Skip to main content

Internal quality control as a tool for planning a robustness study regarding a multiresidue method for pesticides found in olive oil

Abstract

The implementation of the internal quality assurance program allows for demonstration of the performance characteristics of a method, as well as the avoidance of erroneous results. There is increasing concern in testing laboratories to ensure that the analytical process remains stable, giving reliable results under statistical control. Robustness is tested by introducing variations in experimental conditions and examining the effects on the results. The European document SANCO/12495/2011, “Method validation and quality control procedures for pesticide residue analysis in food and feed”, defines robustness as a parameter that can be derived from ongoing method verification. Internal quality control tools, such as the recovery control chart, were employed in this study to enhance the stability of the recovery rates and to investigate the experimental conditions that have a major influence on the quantification of recovery rates. The method investigated in this study permitted us to investigate eighteen pesticides in olive oil by using a gas chromatography–mass spectrometry technique. This method has been accredited to ISO/IEC 17025:2005 standards and was applied for 1 year in routine conditions for pesticide residues at the Italian National Reference Laboratory. The recovery control chart has showed that all recovery rates for 1 year were close to the maximum limit (120 %) of recovery performance criteria. Consequently, a “positive” bias has affected all data over longer periods of time. A robustness test was planned in order to investigate the grounds that most influenced the variability of the results. The robustness test involved the following three parameters: solvent used to dissolve the final extract, internal standards, and type of olive oil.

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

Fig. 1
Fig. 2
Fig. 3

References

  1. Martínez Vidal J, Garrido Frenich A (2006) Pesticide. Humana Press, New Jersey

    Google Scholar 

  2. European Communities. Dir 91/414/EC Council Directive of 15 July 1991 concerning the placing of plant protection products on the market. In: official journal of the European communities n. L230/1

  3. European Union. Reg (EC) 1107/2009. Regulation of the European Parliament and of the Council of 21 October 2009 concerning the placing of plant protection products on the market and repealing Council Directives 79/117/EEC and 91/414/EEC. In: official journal of the European union n. L309/1

  4. European Commission. Commission implementing Regulation (EU) n 1274/2011 of 7 December 2011 concerning a coordinated multiannual control program of the Union for 2012. 2013 and 2014 to ensure compliance with maximum residue levels of pesticides and to assess the consumer exposure to pesticide residues in and on food of plant and animal origin. In: official journal of the European union L325/24

  5. European Council. Regulation (EC) No 396/2005 of the European Parliament and of the Council of 23 February 2005 on maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending Council Directive 91/414/EEC. In: official journal of the European union L70/1

  6. European Council. Commission Regulation (EC) n. 149/2008 of 29 January 2008 amending regulation (EC) n. 396/2005 of the European Parliament and of the Council by establishing Annexes II. III and IV setting maximum residue levels for products covered by Annex I thereto. In: official journal of the European union L58/1

  7. Italian Ministerial Decree of 23 December 1992 transposing the Community Directive 90/642/EEC on the fixing of maximum levels for pesticide residues in and on ceratin products of plant origin including fruit and vegetables. In: official journal of the European communities n. L350/71

  8. European Parliament and Council. Regulation (EC) n. 882/2004 of the European Parliament and of the Council of 29 April 2004 on official controls performed to ensure the verification of compliance with feed and food law. Animal health and animal welfare rules. In: official journal of the European union L165/1

  9. European Standard. EN ISO/IEC 17025:2005 General requirements for the competence of testing and calibration laboratories

  10. Directorate General for Health and Consumer Affairs (DG SANCO) (2011). Method validation and quality control procedures for pesticide residues analysis in food and feed. In: SANCO/12495/2011 Brussels. Belgium

  11. Taverniers I, De Loose M, Van Bockstaele E (2004) Trends in quality in the analytical laboratory II. Analytical method validation and quality assurance. Trends in. Anal Chem 23(8):535–552

    CAS  Google Scholar 

  12. Bertoni Olivares IR, Antunes Lopes F (2012) Essential steps to providing reliable results using the analytical quality assurance cycle. Trends in Anal Chem 35:109–121

    Article  Google Scholar 

  13. Egea Gonzales FJ, Hernandez Torres ME, Garrido Frenich A, Martinez Vidal JL, Garcia Campana AM (2004) Internal quality control and laboratory management tools for enhancing the stability of results in pesticide multi-residue analytical methods. Trends in Anal Chem 23(5):361–368

    Article  Google Scholar 

  14. Bonet-Domingo E, Grau-Gonzalez S, Martin-Biosca Y, Martin-Biosca Y, Medina-Hernandez MJ, Sagrado S (2007) Harmonized internal quality aspects of a multi-residue method for determination of forty-six semi volatile compounds in water by stir-bar-sorptive extraction-thermal desorption gas chromatography-mass spectrometry. Anal Bioanl Chem 387:2537–2545

    Article  CAS  Google Scholar 

  15. International Standard Organization ISO 8258 (2004) Shewhart control charts

  16. NORDEST Report TR 569 (2011) Handbook internal quality control for chemical laboratories, 4th edn. Nordic Innovation, Oslo Norway

    Google Scholar 

  17. CITAC/EURACHEM. Guide to quality in analytical chemistry. An aid to accreditation. Edition 2002

  18. EURACHEM (1998) The fitness for purpose of analytical methods. A laboratory guide to method validation and related topics 1st ed

  19. International Union of Pure and Applied Chemistry (IUPAC) (2002) Technical report harmonized guidelines for single-laboratory validation of methods of analysis. Pure Appli Chem 74(5):835–855

    Article  Google Scholar 

  20. Youden WJ, Steiner EH (1975) Statistical manual of the association of official analytical chemists. Arlington VA USA

  21. Thompson M, Wood R (1995) Harmonized guidelines for internal quality control in analytical chemistry laboratories. Pure Appl Chem 67(4):649–666

    Article  CAS  Google Scholar 

  22. Konieczka P (2007) The role of and the place of method validation in the quality assurance and quality control (QA/QC) system. Crit Rev Anal Chem 37:173–190

    Article  CAS  Google Scholar 

  23. Amadeo I, Mauro LV, Ortì E, Forno G (2011) Determination of robustness and optimal work conditions for a purification process of a therapeutic recombinant protein using response surface methodology. Biotechnol Prog 27(3):724–732

    Article  CAS  Google Scholar 

  24. Masson P (2007) Quality control techniques for routine analysis with liquid chromatography in laboratories. J Chrom A 1158:168–173

    Article  CAS  Google Scholar 

  25. Boqué R, Maroto A, Riu J, Xavier Rius F (2002) Validation of analytical methods. Grasas Aceites 53(1):128–143

    Google Scholar 

  26. Dejaegher B, Vander Heyden Y (2007) Ruggedness and robustness testing. J Chrom A 1158:138–157

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Tiziana Generali.

Rights and permissions

Reprints and Permissions

About this article

Cite this article

Stefanelli, P., Generali, T., Girolimetti, S. et al. Internal quality control as a tool for planning a robustness study regarding a multiresidue method for pesticides found in olive oil. Accred Qual Assur 18, 313–322 (2013). https://doi.org/10.1007/s00769-013-0986-7

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00769-013-0986-7

Keywords

  • Robustness study
  • Pesticide
  • Multiresidue method
  • Olive oil
  • Internal quality control