Abstract
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 conditions 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 stationary phases were evaluated and Hypercarb (porous graphitic 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.
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Acknowledgments
The authors gratefully acknowledge the Spanish Ministry of Economy and Competitiveness (MINECO) and FEDER (project ref. CTQ2012-34304). RDA acknowledges the National Council for Scientific and Technological Development (CNPq, Proc. 249629/2013-5) from Brazil through Science without Borders Program (CsF) for financial support.
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Domingos Alves, R., Romero-González, R., López-Ruiz, R. et al. Fast determination of four polar contaminants in soy nutraceutical products by liquid chromatography coupled to tandem mass spectrometry. Anal Bioanal Chem 408, 8089–8098 (2016). https://doi.org/10.1007/s00216-016-9912-2
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DOI: https://doi.org/10.1007/s00216-016-9912-2