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Determination of polycyclic aromatic hydrocarbons in soy isoflavone nutraceutical products by gas chromatography coupled to triple quadrupole tandem mass spectrometry
Author(s) -
RuizDelgado Ana,
MartínezDomínguez Gerardo,
RomeroGonzález Roberto,
LópezRuiz Rosalía,
Frenich Antonia Garrido
Publication year - 2016
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201500992
Subject(s) - chemistry , chromatography , extraction (chemistry) , gas chromatography/tandem mass spectrometry , mass spectrometry , triple quadrupole mass spectrometer , tandem mass spectrometry , gas chromatography , detection limit , gas chromatography–mass spectrometry , solid phase extraction , matrix (chemical analysis) , hexane , selected reaction monitoring
Thirteen polycyclic aromatic hydrocarbons have been determined in soy‐based nutraceutical products. First, an optimization of extraction procedure was performed, and a solid–liquid extraction assisted by sonication and a dilute and shoot procedure were compared, selecting the dilute and shoot approach for the extraction of target compounds, utilizing a mixture of acetone/ n ‐hexane (1:1 v/v) as extractant solvent. After this, a clean‐up step was needed bearing in mind the complexity of these matrices. Dispersive solid‐phase extraction, using a mixture of C 18 and Zr‐Sep+ (25 mg/mL each) was used. The separation was achieved by gas chromatography and detection with triple quadrupole tandem mass spectrometry. For quantification purposes, matrix‐matched calibration was used. The validation was applied at three concentration levels (20, 100 and 250 μg/kg), obtaining recoveries between 70 and 120% and precision values equal to or lower than 23%. Limits of detection and quantification were below 8 and 20 μg/kg, respectively. The method was applied in 11 samples, detecting five polycyclic aromatic hydrocarbons at concentrations ranging from 4.1 to 18.5 μg/kg.