Rapid Determination of Six Zeranols in Biscuits by Dispersive Solid-phase Extraction Coupled with High Performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A simple and rapid analytical method was established for the determination of six zeranols (α-zearalanol, β-zearalanol, α-zearalenol, β-zearalenol, zearalanone, and zearalenone) in biscuits by dispersive solid phase extraction (d-SPE) coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). After the addition of the isotopic internal standard, the sample was dispersed in water, and zeranols were extracted using a solvent mixture of acetonitrile/formic acid (99:1). Subsequently, the sample was mixed with sorbents PSA, C18, and MgSO4 to conduct d-SPE. The solution was concentrated under a nitrogen stream and reconstituted in a 30% acetonitrile (v/v) solution. After being defatted with n-hexane, the sample was separated and analyzed by HPLC-MS/MS. Negative electrospray ionization was used on a quadrupole mass spectrometer operating under multiple reaction monitoring (MRM) mode. The quantitation was carried out using the internal standard method. The calibration curves of the zeranols were linear in the range 0.20-50.0 μg/L with correlation coefficients higher than 0.996. The limits of detection (LODs) and the limits of qualification (LOQs) of the method varied from 0.03 to 0.11 μg/kg and from 0.11 to 0.31 μg/kg, respectively. The mean recoveries of the zeranols ranged from 70.9% to 107.1%, with intraday precisions (n = 6) and interday precisions (n = 5) less than 12%. This method provides good purification and accurate quantification, and is sensitive, rapid, and suitable for the identification and quantification of the six zeranols in biscuits.
