Multi-residue method for the determination of organofluorine pesticides in fish tissue by liquid chromatography triple quadrupole tandem mass spectrometry
•New LC–MS/MS method for detection of 6 organofluorine pesticides in fish products.•New in SPE: NH2 SPE reduces coextraction interference.•The methanol pH 5 buffer shows better separation than other mobile phase.•Method application for fish, shrimp and eel.•Method is fast with high recoveries and go...
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Veröffentlicht in: | Food chemistry 2016-09, Vol.207, p.195-204 |
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Format: | Artikel |
Sprache: | eng |
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Zusammenfassung: | •New LC–MS/MS method for detection of 6 organofluorine pesticides in fish products.•New in SPE: NH2 SPE reduces coextraction interference.•The methanol pH 5 buffer shows better separation than other mobile phase.•Method application for fish, shrimp and eel.•Method is fast with high recoveries and good precision.
A multiresidue method for the determination of organofluorine pesticides in fish tissue samples was developed and optimized. This method is based on a cleanup step of the extracted samples with acetonitrile, and carried out by solid phase extraction (SPE) with aminopropyl (NH2) cartridge, before the identification and quantification of the residues by liquid chromatography triple quadrupole tandem mass spectrometry (LC–MS/MS). The performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), for each pesticide were determined. The proposed method allowed high recoveries (80.4–99.2%) of spiked extracted fat samples at 0.5–10ngg−1, and very low LODs (between 0.10 and 0.15ngg−1) and LOQs (between 0.3 and 0.5ngg−1) determined in the fish samples. The practicality and high sensitivity of this method have been demonstrated in the determination of residues of OFPs in carp fish fed in water containing 10ngmL−1 OFPs. |
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ISSN: | 0308-8146 1873-7072 |
DOI: | 10.1016/j.foodchem.2016.02.098 |