Gas chromatographic determination of carbonyl compounds in biological and oil samples by headspace single-drop microextraction with in-drop derivatisation

摘要

A suitable method for the gas chromatographic determination of 10 characteristic car-bonyls 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 0.003 mu gmL~(-1)for the aqueous biological samples and from 0.06 to 0.20 mu g mL~(-1)for the oil samples.The limits of quantification were in the range of 0.003-0.010 mu g mL~(-1)and 0.020-0.059 mu g mL~(-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.