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  • Simultaneous determination of perfluorinated compounds and their potential precursors in mussel tissue and fish muscle tissue and liver samples by liquid chromatography-electrospray-tandem mass spectrometry.

Simultaneous determination of perfluorinated compounds and their potential precursors in mussel tissue and fish muscle tissue and liver samples by liquid chromatography-electrospray-tandem mass spectrometry.

Journal of chromatography. A (2015-02-25)
I Zabaleta, E Bizkarguenaga, A Prieto, M Ortiz-Zarragoitia, L A Fernández, O Zuloaga
ABSTRACT

An analytical method for the simultaneous determination in fish liver and muscle tissue and mussel samples of 14 perfluorinated compounds (PFCs), including three perfluoroalkylsulfonates (PFSAs), seven perfluorocarboxylic acids (PFCAs), three perfluorophosphonic acids (PFPAs) and perfluorooctanesulfonamide (PFOSA), and 10 potential precursors, including four polyfluoroalkyl phosphates (PAPs), four fluorotelomer saturated acids (FTCAs) and two fluorotelomer unsaturated acids (FTUCAs), was developed in the present work. Different clean-up strategies by means of solid-phase extraction (SPE) using a mix-mode weak anion exchanger (WAX), reverse phase Envi-Carb or a combination of them was optimized and evaluated for the clean-up of focused ultrasonic solid-liquid (FUSLE) extracts before the analysis by liquid chromatography-triple quadrupole tandem mass spectrometry (LC-MS/MS). Mix-mode WAX coupled in-line to Envi-Carb was finally selected since it rendered the cleanest extracts and minimum matrix effect. The FUSLE-SPE-LC-MS/MS methodology was validated in terms of recovery, precision and method detection limits (MDLs). Apparent recovery values in the 65-116%, 59-119% and 67-126% range and MDLs in the 0.1-2.7 ng/g, 0.1-3.8 ng/g and 0.2-3.1ng/g range were obtained for liver, mussel and fish muscle tissue samples, respectively. The method developed was applied to the analysis of grey mullet liver (Chelon labrosus) and mussel (Mytilus galloprovincialis) samples from the Basque Coast (North of Spain) and Yellowfin tuna muscle tissue (Thunnus albacares) samples from the Indian Ocean. To the best of our knowledge this is the first method that describes the simultaneous determination of 14 PFCs and 10 potential precursors in fish liver, fish muscle tissue and mussel samples. Besides, this is the first time that 8:2 monosubstituted polyfluorodecyl phosphate (8:2 monoPAP) and 8:2 disubstituted polyfluorodecyl phosphate (8:2 diPAP) were detected in mussel and tuna samples, respectively.

MATERIALS
Product Number
Brand
Product Description

Supelco
Supel QuE, PSA/ENVI-Carb Tube 2, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/C18/ENVI-Carb Tube, pk of 50, AOAC® 2007.01, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb Tube 1, pk of 50, suitable for EN 15662:2008 per BS, centrifuge tube volume 15 mL , Shaker Compatible
Supelco
Supel QuE, PSA/ENVI-Carb (EN) Cleanup Tube 1, pack of 100, suitable for EN 15662:2008 per BS
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Carbon - Vitreous, rod, 5mm, diameter 3.0mm, glassy carbon
Carbon - Vitreous, tube, 100mm, outside diameter 10mm, inside diameter 3mm, wall thickness 3.5mm, glassy carbon
Carbon - Vitreous, foam, 150x150mm, thickness 3.2mm, bulk density 0.05g/cm3, porosity 96.5%
Carbon - Vitreous, rod, 100mm, diameter 5.0mm, glassy carbon
Carbon - Vitreous, tube, 50mm, outside diameter 10mm, inside diameter 3mm, wall thickness 3.5mm, glassy carbon
Carbon - Vitreous, foil, 50x50mm, thickness 1.0mm, glassy carbon
Carbon - Vitreous, foam, 150x150mm, 0.05g.cmué, porosity 96.5%, 24 pores/cm
Carbon - Vitreous, foil, 100x100mm, thickness 1.0mm, glassy carbon
Carbon - Vitreous, rod, 100mm, diameter 7.0mm, glassy carbon
Carbon - Vitreous, foil, 10x10mm, thickness 4.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 7.0mm, glassy carbon
Carbon - Vitreous, foil, 25x25mm, thickness 4.0mm, glassy carbon
Carbon - Vitreous, rod, 100mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, rod, 50mm, diameter 1.0mm, glassy carbon
Carbon - Vitreous, rod, 200mm, diameter 10mm, glassy carbon
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Acetonitrile, ≥99.8%, for residue analysis, JIS 300
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Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
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Formic acid, JIS special grade, ≥98.0%
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Acetonitrile, ≥99.8%, suitable for HPLC
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Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles
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5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard