Occurrence of Selected Known or Suspected Endocrine-Disrupting Pesticides in Portuguese Surface Waters Using SPME-GC-IT/MS

Abstract

A multiresidue analytical methodology based on a solid-phase microextraction (SPME), followed by gas chromatography-ion trap mass spectrometry (GC–IT/MS), has been developed for trace analysis of 20 known or suspected endocrine-disrupting pesticides. The SPME conditions are optimized considering several key parameters to obtain the maximum sensitivity. After the optimization, the method validation is performed, and the limits of detection (ranged from 2–150 ng/L) and the coefficient of determination (above 0.990) of studied compounds are determined for all the analytes. A robust sampling of twenty sampling points of surface water samples from the north and center of Portugal is performed, and the validated methodology is applied. In total, 20 compounds from four chemical families (13 organochlorine, 1 organophosphorus, 2 dicarboximide, and 4 pyrethroids) are studied, and the pesticides most frequently detected are eight organochlorine pesticides (α-, β-HCHs, lindane, HCB, o,p′-DDT, p,p′-DDE, p,p′-DDD, α-endosulfan), cypermethrin, and vinclozolin.

Improving knowledge on genotoxicity dynamics in somatic and germ cells of crayfish (Procambarus clarkii)

“…Adult specimens of Procambarus clarkii (commonly known as red swamp crayfish of Louisiana), from both genders, with an average length of 11.00 ± 0.89 cm, were collected at Rio Minho (Vila Nova de Cerveira, NW Portugal), a low impacted area concerning the presence of pesticides, as well as inorganic and organic contaminants (Castro‐Valencia et al, 2019; Rocha et al, 2021; Vera et al, 2021). In the laboratory, crayfish were kept in aquaria (60 L), separated by gender, during 2 weeks for acclimation, with the following water conditions: constant temperature (19 ± 1°C), freshwater (salinity 0), with aeration (dissolved oxygen 8.1 ± 0.5 mg L −1 ), UV disinfection, weekly control of nitrites (0.06 ± 0.03 mg L −1 ), nitrates (25 ± 6.0 mg L −1 ), and ammonia (<0.1 mg L −1 ) and pH (7.3 ± 0.2).…”

Blueberry Pruning Wastes: From an Undervalued Agricultural Residue to a Safe and Valuable Source of Antioxidant Compounds for the Food Industry

“…Once the potential of the blueberry canes regarding their phenolic content and antioxidant capacity was determined and demonstrated, a safety assessment of the samples was performed. The presence of environmental contaminants, specifically persistent organic pollutants (POPs) like PCB and BDE, in both food and environmental samples is a pressing concern due to their long-term persistence, bioaccumulation and potential adverse effects on human health and ecosystems [21,36]. Therefore, the goal was to understand if any of these POPs were present in the canes and, most importantly, in the extracts.…”

Green Extraction Techniques as Advanced Sample Preparation Approaches in Biological, Food, and Environmental Matrices: A Review

“…MEPS seems to be tailored for these requirements and has been applied in the analysis of benzene, phenol and their derivates [165], diazinon [166], La 3+ and Tb 3+ [167], organophosphorus pesticides [168] in water samples, fipronil and fluazuron residues in wastewater [169], and PAHs in the most diverse samples (see Table S3), including Antarctic snow [170], and in the detection of phthalates in tap and river water [171]. SPME is eventually one of the most used sample extraction procedures and has been applied for the detection of different pesticides in water [172] (additional examples in Table S3), microplastic in coral reef invertebrates [173], PAHs in rainwater [174], and volatile organic compounds (VOCs) in wastewater [69]. Molecularly imprinted polymers (MIPs) have also been employed in the extraction of polychlorinated aromatic compounds from environmental samples.…”