M. Adam et al., Comparison of attenuated total reflection infrared spectroscopy to capillary gas chromatography for trans fatty acid determination, J AM OIL CH, 76(3), 1999, pp. 375-378
Gas chromatography (GC) has been a standard analytical tool in lipid chemis
try. The rapid attenuated total reflection (ATR) infrared (IR) American Oil
Chemists' Society (AOCS) Recommended Practice (Cd 14d-97) was compared to
the capillary GC AOCS Recommended Practice (Ce 1f-97) that was optimized to
accurately determine total trans fatty acids on highly polar stationary ph
ases. This comparative evaluation was validated in an independent laborator
y. These procedures were used to quantitate the total trans fatty acid leve
ls in partially hydrogenated vegetable oils, measured as neat(without solve
nt) triacylglycerols (TAG) by ATR and as fatty acid methyl ester (FAME) der
ivatives by capillary GC. Unlike FAME, TAG determination by ATR required no
derivatization, but samples had to be melted prior to measurement. Five bl
ind replicates for each of three accuracy standards and three test samples
were analyzed by each technique. The GC and ATR determinations were in good
agreement. Accuracy was generally high. The ratios of ATR mean trans value
s (reported as percentage of total TAG) to the true values (based on the am
ount of trielaidin added gravimetrically) were 0.89, 0.98, and 1.02 for acc
uracy standards having about 1, 10, and 40% trans levels. The corresponding
GC values, determined as percentage of total FAME, were 0.98, 0.99 and 1.0
4. The ratios of mean trans values determined by these techniques were ATR/
GC 0.85, 1.04, and 1.01 for test samples having trans levels of about 0.7,
8, and 38%, respectively. The optimized GC procedure also minimized the exp
ected low bias in trans values due to GC peak overlap found with the GC Off
icial Method Ce 1c-89. Satisfactory repeatability and reproducibility were
obtained by both ATR and GC.