Study of vortex-assisted MSPD and LC-MS/MS using alternative solid supports for pharmaceutical extraction from marketed fish
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.
KeywordsPharmaceuticals Fish MSPD Alternative solid supports LC-MS/MS
The authors acknowledge the financial support and fellowships granted by the Brazilian agencies CAPES, FINEP, and FURG. Part of this study was funded by CNPq/CAPES (process number 552318/2011-6), FAPERGS (process number 810-25.51/13-3), FAPERGS (process number 831-25.51/13-0), and CAPES/PNPD (process number 23038.028239/2009-69). E.G. Primel received a productivity research fellowship from the Brazilian Agency CNPq (DT 310517/2012-5).
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