Gas chromatographic determination of carbonyl compounds in biological and oil samples by headspace single-drop microextraction with in-drop derivatisation.
A suitable method for the gas chromatographic determination of 10 characteristic carbonyls in biological and oil samples based on the in-drop formation of hydrazones by using 2,4,6-trichlorophenylhydrazine (TCPH), has been developed. The derivatisation-extraction procedure was optimized separately for aqueous and oil samples with respect to the appropriate organic drop solvent, drop volume, in-drop TCPH concentration, sample stirring rate, temperature during single-drop microextraction (SDME), reaction time and headspace-to-sample volume ratio. The optimization showed differentiation of optimum values between the studied matrices. The limits of detection were found to range from 0.001 to 0.003microgmL(-1) for the aqueous biological samples and from 0.06 to 0.20microgmL(-1) for the oil samples. The limits of quantification were in the range of 0.003-0.010microgmL(-1) and 0.020-0.059microgmL(-1) for aqueous and oil samples, respectively. The overall relative standard deviations of the within-day repeatability and between-day reproducibility were <4.4% and <8.2% for the aqueous biological samples and <3.9% and <7.4% for the oxidized oil samples.
Fiamegos
Yiannis C
YC
Laboratory of Analytical Chemistry, Chemistry Department, University of Ioannina, 45110 Ioannina, Greece. yfiameg@cc.uoi.gr
Stalikas
Constantine D
CD
D000447:Aldehydes / Q000737:chemistry; D002255:Carbonic Acid / Q000032:analysis* / Q000737:chemistry*; D002849:Chromatography, Gas / Q000379:methods*; D013058:Mass Spectrometry; D015394:Molecular Structure; D009821:Oils / Q000032:analysis* / Q000737:chemistry
D000447:Aldehydes; D009821:Oils; D002255:Carbonic Acid; C018475:butyraldehyde