Browsing by Subject "Liquid chromatography"

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    Open Access
    Monitoring of hydroxylated polycyclic aromatic hydrocarbons in human tissues: targeted and untargeted approaches using liquid chromatography‐high resolution mass spectrometry
    (Wiley-VCH Verlag , 2023-07-04) León Morán, Lixy Olinda; Pastor Belda, Marta; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Torres Sánchez, Carmen; Viñas López-Pelegrin, Pilar; Química Analítica; Facultades de la UMU::Facultad de Química
    Hydroxylated polycyclic aromatic hydrocarbons are metabolites of persistent organic pollutants which are formed during the bioactivation process of biological matrices and whose toxicity is being studied. The aim of this work was the development of a novel analytical method for the determination of these metabolites in human tissues, known to have bioaccumulated their parent compounds. Samples were treated by salting‐out assisted liquid‐liquid extraction and the extracts were analyzed by ultra‐high performance liquid chromatography coupled to mass spectrometry with a hybrid quadrupole‐time‐of‐flight analyzer. The proposed method achieved limits of detection in the 0.15–9.0 ng/g range for the five target analytes (1‐hydroxynaphthalene, 1‐hydroxypyrene, 2‐hydroxynaphthalene, 7‐hydroxybenzo[a]pyrene, and 9‐hydroxyphenanthrene). The quantification was achieved by matrix‐matched calibration using 2,2´‐biphenol as internal standard. For all compounds, relative standard deviation, calculated for six successive analyses, was below 12.1%, demonstrating good precision for the developed method. None of the target compounds was detected in the 34 studied samples. Moreover, an untargeted approach was applied to study the presence of other metabolites in the samples, as well as their conjugated forms and related compounds. For this objective, a homemade mass spectrometry database covering 81 compounds was created and none of them was detected in the samples.
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    Targeted and untargeted approaches using liquid chromatography with high-resolution mass spectrometry for the determination of lipophilic marine biotoxins in seawater and mussel samples
    (Elsevier, 2025-09-12) Pastor Belda, Marta; Arroyo Manzanares, Natalia; Viñas López-Pelegrin, Pilar; Sánchez Fernández, Olga; Pérez Ruzafa, Ángel; Campillo Seva, Natalia; León Morán, Lixy Olinda; Química Analítica
    Marine biotoxins are naturally occurring compounds produced around the world by various species of microalgae, whose presence increases significantly due to harmful algal blooms. This phenomenon is a major public health concern, as a large amount of marine fauna is exposed to these biotoxins. The aim of this study was the improvement and application of dispersive liquid-liquid microextraction and liquid chromatography coupled to high-resolution mass spectrometry for the determination of eight lipophilic marine biotoxins, okadaic acid (OA), dinophysistoxin 1 (DTX-1), dinophysistoxin 2 (DTX-2), 16:0 7-O-acyl okadaic acid (DTX-3a), gambierone (GAM), 44-methylgambierone (44-GAM), yessotoxin (YTX), and homoyessotoxin (hYTX), and their derivatives in seawaters and mussels by targeted and untargeted approaches. The proposed method provided detection limits ranging from 0.0004 to 1.7 ng mL-1 in seawater and 0.06 to 119 ng g-1 in mussel samples, depending on the biotoxin. A total of 23 seawater samples collected in the Mar Menor lagoon between 2021 and 2023 were analyzed and several of them were found to contain OA and DTX-3a at concentration levels in the 0.006–1.5 ng mL-1 range. OA and DTX-2 were also found at maximum levels of 8.0 and 1.2 ng g-1, respectively, in several mussel samples from commercial origin. In addition, a suspect screening was developed in the untargeted approach to investigate the presence of other derivatives of the target marine biotoxins in the samples using a home-made database covering 93 compounds. An unsaturated ester derivative of OA/DTX-2 was detected in the seawater samples collected during a red tide.