Skip to main content
SpringerLink
Log in

In-house validation and factorial effect analysis of a liquid chromatography–tandem mass spectrometry method for the determination of corticosteroids in bovine and porcine muscle tissue

  • Research Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

A sensitive and robust liquid chromatography–tandem mass spectrometry method allowing the rapid screening and confirmation of ten synthetic corticosteroids in bovine and porcine muscle tissue was developed and validated. The validation was conducted according to Commission Decision 2002/657/EC, Sect. 3.1.3 (“Validation according to alternative models”), by applying a matrix-comprehensive in-house validation concept. The decision limit, detection capability, recovery, repeatability, within-laboratory-reproducibility and measurement uncertainty were calculated. Furthermore, a factorial effect analysis was conducted to identify factors that have a significant influence on the method. To this end, factors considered to be relevant for the method in routine analysis (e.g. operator, duration of storage of the extracts before measurement, different lots of the cartridges and different species) were systematically varied on two levels during the validation study. Subsequently, the extent to which these factors influence the measurement results of the individual analytes was examined.

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

Similar content being viewed by others

References

  1. Blood DC, Radostis OM (1989) Veterinary medicine, 7th edn. Ballière Tindall, London, pp 1129–1130

    Google Scholar 

  2. Philipp H, Goossens L, Limper J, Quirke JF (1991) Effect of dexamethasone isonicotinate on milk yield in ketotic cows. Vet Rec 128:427

    Article  CAS  Google Scholar 

  3. Schimmer BP, Parker K (1996) In: Hardmann JG, Limbird LE (eds) The pharmacological basis of therapeutics, 9th edn. New York, McGraw-Hill

    Google Scholar 

  4. Duchatel JP, Beduin JM, Jauniaux T, Coignoul F, Vindevogel H (1993) Glucocorticoids as doping agents in homing pigeons. Ann Med Vet 137:557–564

    Google Scholar 

  5. Istasse L, De Haan V, Van Eenaeme C, Buts B, Baldwin P, Gielen M, Demeyer D, Bienfait JM (1989) Effect of dexamethasone injections on performance in a pair of monozygotic cattle twins. J Anim Physiol Anim Nutr 62:150–158

    Article  CAS  Google Scholar 

  6. Rijckaert MLJ, Vlemmix HPJ (1992) The growth-promoting effect of glucocorticosteroids. Eindhoven University of Technology, Eindhoven, Department of Chemical Engineering

    Google Scholar 

  7. Courtheyn D, Vercammen J, De Brabander H, Vanderreyt I, Batjoens P, Vanoosthuyze K, Van Peteghem C (1994) Determination of dexamethasone in urine and faeces of treated cattle with negative chemical ionization-mass spectrometry. Analyst 119:2557–2564

    Article  CAS  Google Scholar 

  8. De Wasch K, de Brabander H, Courtheyn D, Van Peteghem C (1998) Detection of corticosteroids in injection sites and cocktails by MSn. Analyst 123:2415–2422

    Article  Google Scholar 

  9. European Council (1996) Council Directive 96/22/EC of 29 April 1996 concerning the prohibition on the use in stockfarming of certain substances having a hormonal or thyrostatic action and of beta-agonists. Off J Eur Communities L 125:3–9

    Google Scholar 

  10. European Parliament and Council (2003) Directive 2003/74/EC of the European Parliament and of the Council of 22 September 2003 amending Council Directive 96/22/EC concerning the prohibition on the use in stockfarming of certain substances having a hormonal or thyrostatic action and of beta-agonists. Off J Eur Communities L 262:17–21

    Google Scholar 

  11. European Council (1996) Council Directive 96/23/EC on measures to monitor certain substances and residues thereof in live animals and animal products. Off J Eur Communities L 125:10–32

    Google Scholar 

  12. European Parliament and Council (2004) Regulation (EC) No 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. Off J Eur Union 165:1–141

    Google Scholar 

  13. European Commission (2010) Commission Regulation (EU) No 37/2010 of 22 December 2009 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Off J Eur Union 15:1–72

    Google Scholar 

  14. Antignac JP, Le Bizec B, Monteau F, Poulain F, André F (2001) Multi-residue extraction-purification procedure for corticosteroids in biological samples for efficient control of their misuse in livestock production. J Chromatogr B 757:11–19

    Article  CAS  Google Scholar 

  15. Van den Hauwe O, Dumoulin F, Elliot C, Van Peteghem C (2005) Detection of synthetic glucocorticoid residues in cattle tissue and hair samples after a single dose administration using LC-MS/MS. J Chromatogr B Analyt Technol Biomed Life Sci 817:215–223

    Article  Google Scholar 

  16. Tölgyesi A, Sharma VK, Fekete S, Lukonics D, Fekete J (2012) Simultaneous determination of eight corticosteroids in bovine tissues using liquid chromatography-tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci 906:75–84

    Article  Google Scholar 

  17. European Commission (2002) 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 Communities L 221:8

    Google Scholar 

  18. Jülicher B, Gowik P, Uhlig S (1998) Assessment of detection methods in trace analysis by means of a statistically based in-house validation concept. Analyst 123:173–179

    Article  Google Scholar 

  19. Jülicher B, Gowik P, Uhlig S (1999) A top-down in-house validation based approach for the investigation of the measurement uncertainty using fractional factorial experiments. Analyst 124:537–545

    Article  Google Scholar 

  20. Rizea Savu S, Silvestro L, Haag A, Sörgel F (1996) A confirmatory HPLC–MS/MS method for ten synthetic corticosteroids in bovine urines. J Mass Spectrom 31:1351–1363

    Article  Google Scholar 

  21. Kim Y, Kim T, Lee W (1997) Detection of corticosteroids in the presence of organic acids in a liquid chromatography eluent using the negative-ion mode of thermospray mass spectrometry. Rapid Commun Mass Spectrom 11:863–868

    Article  CAS  Google Scholar 

  22. Volmer DA, Hui JP (1997) Rapid determination of corticosteroids in urine by combined solid phase microextraction/liquid chromatography/mass spectrometry. Rapid Commun Mass Spectrom 11:1926–1934

    Article  CAS  Google Scholar 

  23. European Commission (2008) Guidelines for the implementation of Decision 2002/657/EC. SANCO/2004/2726-rev 4. http://crl.fougeres.anses.fr/publicdoc/Guidelines-Consolidated_2002-657_2004-2726rev4_en.pdf

  24. Schmidt K, Stachel C, Gowik P (2008) Development and in-house validation of an LC-MS/MS method for the determination of stilbenes and resorcylic acid lactones in bovine urine. Anal Bioanal Chem 391:1199–1210

    Article  CAS  Google Scholar 

  25. Gowik P, Polzer J, Uhlig S (2007) Reference material in residue control: assessment of matrix effects. Accred Qual Assur 12:161–166

    Article  CAS  Google Scholar 

  26. Schmidt KS, Stachel CS, Gowik P (2009) In-house validation and factorial effect analysis of a liquid chromatography-tandem mass spectrometry method for the determination of steroids in bovine muscle. Anal Chim Acta 637:156–164

    Article  CAS  Google Scholar 

  27. Schmidt KS, Stachel CS (2013) In-house validation and factorial effect analysis of a LC-MS/MS method for the determination of steroids in bovine and porcine blood plasma. Food Addit Contam Part A Chem Anal Control Expo Risk Assess. doi:10.1080/19440049.2013.779751

Download references

Acknowledgments

The author wishes to thank M. Grunow (BVL) and D. Holzkamp (BVL) for their technical assistance in the in-house validation study.

Author information

Authors and Affiliations

  1. Federal Office of Consumer Protection and Food Safety (BVL), Unit 501, Mauerstrasse 39-42, 10117, Berlin, Germany

    Kathrin S. Schmidt & Carolin S. Stachel

Authors
  1. Kathrin S. Schmidt
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Carolin S. Stachel
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Kathrin S. Schmidt.

Additional information

Dr. Carolin Stachel regrettably deceased in January 2013.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Schmidt, K.S., Stachel, C.S. In-house validation and factorial effect analysis of a liquid chromatography–tandem mass spectrometry method for the determination of corticosteroids in bovine and porcine muscle tissue. Anal Bioanal Chem 405, 6287–6297 (2013). https://doi.org/10.1007/s00216-013-7052-5

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-013-7052-5

Keywords

Search

Navigation