Validation of SPME-GC and HS-GC procedures for the determination of selected solvent residues in edible oil matrices

• Published in: Accreditation and quality assurance Vol. 12; no. 2; pp. 94 - 104
• Main Authors: MICHULEC, Magdalena, WARDENCKI, Waldemar
• Format: Journal Article
• Language: English
• Published: Heidelberg Springer 01-02-2007; Berlin Springer Nature B.V
• Subjects: Analytical chemistry; Benzene; Beta decay; Calibration; Chemistry; Chloroform; Chromatographic methods and physical methods associated with chromatography; Chromatography; Electron capture detectors; Exact sciences and technology; Flame ionization detectors; Food; Gas chromatographic methods; Gas chromatography; Helium; Hexanes; Hydrocarbons; Nitrogen; Oils & fats; Residues; Sensors; Solid phases; Solvents; Toluene; Trichloroethane; Electron capture detector; Uncertainty; Headspace analysis; Toluene; Microanalysis; Flame ionization detector; Edible oil; Chemical enrichment; Solid phase microextraction; Gas chromatography; Repeatability; Sample preparation; Validation parameters; Residue; Benzene; Chlorocarbon; Detection limit; Linearity; Headspace; Hexane; Procedure development; Comparative study
• ISSN: 0949-1775; 1432-0517
• DOI: 10.1007/s00769-006-0235-4

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.