Development of non-aqueous single stage derivatisation method for the determination of putrescine and cadaverine using GC-MS

Abstract

A single step derivatisation for the determination of putrescine and cadaverine by gas chromatography using trifluoroacetylacetone (TFAA) in methanol or ethanol was studied and optimised. The derivatives were analysed by an iontrap gas chromatograph-mass spectrometer (GC-MS) operating with electron impact ionisation with selective ion storage (EI-SIS) mode. The optimised mole ratios for TFAA/putrescine and TFAA/ cadaverine reactions were 5/1 and 5.8/1 respectively with a reaction time of 15 minutes at 95°C. The retention times for the derivatised putrescine and cadaverine were 11.3 and 12.2 minutes respectively using the capillary column, CP-Sil 8CB; 30 m length × 0.25 mm i.d. × 0.25 mm film. The correlation coefficients (R2) of calibration curves for putrescine and cadaverine were 0.991 and 0.990 respectively over a concentration range of 100 ng cm-3 to 1500 ng cm-3. The method developed was found to be simple (single-stage derivatisation), rapid (15 minutes derivatisation & 14 minutes GC/MS run) and accurate (putrescine and cadaverine recoveries 94.8%-97.7%). © Versita Warsaw and Springer-Verlag Berlin Heidelberg 2008.