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Coupled SFE/SFC/GC for the trace analysis of pesticide residues in fatty food samples

1994; Wiley; Volume: 17; Issue: 8 Linguagem: Inglês

10.1002/jhrc.1240170803

1521-4168

Ki‐Souk Nam, Jerry W. King,

Mass Spectrometry Techniques and Applications

Abstract An on‐line SFE‐chromatographic system, where SFE has been coupled with SFC and GC, was developed and utilized for trace analyses of organochlorine and organophosphorus pesticide residues from gram‐sized complex sample matrices, such as chicken fat, ground beef, and lard. The SFE process and chromatographic techniques were instrumentally integrated for efficient and automated on‐line analysis, having minimal sample handling between the sample preparation and separation steps. A cleanup step, incorporating packed column SFC, allowed the fractionation of relatively small‐sized, non‐polar pesticides from the co‐extracted fatty materials. This permitted final high‐resolution separation of analytes on a capillary GC column. Detection of pesticides was accomplished using selective electron‐capture and nitrogen‐phosphorus detectors. Pesticide concentrations determined with the on‐line system were accurate and reproducible, for fatty samples containing both fortified and incurred pesticides. This method, utilizing supercritical carbon dioxide, was considerably faster and less laborious than the conventional analytical procedures based on liquid extraction.