Analytical and Bioanalytical Chemistry

, Volume 394, Issue 8, pp 2241–2247 | Cite as

Rapid analysis of organic farming insecticides in soil and produce using ultra-performance liquid chromatography/tandem mass spectrometry

Original Paper

Abstract

A new method for the analysis of three ecological insecticides, namely azadyrachtin, spinosad (sum of spinosyn A and spinosyn D) and rotenone, in produce and soil samples is presented. Investigated compounds are one of the most significant insecticides authorized for organic farming crop protection in many countries. Extraction of the pesticides from plant and soil matrices was performed by using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The method entailed a single extraction of the investigated compounds with acidified acetonitrile followed by a dispersive solid-phase extraction cleanup step prior to the final determination by reverse-phase ultra-performance liquid chromatography/tandem quadrupole mass spectrometry (UPLC-MS/MS). Validation studies were carried out on cabbage, tomato and soil samples. Recoveries of the spiked samples were in the range between 67% and 108%, depending on the matrix and the spiking level. Relative standard deviations for all matrix–compound combinations did not exceed 12%. The limits of quantification were ≤0.01 mg kg−1 in all cases, except for azadirachtin. The developed method was applied to the analysis of real samples originating from organic farming production.

Keywords

Ecological insecticides Soil Food QuEChERS UPLC-MS/MS 

References

  1. 1.
    Scott RH, O'Brien K, Roberts L, Mordue W, Luntz M (1999) J Comp Biochem Physiol C Pharmacol Toxicol Endocrinol 123:85–93CrossRefGoogle Scholar
  2. 2.
    Sparks TC, Crouse GD, Durst G (2001) Pest Manag Sci 57:896–905CrossRefGoogle Scholar
  3. 3.
    Salgado VL (1998) Pestic Biochem Physiol 60:91–102CrossRefGoogle Scholar
  4. 4.
    Kowalska J ISOFAR/IFOAM/Organic World Congress Proceedings, Modena 18-20 June 2008, 1, 532-535Google Scholar
  5. 5.
    Kowalska J (2008) Ecol Chem Eng A 15:939–943Google Scholar
  6. 6.
    Tomline CDS (ed) (2000) The Pesticide Manual (12th ed). BCPC: Surrey, UK & the Royal Society of Chemistry: Cambridge, UKGoogle Scholar
  7. 7.
    West SD, Turner LG (2000) J Agric Food Chem 48:366–372CrossRefGoogle Scholar
  8. 8.
    Jiménez JJ, Bernal JL, del Nozal MJ, Novo M, Higes M, Llorente J (2000) J Chromatogr A 871:67–73CrossRefGoogle Scholar
  9. 9.
    Schwedler DA, Thomas AD, Yeh L-T (2000) J Agric Food Chem 48:5138–5145CrossRefGoogle Scholar
  10. 10.
    Caboni P, Sarais G, Angioni A, Garau VL, Cabras P (2005) J Agric Food Chem 53:8644–8649CrossRefGoogle Scholar
  11. 11.
    Sannino A (2007) Rapid Commun Mass Spectrom 21:2079–2086CrossRefGoogle Scholar
  12. 12.
    Sarais G, Caboni P, Sarritzu E, Russo M, Cabras P (2008) J Agric Food Chem 56:2939–2943CrossRefGoogle Scholar
  13. 13.
    Schaaf O, Jarvis AP, van der Esch SA, Giagnacovo G, Oldham NJ (2000) J Chromatogr A 886:89–97CrossRefGoogle Scholar
  14. 14.
    Dai J, Yaylayan VA, Vijaya Raghavan GS, Pare JR (1999) J Agric Food Chem 47:3738–3742CrossRefGoogle Scholar
  15. 15.
    Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) J AOAC Int 86:412–431Google Scholar
  16. 16.
    Walorczyk S (2007) J Chromatogr A 1165:200–212CrossRefGoogle Scholar
  17. 17.
    Pizzutti IR, de Kok A, Zanella R, Adaime MB, Hiemstra M, Wickert C, Prestes OD (2007) J Chromatogr A 1142:123–136CrossRefGoogle Scholar
  18. 18.
    European Commission, Method Validation and Quality Control Procedures for Pesticide Residues Analysis in Food and Feed, Document No. SANCO/2007/3131, Brussels, 31 October 2007Google Scholar
  19. 19.
    Commission Decision (2002/657/EC) of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results, Off. J. Eur. Comm., No. L221/8,17 August 2002Google Scholar

Copyright information

© Springer-Verlag 2009

Authors and Affiliations

  1. 1.Institute of Plant Protection, National Research InstitutePoznańPoland

Personalised recommendations