In this study, a robust analytical method based on high performance liquid chromatography coupled to inductively coupled plasma - tandem mass spectrometry (HPLC-ICP-MS/MS) was developed and validated for the simultaneous determination of ethylene thiourea (ETU) and propylene thiourea (PTU) in fruits and sulfur-rich vegetables such as plums, apricots, cherries broccoli and Brussels sprouts. Sample preparation was based on a Quick Polar Pesticides (QuPPe) extraction using methanol, followed by an anion-exchange solid-phase extraction (SPE) cleanup to efficiently remove sulfur-containing matrix interferences released during homogenization. Method validation was carried out according to the accuracy profile approach (NF V03-110) across five levels (10-400 μg L?1) for each of the matrices mentioned above. The method showed satisfactory trueness, repeatability, and intermediate precision for both analytes, with limits of quantification of 10 μg L?1 for both ETU and PTU in all matrices. The proposed method demonstrates strong robustness and versatility for the determination of ETU and PTU in challenging sulfur-rich plant matrices and provides a promising ICP-MS/MS-based alternative for the quantification of sulfur-containing organic contaminants in food.