Abstract
The validation process – in accordance with the recommendation of the International Conference on Harmonization – was performed in order to define and determine the application of the developed procedures for the determination of solvent residues (hexane, benzene, toluene and chlorinated hydrocarbons – trichloromethane, 1,1,1-trichloroethane, tetrachloromethane, trichloroethene, tetrachloroethene) in oil samples. For extraction and preconcentration of analytes, two simple sample preparation techniques – static headspace analysis (HSA) and solid phase microextraction (SPME) – have been used. Gas chromatography with a flame ionization detector (FID) and electron capture detector (ECD) was applied for the final determination. A critical comparison of developed procedures was conducted considering the values of: limits of detection, concentration ranges, repeatability and uncertainty. The linearity issue was described in details due to the broad measurement ranges of the proposed procedures.
References
Ordinances of the Minister of Health of April 30th,2004 (Dz. U. 04.94.933) on allowed additives and substances assisting food processing (in Polish)
PN-EN ISO 9832 November 2004– Oils and vegetable and animal fats. Determination of residual technical hexane content (in Polish)
European Pharmacopoeia, Edition 5 (2002) – in Polish
Kumar N, Gow J (1994) J Chromatogr A 667:235–240
Peña F, Cárdenas S, Gallego M, Valcárel M (2003) JAOCS 80:613–618
Josephs RD, Derbyshire M, Stroka J, Emons H, Anklam E (2004) Toxicology Lett 153:123–132
International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use: Text on Validation of Analytical Procedures, ICH–Q2A, Geneva 1994
International Conference on Harmonization (ICH) of Technical Requirements for the Registration of Pharmaceuticals for Human Use: Text on Validation of Analytical Procedures: Metrology, ICH–Q2(R1), Geneva 2005
Heydorn K, Anglov Th (2002) Accred Qual Assur 7:153–158
Konieczka P, Namieśnik J, Zygmunt B, Bulska E, Świtaj–Zawadka A, Naganowska A, Kremer E, Rompa M (2004) Evaluation and quality control of analytical results (in Polish) CEEAM, Gdańsk
Emons H, Linsinger TPJ, Gawlik BM (2004) Trends Anal Chem 23:442–449
Konieczka P (2003) Chem Inż Ekol 10:639–654 (in polish)
Geiß S, Einax JW (2001) Fresenius J Anal Chem 370:673–678
Konieczka P (2003) Chem Inż Ekol 10:1071–1100 (in polish)
http://www.waters.com/watersdivision/contentd.asp?watersit= JDRS–5LT6WZ
Konieczka P (2003) Chem Inż Ekol 10:627–637 (in polish)
Wardencki W, Michulec M, Curyło J (2004) Int J Food Sci Tech 39:703–717
Lord H, Pawliszyn J (2000) J Chromatogr A 902:17–63
Świtaj-Zawadka A, Konieczka P, Przyk E, Namieśnik J (2005) Anal Lett 38:353–376
Michulec M, Wardencki W (2004) Chromatographia 60:S273–S277
Michulec M, Wardencki W (2005) J Chromatogr A 1071:119–124
Ellison SLR, Barwick VJ (1998) Analyst 123:1387– 1392
Van Loco J, Elskens M, Croux C, Beernaert H (2002) Accred Qual Assur 7:281–285
Huber W (2004) Accred. Qual. Assur. 9:726–726
EURACHEM Guide: The Fitness for Purpose of Analytical Methods, First Internet Version,1998
Ellison SLR, Rosslein M, Williams A (eds) (2000) Eurachem/CITAC Guide, Quantifying Uncertainty in Analytical Measurements, 2nd edn, Available from: www.measurementuncertainty.org
http://mot.vuse.vanderbilt.edu/mt322/Ishikawa.htm
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Michulec, M., Wardencki, W. Validation of SPME-GC and HS-GC procedures for the determination of selected solvent residues in edible oil matrices. Accred Qual Assur 12, 94–104 (2007). https://doi.org/10.1007/s00769-006-0235-4
Received:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00769-006-0235-4