenol A in honey using dispersive liquid–liquid microextraction followed by gas chromatography–flame ionization detection. Food Anal. Methods 8(8), 2035–2043 (2015)

    Article  Google Scholar 

  43. M.A. Farajzadeh et al., Development and validation of a rapid and sensitive gas chromatographic method for the analysis of some phenolic compounds in vegetable oils. Anal. Methods 6(14), 5314–5321 (2014)

    Article  CAS  Google Scholar 

  44. P. Reboredo-Rodríguez et al., Ultrasound-assisted emulsification–microextraction for the determination of phenolic compounds in olive oils. Food Chem. 150, 128–136 (2014)

    Article  Google Scholar 

  45. S. Panseri et al., Occurrence of pesticide residues in Italian honey from different areas in relation to its potential contamination sources. Food Control 38, 150–156 (2014)

    Article  CAS  Google Scholar 

  46. Ż. Bargańska, M. Ślebioda, J. Namieśnik, Pesticide residues levels in honey from apiaries located of Northern Poland. Food Control 31(1), 196–201 (2013)

    Article  Google Scholar 

  47. G.P. de Pinho et al., Optimization of the liquid–liquid extraction method and low temperature purification (LLE–LTP) for pesticide residue analysis in honey samples by gas chromatography. Food Control 21(10), 1307–1311 (2010)

    Article  Google Scholar 

  48. C.K. Zacharis et al., Dispersive liquid–liquid microextraction for the determination of organochlorine pesticides residues in honey by gas chromatography–electron capture and ion trap mass spectrometric detection. Food Chem. 134(3), 1665–1672 (2012)

    Article  CAS  Google Scholar 

Download references

Acknowledgments

The authors would like to thank the ‘Drug Applied Research Center of Tabriz University of Medical Science’ for financial assistance.

Author information

Authors and Affiliations

  1. Drug Applied Research Center, Tabriz University of Medical Sciences, Tabriz, Iran

    Mir-Michael Mousavi & Mahboob Nemati

  2. Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran

    Mahboob Nemati

  3. Food and Drug Control Laboratories, Tabriz University of Medical Sciences, Tabriz, Iran

    Mahboob Nemati & Ali Akbar Alizadeh Nabili

  4. Faculty of Nutrition, Tabriz University of Medical Sciences, Tabriz, Iran

    Mir-Michael Mousavi, Mansour mahmoudpour & Seyedrafie Arefhosseini

  5. Students’ Research Committee, Faculty of Nutrition, Tabriz University of Medical Sciences, Tabriz, Iran

    Mir-Michael Mousavi & Mansour mahmoudpour

Authors
  1. Mir-Michael Mousavi
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Mahboob Nemati
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Ali Akbar Alizadeh Nabili
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Mansour mahmoudpour
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Seyedrafie Arefhosseini
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Seyedrafie Arefhosseini.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Mousavi, MM., Nemati, M., Alizadeh Nabili, A.A. et al. Application of dispersive liquid–liquid microextraction followed by gas chromatography/mass spectrometry as effective tool for trace analysis of organochlorine pesticide residues in honey samples. J IRAN CHEM SOC 13, 2211–2218 (2016). https://doi.org/10.1007/s13738-016-0939-2

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s13738-016-0939-2

Keywords

Search

Navigation