Headspace Solid Phase Microextraction (HS-SPME) coupled to Gas Chromatography-Mass Spectrometry (GC/MS) for the Analysis of Multi-Class Pesticides

Abstract

The development of a method based on headspace solid phase microextraction (HS-SPME) technique, for the simultaneous determination of 7 multiclass and multiresidue pesticides (fenobucarb, diazinon, chlorothalonil, thiobencarb,chlorpyrifos,endosulfan I and endosulfan II) in two species of apple, using gas chromatography-mass spectrometry is discussed. The different parameters affecting the SPME technique were evaluated. The extraction capacity of three fiber coatings; polydimethylsiloxane (100µm PDMS), polyacrylate (65µm PA), and polydimethylsiloxane-divinylbenzene (85µm PDMS-DVB), were studied and compared. Validation of the method using two apple species spiked with standard solution yield better linear range, accuracy, precision, detection and quantification limits. The linearity was between 5 to 500 µg.kg^–1 with good correlation coefficients (R) greater than 0.989. The average recoveries for all pesticides investigated were between 89–100% in green apple and 94–103% in red apple with RSD ranging from 0.67–3.32% and 1.00 - 2.69 % respectively. The LOQs were between 6.71 and 14.56 µg.kg^–1 and LODs ranged from 2.23 to 11.11 µg.kg^-1.