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Study of the performance of three LC-MS/MS platforms for analysis of perfluorinated compounds

Llorca, Marta, Farré, Marinella, Picó, Yolanda, Barceló, Damià
Analytical and bioanalytical chemistry 2010 v.398 no.3 pp. 1145-1159
Xiphias gladius, acids, anchovies, liquid chromatography, markets, monitoring, mussels, oysters, perfluorocarbons, shellfish, solid phase extraction, surveys, tandem mass spectrometry, tuna, Spain
The analytical suitabilities of three different liquid chromatography-tandem mass spectrometry (LC-MS/MS) systems, (1) triple quadrupole (QqQ), (2) conventional 3D ion trap (IT), and (3) quadrupole-linear IT (QqLIT), to determine trace levels of perfluorinated compounds (PFCs) in fish and shellfish were compared. Sample preparation was performed using alkaline extraction and solid-phase-extraction cleanup. This evaluation was focused on both quantitative (sensitivity, precision, and accuracy) and qualitative (identification capabilities) aspects. In the three instruments, the former facet was evaluated using selected reaction monitoring (SRM), which is the standard mode for quantitative LC-MS/MS analysis. Accuracy was similar in the three systems, with recoveries always over 70 %. Precision was better for the QqLIT and QqQ systems (7-15%) than for the IT system (10-17%). The QqLIT (working in SRM mode) and QqQ systems offered a linear dynamic range of at least 3 orders of magnitude, whereas that of the IT system was 2 orders of magnitude. The QqLIT system achieved at least 20-fold higher sensitivity than the QqQ system, and this was at least tenfold higher sensitivity than for the IT system. In the IT system, identification was based on sensitive full mass range acquisition and MS n fragmentation and in the QqLIT system, it was based on the use of an information-dependent-acquisition scan function, which allows the combination of an SRM or MS full scan acting as the survey scan and an enhanced product ion scan followed by MS³ as the dependent scan in the same analysis. Three instruments were applied to monitor the content in fish and shellfish (anchovies, swordfish, tuna, mussels, and oysters) obtained from Valencia and Barcelona markets (Spain). The eight target PFCs were detected at mean concentrations in the range from 10 ng kg⁻¹ (perfluoro-7-methyloctanoic acid and perfluoro-1-decanesulfonate) to 4,200 ng kg⁻¹ (perfluoropentanoic acid). Furthermore, perfluoroheptanoic and perfluoroundecanoic acids (not covered as target analytes) were identified in some samples. [graphic removed]