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  • Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish.

Analytical and bioanalytical chemistry (2015-04-26)
Gabriel I Hertzog, Karina L Soares, Sergiane S Caldas, Ednei G Primel
ZUSAMMENFASSUNG

A procedure based on vortex-assisted matrix solid-phase dispersion (MSPD) for the extraction of 15 pharmaceuticals from fish samples with determination by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was validated. Florisil, C18, diatomaceous earth, chitin, and chitosan were evaluated as solid supports. Best results were obtained with 0.5 g of diatomaceous earth, 0.5 g of sodium sulfate, and 5 mL of methanol. Analytical recoveries ranged from 58 to 128 % with relative standard deviation (RSD) lower than 15 %. Limit of quantification (LOQ) values for the 15 compounds ranged from 5 to 1000 ng g(-1). The method under investigation has shown to be a simple and fast extraction tool with minimum instrumentation and low amount of reagent, resulting in method low cost. Besides, alternative materials, such as chitin and chitosan, which were applied to the dispersion step for the first time, were found to be interesting alternatives.

MATERIALIEN
Produktnummer
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Produktbeschreibung

Sigma-Aldrich
Methanol, anhydrous, 99.8%
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Essigsäure, suitable for luminescence, BioUltra, ≥99.5% (GC)
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5α-Androstan-17β-ol-3-on, ≥97.5%
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Ameisensäure, ≥95%, FCC, FG
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Essigsäure, ≥99.5%, FCC, FG
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Essigsäure, natural, ≥99.5%, FG
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5α-Androstan-17β-ol-3-on, purum, ≥99.0% (TLC)
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Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Methanol -Lösung, suitable for NMR (reference standard), 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
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Essigsäure-12C2, 99.9 atom % 12C