Solid-Phase Extraction-Based Ultra-Sensitive Detection of Four Lipophilic Marine Biotoxins in Bivalves by High-Performance Liquid Chromatography–Tandem Mass Spectrometry
A solid-phase extraction (SPE) method for ultra-sensitive determination of four lipophilic marine biotoxins in bivalve samples by coupling high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS-MS) was developed. Azaspiracid-2 (AZA2), pectenotoxins-2, spirolide (SPX) and gymnodimin...
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Veröffentlicht in: | Journal of chromatographic science 2015-02, Vol.53 (2), p.373-379 |
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Sprache: | eng |
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Zusammenfassung: | A solid-phase extraction (SPE) method for ultra-sensitive determination of four lipophilic marine biotoxins in bivalve samples by coupling high-performance liquid chromatography–tandem mass spectrometry (HPLC–MS-MS) was developed. Azaspiracid-2 (AZA2), pectenotoxins-2, spirolide (SPX) and gymnodimine were simultaneously determined by HPLC–MS-MS in a positive multiple reaction monitoring mode. Separation was achieved on a reversed-phase C18 column with an acetonitrile–water gradient containing formic acid. During the analysis, solvent effects on the analytes were eliminated by using 1 : 1 water–methanol as dissolving solvent instead of pure methanol. Matrix effects in post-SPE extract and crude extract were seriously evaluated. Increased matrix effects in post-SPE extract countervailed the concentration purpose to some extent. The limits of detection of the SPE–HPLC–MS-MS method were determined to be in the range of 0.013–0.085 µg kg−1, and the linear range of the method was in the range of 0.128–55.2 ng mL−1 for the detected toxins. The proposed method was validated in terms of linearity (matrix-matched standard curves), precision, recovery, repeatability and limits of quantification. The recoveries of fortified samples at three different concentration levels were satisfactory, and the intra- and interday precisions were |
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ISSN: | 0021-9665 1945-239X |
DOI: | 10.1093/chromsci/bmu054 |