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J AOAC Int


Title:Determination of volatile compounds in wine by gas chromatography-flame ionization detection: comparison between the U.S. Environmental Protection Agency 3sigma approach and Hubaux-Vos calculation of detection limits using ordinary and bivariate least squares
Author(s):Caruso R; Scordino M; Traulo P; Gagliano G;
Address:"Department of Food Processing Products Quality Safeguard and Fraud Repression Central Inspectorate (I.C.Q.R.F.), Catania Laboratory, Via Alessandro Volta, 19-95122 Catania, Italy. r.caruso@mpaaf.it"
Journal Title:J AOAC Int
Year:2012
Volume:95
Issue:2
Page Number:459 - 471
DOI: 10.5740/jaoacint.11-044
ISSN/ISBN:1060-3271 (Print) 1060-3271 (Linking)
Abstract:"A capillary GC-flame ionization detection (FID) method to determine volatile compounds (ethyl acetate, 1,1-diethoxyethane, methyl alcohol, 1-propanol, 2-methyl-1-propanol, 2-methyl-1-butanol, 3-methyl-1-butanol, 1-butanol, and 2-butanol) in wine was investigated in terms of calculation of detection limits and calibration method. The main objectives were: (1) calculation of regression coefficient parameters by ordinary least-squares (OLS) and bivariate least-squares (BLS) regression models, taking into account errors in both axes; (2) estimation of linear dynamic range (LDR) according to International Conference on Harmonization recommendations; (3) performance evaluation of a method by using three different internal standards (ISs) such as acetonitrile, acetone, and 1-pentanol; (4) evaluation of LODs according to the U.S. Environmental Protection Agency (EPA) 3sigma approach and the Hubaux-Vos (H-V) method; (5) application of H-V theory to a gas chromatographic analytical method and to a food matrix; and (6) accuracy assessment of the method relative to methyl alcohol content through a Unione Italiana Vini (UIV) interlaboratory proficiency test. Calibration curves calculated via BLS and OLS show similar slopes, while intercepts are closer to zero in the first case, independent of the chosen IS. The studied ISs show a substantially equivalent behavior, even though the IS closer to the analyte retention time seems to be more appropriate in terms of LDR and LOD. Results indicate an underestimation of LODs using the EPA 3sigma approach instead of the more realistic H-V method, both with OLS and BLS regression models. Methanol contents compared with UIV average values indicate recovery between 90 and 110%"
Keywords:Flame Ionization/*methods Food Analysis Sensitivity and Specificity United States United States Environmental Protection Agency/*standards Volatile Organic Compounds/*chemistry Wine/*analysis;
Notes:"MedlineCaruso, Rosario Scordino, Monica Traulo, Pasqualino Gagliano, Giacomo eng England 2012/06/02 J AOAC Int. 2012 Mar-Apr; 95(2):459-71. doi: 10.5740/jaoacint.11-044"

 
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