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Parameter Validation of Analytical Methods of Insecticide Residue Analyses in Foods of Animal Origin, Feed and Water

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The study was conducted to examine the interrelationship and coherence of analytical parameters in method validation. Recovery, sensitivity, linearity, precision and limits of detection (LOD) were tested in six methods for organochlorine and organophosphate insecticides. Compounds that fell out of the stipulated recovery, 70–120%, in a matrix have concurrently failed to meet the requirements for sensitivity (≥0.7), linearity (R2 > 0.99) and precision (<0.2) in the same matrix. Highest LOD was recorded in those compounds and matrices. Different from the conventional point estimate, a new approach was introduced for setting upper and lower confidence limits of the LOD in quantitative analyses.

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  1. AOAC/FAO/IAEA/IUPAC (1999) Guidelines for single-laboratory validation of analytical methods for trace-level concentrations of organic chemicals. Available via http://www.iaea.org/trc/pest-qa. Accessed 15 March 2009

  2. Barwick VJ, Ellison LR (1999) Measurement uncertainty: approaches to the evaluation of uncertainties associated with recovery. Analyst 124:981–990

  3. CAC (1999) Recommended methods of sampling for the determination of pesticide residues for compliance with MRL. Document No. CAC/GL 33

  4. Caldas SS, Demoliner A, Primel EG (2009) Validation of a method using solid phase extraction and liquid chromatography for the determination of pesticide residues in groundwaters. J Brazilian Chem Soc 20:125–132

  5. DFG (Deutsche Forschungsgemeinschaft) (1992) Manual of pesticide residue analysis, vol 2. VCH mbH, Weinheim

  6. Hill AR, Reynolds SL (1999) Guidelines for in-house validation of analytical methods for pesticide residues in food and animal feed. Analyst 124:953–958

  7. IUPAC (1995) Nomenclature in evaluation of analytical methods including detection and quantification capabilities. Pure Appl Chem 67:1699–1723

  8. Kan CA, Meijer GA (2007) The risk of contamination of food with toxic substances present in animal feed. Anim Feed Sci Technol 133:84–108

  9. MacNeil JD, Patterson J, Martz V (2000) Validation of analytical methods proving your method is “fit for purpose”. In: Fajgelj A, Ambrus A (eds) Principles and practices of method validation. RSC, Cambridge, p 305

  10. Quevauviller P, Morabito R (2000) Evaluation of extraction recoveries for organometallic determinations in environmental matrices. Trends Anal Chem 19:86–96

  11. Rodrigues MV, Reyes FG, Magalhães PM, Rath S (2007) GC-MS determination of organochlorine pesticides in medicinal plants harvested in Brazil. J Brazilian Chem Soc 18:135–142

  12. SANCO (2007) Method validation and quality control procedures for pesticide residue analysis in food and feed. Document no. SANCO/2007/3131

  13. Sharma KK (2007) Pesticide residue analysis manual. ICAR, New Delhi

  14. Trullols E, Ruisánchez I, Rius FX, Òdena M, Feliu MT (2004) Qualitative method for determination of aflatoxin B1 in nuts. J AOAC Int 87:417–423

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Correspondence to Amsalu Debebe.

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Debebe, A., Kuttalam, S. Parameter Validation of Analytical Methods of Insecticide Residue Analyses in Foods of Animal Origin, Feed and Water. Bull Environ Contam Toxicol 86, 571–575 (2011). https://doi.org/10.1007/s00128-011-0284-1

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  • Analytical methods
  • Parameters
  • LOD