Multiclass determination of pesticides and priority organic pollutants in fruit-based soft drinks by headspace solid-phase microextraction/gas chromatographytandem mass spectrometry

Abstract

In this work, a simple, environmentally friendly, rapid and reliable GC-MS/MS method has been developed for the determination of 45 organic contaminants (32 pesticides and 13 PAHs) in fruit-based soft-drinks. The proposed method consists of a solventless sample treatment procedure based on headspace solid-phase microextraction using a fiber of polyacrylate (PA), followed by identification and quantitation of the target pesticides by gas chromatography-tandem mass spectrometry (GC-MS/MS) using a triple quadrupole analyzer in the multiple reaction monitoring (MRM) acquisition mode. Several parameters of the automated extraction were studied including the incubation time, temperature, sample volume and type of SPME fibers. The identification and confirmation of the compounds were based on the retention time matching along with the presence (and relative abundances ratio) of three characteristic MRM transitions (except for PAHs, in which two transitions were used). Fruit-based soft drinks spiked at 100 ng L⁻¹ yielded average recoveries in the range 75–113% with RSD (%) below 15% (n = 8). The obtained limits of detection varied in the range 0.1–180 ng L⁻¹. The proposed method was successfully applied to the analysis of 26 market purchased fruit-based soft drink samples collected mainly in Spain, but also in some other countries, showing its potential applicability and revealing the presence of some of the target species in the ng L⁻¹ range (from 1.5 to 320.8 ng L⁻¹).