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Abstract: A novel analytical method is reported that combines continuous solid-phase extraction and gas chromatography for the determination of 22 carboxylic acids in water. The highly polar and hydrophilic analytes were preferentially sorbed on a mixture of LiChrolut EN–Supelclean ENVI-18 (1:1) sorbent column and eluted with methanol; this extraction process did not require derivatisation. The extract was analysed by gas chromatography coupled to a flame ionisation detector as well as a mass spectrometer with electron impact (EI) or positive chemical ionisation modes. The highest sensitivity was achieved when using MS-EI, with good linearity in calibration curves and low detection limits (2–40ngL−1) for 50mL of sample. The entire procedure from raw aqueous sample to a ready-to-inject methanol solution of the acids requires less than 15min. Another benefit of this method is the good accuracy (recoveries between 93 and 102%) and precision (relative standard deviation, 3.4–6.2%), which allows the determination of carboxylic acids in environmental water and in real chlorinated and ozonated drinking water. [ABSTRACT FROM AUTHOR]

Abstract: A recently introduced two-dimensional fatty acid retention index system (2D-FARI) was used as basis for prediction of equivalent chain lengths (ECL) of fatty acid methyl esters (FAME) on a BPX-70 stationary phase. Models for the relationship between 2D-FARI data and ECL values of a calibration sample with 30 common fatty acids were established by a simple multivariate regression. The models were thereafter applied on 2D-FARI data for other FAMEs and used to predict the ECLs for these compounds. The 2D-FARI values for the fatty acids in the calibration sample are given by definition. Thus, the only information necessary to calculate the ECL value for a compound run under identical conditions as the calibration sample is the 2D-FARI values for the compound, which can be acquired from literature data. The method was validated with test sets analysed with different temperature and flow programs. ECLs of various marine FAME and trans isomers of Eicosapentaenoic and Docosahexaenoic acid were predicted with root mean squared error of prediction from 0.002 to 0.012 ECL units. [Copyright &y& Elsevier]

Abstract: The accurate and reproducible analysis of long-chain polyunsaturated fatty acids (PUFA) is of growing importance. Especially for labeling purposes, clear guidelines are needed in order to achieve optimum accuracy. Since calibration standards cannot be used for method validation due to the instability of PUFAs, there is no direct way to check for the absence of systematic errors. In this study the sources of error that weaken the accuracy were evaluated using theoretical considerations and calibration standards with corrected composition. It was demonstrated that the key role for optimum accuracy lies in the optimization of the split injection system. Even when following the instructions outlined in the official methods of the American Oil Chemist''s Society (AOCS), systematic errors of more than 7% can arise. Clear guidelines regarding system calibration and selection of appropriate internal standards (IS) can improve precision and accuracy significantly. [Copyright &y& Elsevier]