A gas chromatography-mass spectrometry (GC/MS) method for the quantitation of n-alkanes (carbon backbones ranging from 21 to 36 carbon atoms) in forage and fecal samples has been developed. Automated solid-liquid extraction using elevated temperature and pressure minimized extraction time to 30 min per sample as compared to more than 24 h for traditional GC-flame ionization detection methods that use saponification and liquid-liquid extraction. Extraction solvent requirements were also minimized to 10 mL per sample. Under optimal conditions, complete method recoveries, including extraction efficiency, were greater than 91%. The linear dynamic range was 5 to 100 nmol injected onto the column, with a limit of quantitation of 5 nmol. Intra-assay coefficients of variation for the analysis of annual ryegrass (Lolium rigidum), subterranean clover (Trifolium subterranean), and bovine feces ranged from 0.1%-12.9%, where lower concentrations of n-alkane produced a higher degree of imprecision. The reported GC/MS method permits simple, rapid, and precise quantitation of n-alkanes in plant and fecal material and reduces reagent and labor requirements.
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Smith et al. (2007) studied this question.
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