Determination of 15 Aldehyde and Ketone Carbonyl Compounds in Environmental Solid Matrix by Liquid Chromatography with 2,4-Dinitrophenylhydrazine Derivatization and Solid Phase Extraction

Acetic acid-sodium acetate buffer solution (pH 5.0, 200 mL) was added to 10.000 g of the sample, and the mixture was oscillated for 18 h and then centrifuged. The extract of 100 mL was taken and citric acid-sodium citrate buffer solution (pH 3.0, 4 mL) and 3.00 g·L^-1 of 2,4-dinitrophenylhydrazine (DNPH) derivatized solution (acetonitrile as solvent, 6 mL) were added, and then the mixture was derivatized ultrasonically at room temperature for 30 min. The derivatives were further extracted by C₁₈ solid phase extraction column, eluted with acetonitrile, and the eluant was diluted to 10 mL with acetonitrile. The 15 aldehyde and ketone carbonyl compounds were determined by liquid chromatography with diode array detector. Linear relationships between values of peak area and mass concentration of 15 aldehyde and ketone carbonyl compounds were found in the same range of 30.0-1.50×10³μg·L^-1, with detection limits ranging from 0.016 to 0.045 mg·kg^-1. Tests for recovery were made by standard addition method, giving results in the range of 39.6%-43.3% for actone and 69.0%-99.4% for the other aldehydes and ketones, and RSDs (n=6) ranged from 5.7% to 18%.