title: Determination of biogenic diamines with a vaporisation derivatisation approach using solid-phase microextraction gas chromatography-mass spectrometry.
abstract: A gas-phase on-fibre derivatisation method for the determination of putrescine and cadaverine by gas chromatography/mass spectrometry using trifluoroacetylacetone (TFAA) has been studied and optimised. Small amounts (2μl) of putrescine, cadaverine and TFAA standards were vaporised at high temperature in a 20cm(3) closed SPME vial. The subsequent derivatives were recovered from the headspace of the vial using a PDMS/DVB fibre. The optimised mole ratio for [TFAA]/[Putrescine+Cadaverine] reaction was 22.3/1 with a derivatisation and extraction temperature of 120(o)C and an extraction time of 20min. The retention times for the derivatised putrescine and cadaverine were 20.5 and 22.2min, respectively on a capillary column, CP-Sil 8CB; 30m length×0.25mmi.d.×0.25μm film thickness. The correlation coefficients (R(2)) of calibration curves for putrescine and cadaverine were 0.999 and 0.997, respectively over a range of sample masses of 20-350ng, using nonadecane as an internal standard. Putrescine and cadaverine recoveries were determined to be 93.9% and 103.3%, respectively. The method was found to be a straightforward single step procedure that was unaffected by complex sample matrices and was successfully tested on samples of meat, vegetables and cheese.
authors.affiliation: Institute of Environmental Science and Engineering, National University of Sciences and Technology, Rawalpindi, Pakistan.
authors.forename: M
authors.initials: M
authors.lastname: Ali Awan
authors.affiliation: Centre for Instrumentation and Analytical Science, School of Chemical Engineering and Analytical Science, The University of Manchester, Manchester, UK.
authors.forename: I
authors.initials: I
authors.lastname: Fleet
authors.affiliation: Department of Chemistry, Loughborough University, Leicestershire LE11 3TU, UK. Electronic address: C.L.P.Thomas@lboro.ac.uk.
authors.forename: C L
authors.initials: CL
authors.lastname: Paul Thomas
keywords: Biogenic amines; Cadaverine; Gas-phase derivatisation; On-fibre derivatisation; Putrescine; Trifluoroacetylacetone