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

Analytica chimica acta (2008-02-12)
Yiannis C Fiamegos, Constantine D Stalikas
ABSTRACT

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.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Butyraldehyde, ≥96.0%
Sigma-Aldrich
Butyraldehyde, purified by redistillation, ≥99.5%
Sigma-Aldrich
Butyraldehyde, ≥99.0%, dry
Sigma-Aldrich
Butyraldehyde, natural, FG

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