Browsing by Subject "DLLME"

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    Open Access
    Evaluation of distribution of emerging mycotoxins in human tissues: applications of dispersive liquid–liquid microextraction and liquid chromatography‑mass spectrometry
    (Springer, 2023-11-21) Castell Martínez, Ana; Arroyo Manzanares, Natalia; Palma Manrique, Rosa; Campillo Seva, Natalia; Torres, Carmen; Fenoll, José; Viñas López-Pelegrin, Pilar; Química Analítica
    In this work, a complete study of the distribution of emerging mycotoxins in the human body has been carried out. Specifically, the presence of enniatins (A, A1, B, B1) and beauvericin has been monitored in brain, lung, kidney, fat, liver, and heart samples. A unique methodology based on solid–liquid extraction (SLE) followed by dispersive liquid–liquid microextraction (DLLME) was proposed for the six different matrices. Mycotoxin isolation was performed by adding ultrapure water, acetonitrile, and sodium chloride to the tissue sample for SLE, while the DLLME step was performed using chloroform as extraction solvent. Subsequently, the analysis was carried out by high-performance liquid chromatography coupled to tandem mass spectrometry (HPLC–MS/MS). The proposed method allowed limits of quantification (LOQs) to be obtained in a range of 0.001–0.150 ng/g, depending on the tissue and mycotoxin. The precision was investigated intraday and interday, not exceeding of 9.8% of relative standard deviation. In addition, trueness studies achieved 75 to 115% at a mycotoxin concentration of 25 ng/g and from 82 to 118% at 5 ng/g. The application of this methodology to 26 forensic autopsies demonstrated the bioaccumulation of emerging mycotoxins in the human body since all mycotoxins were detected in tissues. Enniatin B (ENNB) showed a high occurrence, being detected in 100% of liver (7 ± 13 ng/g) and fat samples (0.2 ± 0.8 ng/g). The lung had a high incidence of all emerging mycotoxins at low concentrations, while ENNB, ENNB1, and ENNA1 were not quantifiable in heart samples. Co-occurrence of mycotoxins was also investigated, and statistical tests were applied to evaluate the distribution of these mycotoxins in the human body.
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    Publication
    Open Access
    Non-targeted analysis by DLLME-GC-MS for the monitoring of pollutants in the Mar Menor lagoon
    (Elsevier, 2021-07-17) Peñalver Soler, Rosa María; Ortiz, Alberto; Arroyo-Manzanares, Natalia; Campillo Seva, Natalia; López-García, Ignacio; Viñas López-Pelegrín, Pilar; Química Analítica
    Non-targeted analysis for the monitoring of organic pollutants resulting from agricultural and industrial practices, plastics and pharmaceutical products of seawater from the Mar Menor lagoon (SE Spain) is proposed using dispersive liquid-liquid microextraction (DLLME) and gas chromatography-mass spectrometry (GC-MS). Initially, a home-made MS database including 118 environmental organic pollutants, whose presence in different ecosystems has already been reported, was created. The analytical method was applied for the analysis of 42 samples and a total of 18 pollutants were detected and identified. Samples were obtained from different sites around the Mar Menor in three sampling campaigns, enabling the assessment of impact of rain on the input of the detected chemicals and their distribution. In addition, this methodology was validated using a standard mixture containing 54 of the environmental pollutants included in the database, allowing the quantification of the 9 of the identified compounds (dibutyl phthalate, diisobutyl phthalate, diethyl phthalate, bis(2-ethylhexyl) phthalate, anthracene, 2-methylnaphthalene, hexachlorocyclopentadiene, bis(2-ethylhexyl) adipate and oleamide) with concentration between 3 and 271 μg L−1.