Rapid analysis of organic farming insecticides in soil and produce using ultra-performance liquid chromatography/tandem mass spectrometry
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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.
KeywordsEcological insecticides Soil Food QuEChERS UPLC-MS/MS
This work was financially supported by the Polish Ministry of Science and Higher Education, Grant No. NN 310 4358 33r. The authors thank Stanisław Walorczyk, Ph.D., for helpful discussions.
- 4.Kowalska J ISOFAR/IFOAM/Organic World Congress Proceedings, Modena 18-20 June 2008, 1, 532-535Google Scholar
- 5.Kowalska J (2008) Ecol Chem Eng A 15:939–943Google Scholar
- 6.Tomline CDS (ed) (2000) The Pesticide Manual (12th ed). BCPC: Surrey, UK & the Royal Society of Chemistry: Cambridge, UKGoogle Scholar
- 15.Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) J AOAC Int 86:412–431Google Scholar
- 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.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