Determination of chlorinated pesticide residues in foods part 3 simultaneous analysis of chlorinated pesticide and phthalate residues by using silver nitrate coated florisil column chromatography for cleanup of various samples

Suzuki, T.; Ishikawa, K.; Sato, N.; Sakai K I.

Journal - Association of Official Analytical Chemists 62(3): 689-694


ISSN/ISBN: 0004-5756
Accession: 005122090

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A simplified method suitable for simultaneous analysis of chlorinated pesticide and phthalate ester residues in various foods was developed. Chemical residues were quantitatively extracted from fatty and vegetable samples with acetonitrile as follows: Chemical standard in 0.5 ml ethanol solution was added to 10 g homogenized sample. After 3 h, pork and beef were extracted 3 times with 20 ml portions of acetonitrile. The acetonitrile layers were diluted with water and extracted with n-hexane. Rice samples were combined with 10 ml water, 5 ml acetonitrile and 1 ml ethanol and extracted 3 times with 20 ml portions of n-hexane. The n-hexane concentrate from each sample was submitted to AgNO3-coated Florisil column chromatography. The AgNO3 coating adequately adsorbed interfering coextractives. Extracts of fish and vegetable samples were separated into 2 fractions by the above column chromatography. Supplemental cleanup procedures were also developed to accurately determine phthalate esters eluted in the 2nd fraction. Satisfactory gas chromatograms were obtained for most samples.