Ochratoxin A (OTA) is a mycotoxin produced by several species of Aspergillus and Penicillium and commonly detected in a wide range of foodstuffs. The purpose of this work was to monitor the presence of OTA in cheeses and pork meat products. A simple and accurate “dilute and shoot” method with no need of immunoaffinity column and isotopic labeled internal standard, by liquid chromatography–tandem mass spectrometry, was validated in accordance with the criteria set out in Commission Regulation (EC) No. 401/2006. The method showed good linearity in solvent and in matrix ( R ² ≥ 0.995), limit of detection was 0.2 µg/kg for cheese and 0.3 µg/kg for pork meat products, limit of quantification was fixed at 1 µg/kg, and recovery was estimated at two different concentration levels (1 and 5 µg/kg) and ranged from 75% to 101%. The interday and intraday laboratory precisions were lower than 7%. The matrix effect, the recovery of the extraction process, and the overall process efficiency were evaluated. No significant ME was observed in the two matrices considered. This method was applied to the analysis of 75 samples, coming from official controls implemented by the Lazio Region (Central Italy). In one sample of dry‐cured ham, the concentration found (69.3 µg/kg) was well above the guidance value recommended by the Italian Ministry of Health (1 µg/kg). These data together with the detection of OTA in three grated cheeses suggest the importance of monitoring these products. Considering the high dietary intake of these matrices, especially among vulnerable populations, further research should be devoted to estimate exposure and risk assessment for OTA.

The presence and accumulation of marine biotoxins, including paralytic shellfish toxins (PSTs) and tetrodotoxin (TTX) analogues, in marine organisms poses a significant food safety concern. This study describes the validation of a quantitative confirmatory HILIC–LC–MS/MS method for the simultaneous determination of a broad panel of marine toxins in four matrices: mussels, clams, sea snails, and sea urchins. The method covered 17 target compounds, including TTX analogues (TTX, 4-epiTTX, and 4.9-anhTTX), saxitoxin and analogues (STX, dcSTX, NEO, and dcNEO), gonyautoxins (GTX 1–4, GTX 2–3, GTX 5, GTX 6, and dcGTX 2–3), and sulfocarbamoyl toxins C1–C2. Particular attention was devoted to the evaluation of matrix effects (ME), a critical factor affecting LC–MS/MS quantification. The method was validated according to SANTE/11312/2021 guidelines, showing satisfactory selectivity, precision (RSD ≤ 20%), and accuracy (recoveries within 70–120%). Significant matrix-dependent signal suppression and enhancement were observed among the investigated species. Matrix-matched calibration enabled reliable quantification in mussels, clams, and sea snails, whereas sea urchin samples showed greater analytical complexity. The validated method provides a robust approach for the determination of PSTs and TTX analogues in different marine organisms and supports its application in official monitoring programs.