Assessing pharmaceuticals in the green seaweed Ulva lactuca through a multi-residue UHPLC-ToF-MS strategy.

Seaweeds have become an important asset in several sectors, including the food and feed industries, cosmetics, and pharmaceuticals, among others. Whether harvested or reared, interest in algae has been growing worldwide due to the resources they offer, including proteins, vitamins, minerals, carbohydrates, essential fatty acids, and dietary fiber, as well as sources of biologically active compounds. However, given their morphology and physiology, as well as their harvest and cultivation environments, algae are prone to the presence of hazards, including pharmaceuticals taken up from the water. Thus, to ensure human and animal safety as well as environmental health, monitoring is essential. Therefore, this work describes the development and validation of a sensitive screening and confirmatory analytical method based on ultra-high-performance liquid chromatography coupled with time-of-flight mass spectrometry (UHPLC-ToF-MS). This multi-residue method enables the determination of 62 pharmaceuticals distributed between 8 therapeutic classes and was fully validated according to Commission Implementing Regulation (EU) 2021/808.

Development and validation of a multi-residue and multi-class screening method of 44 antibiotics in salmon (Salmo salar) using ultra-high-performance liquid chromatography/time-of-flight mass spectrometry: Application to farmed salmon.

A fast and sensitive multi-residue and multiclass screening method for the simultaneous determination of 44 antimicrobials in salmon muscle, using ultra- high-performance liquid chromatography/time-of-flight mass spectrometry (UHPLC-TOF/MS), was develop and validated. Two different procedures for the extraction step were tested, and an extraction with acetonitrile, ethylenediaminetetra acetic acid (EDTA) and n-hexane proved to be the best alternative. The method was validated, in accordance with Decision 2002/657/EC, using a qualitative approach at the CCß level. The detection of the analytes was accomplished by retention time and accurate mass, whose maximum error should not exceed 5 ppm. All the compounds were successfully detected and identified at concentration levels corresponding to ½ maximum residue limit (MRL). The screening method was applied to 39 store bought samples of farmed salmon purchased in Portugal, originating from Norway and Denmark, and no antibiotic residues were detected.

Oxytetracycline accumulation in the macroalgae Ulva: Potential risks for IMTA systems.

Oxytetracycline (OTC) is one of the most used antibiotics in aquaculture. With the development of Integrated Multitrophic Aquaculture (IMTA) systems in order to mitigate some aquacultures' adverse effects, attention needs to be shifted to other co-cultured species that can also accumulate such pharmaceuticals and pose a risk to human consumption. Therefore, the present work evaluated the exposure of the seaweed Ulva to OTC at two realistic concentrations (0.040 and 0.120 mg L-1). Oxytetracycline degradation rates in seawater were dependent on the initial concentration but were not influenced by the presence of Ulva. The macroalgae presented good assimilation rates of OTC, with internal concentrations reaching 40.9934 ng g-1 WW for the lowest concentration tested and 108.6787 ng g-1 WW for the highest, with a steep decrease after 48 and 24 h, respectively. Nonetheless, concentrations were still half of the Maximum Residue Limit set for fish (100 µg kg-1) 48 h after C2 treatment. The highest dosage tested stimulated growth 96 h after the beginning of the trial, although some signs of decay could also be found in Ulva's fronds.