Simultaneous extraction and cleanup method based on pressurized solvent extraction for multiresidue analysis of...

The development of a multiresidue method based on pressurized solvent extraction (PSE) to determine a large number of pesticides (mostly pyrethroids and organochlorines) in cattle feed is described. As far as we know, this is the first work dedicated to the PSE of many of the target pesticides from animal feed. A mixed level fraction design was performed to investigate the influence of several operational variables on the PSE procedure; integrated cleanup strategies were also assessed allowing the direct chromatographic analysis of the extracts. Method accuracy was evaluated by the analysis of a certified reference material (BCR-115) and different fortified cattle feed samples. Most analytes were recovered in the range of 70-110%, with relative standard deviations generally lower than 15%. Limits of detection (LODs) were below the maximum residue levels (MRLs) set by the European Union for animal feed and main crops used in the preparation of feedingstuffs. The applicability of the proposed method was demonstrated by the analysis of real cattle feed samples collected from 23 dairy farms located in Galicia (NW Spain).