The aim of this research was to develop and validate a headspace-solid phase micro-extraction–gas chromatography–mass spectrometry (HS-SPME–GC–MS) method for the determination of volatile emerging contaminants in fruit. The method showed good precision (RSD ≤ 14%) and satisfactory recoveries (99.1–101.7%) and LOD and LOQ values ranging between 0.011–0.033 μg kg−1 and 0.037–0.098 μg kg−1, respectively. The method was applied to investigate the content of volatile emerging contaminants in two varieties of melon fruit (Cucumis melo L.) cultivated adjoining high-risk areas. Glycol ethers, BHT, BHA and BTEX (benzene, toluene, ethylbenzene and xylene) were determined in melon fruit pulps for the first time, with different sensitivities depending on sample and variety. Although the amount of the volatile contaminants in the melon samples were in the order of µg kg−1, the safety of vegetable crops cultivated near risk areas should be more widely considered. The results showed that this accurate and reproducible method can be useful for routine safety control of fruits and vegetables.
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