Artigo
Fast determination of four polar contaminants in soy nutraceutical products by liquid chromatography coupled to tandem mass spectrometry
Autor
Romero-González, Roberto
Alves, Renata Domingos
López-Ruiz, Rosalía
Jiménez-Medina, M. L.
Frenich, Antonia Garrido
Institución
Resumen
An analytical method based on a modified QuPPe (quick polar pesticide) extraction procedure coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS)
was evaluated for the determination of four polar compounds
(chlorate, fosetyl-Al, maleic hydrazide, and perchlorate) in
nutraceutical products obtained from soy. Experimental con-
ditions including extraction such as solvent, acidification,
time, and clean-up sorbents were varied. Acidified acetonitrile
(1 % formic acid, v/v) was used as extraction solvent instead of
methanol (conventional QuPPe), which provides a doughy
mixture which cannot be injected into the LC. Clean-up or
derivatization steps were avoided. For analysis, several sta-
tionary phases were evaluated and Hypercarb (porous graphit-
ic carbon) provided the best results. The optimized method
was validated and recoveries ranged between 46 and 119 %,
and correction factors can be used for quantification purposes
bearing in mind that inter-day precision was equal to or lower
than 17 %. Limits of quantification (LOQs) ranged from 4 to
100 μg kg^−1. Soy-based nutraceutical products were analyzed
and chlorate was detected in five samples at concentrations
between 63 and 1642 μg kg^−1.