Rapid HPLC Determination of Crotonaldehyde in Mainstream of Cigarette Smoke

Crotonaldehyde in mainstream of cigarette smoke was trapped and derivatized simultaneously on a piece of cambridge filter (on which 2 mL of 0.075 mol·L-1 2,4-dinitrophenylhydrazine-acetonitrile solution,or abbreviated as DNPH solution,were dropped homogeneously and dried in a desiccator,ready for use) by smoking 2 cigarettes with a smoking machine. A mixed solution of pyridine and acetonitrile (2+98) was used to extract the derivatized product of 2,4-dinitrophenylhydrazone from the filter into the extraction solvent. An aliquot of the extract was used for HPLC analysis. Rapid separation of crotonaldehyde in the extract was attained within 5.5 min by using ZORBAX Stable Bound C18 (2.1 mm×50 mm,1.8 μm) column and by using mixtures of acetonitrile (A) and water (B) of different ratios for gradient elution. DAD at the wavelength of 365 nm was adopted in the determination. Detection limit (3S/N) found for the method was 8.0 μg·L-1. Tests for recovery were made at 3 concentration levels (0.05,0.10,0.2 mg),and results of recovery found were in the range of 96%-101%. Repeatability and reproducibility were also tested and the values of RSD′s (n=7) founs were 2.2% and 2.9% respectively.