Campillo Seva, Natalia

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Campillo Seva, Natalia

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Campillo Seva, Natalia

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Universidad de Murcia. Departamento de Química Analítica

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Open Access
Bioaccumulation of mycotoxins in human forensic liver and animal liver samples using a green sample treatment
(Elsevier, 2023-11-23) Castell Martínez, Ana; Arroyo Manzanares, Natalia; Campillo Seva, Natalia; Torres Sánchez, Carmen; Fenoll, José; Viñas López-Pelegrin, Pilar; Química Analítica
The investigation of the mycotoxin bioaccumulation in human and animals is of wide relevance due to the potential toxicity associated with these secondary metabolites. This study proposes an analytical methodology consisting of salting-out liquid–liquid extraction (SALLE) followed by dispersive liquid–liquid microextraction (DLLME) for the determination of 13 mycotoxins: aflatoxins (G1, G2, B1 and B2), enniatins (A, A1, B and B1), beauvericin, HT-2 and T-2 toxins, zearalenone and deoxynivalenol, in human and animal liver. A targeted analysis was performed by high-performance liquid chromatography with tandem mass spectrometry (HPLC-MS/MS), as well as the screening of derived metabolites by ultrahigh performance LC and high-resolution mass spectrometry (UHPLC-HRMS). The proposed method was in-home validated, and trueness was verified by apparent recovery studies with values between 94 and 110 %. Furthermore, suitable linearities were obtained by the proposed method for all the mycotoxins and detection and quantification limits allow the mycotoxin monitoring at the low levels expected in biological samples. Repeatability and intermediate precision were calculated at two concentration levels, obtaining values of relative standard deviation below 9.5 %. The proposed methodology allowed to study the bioaccumulation of mycotoxins in both human and animal liver, demonstrating the presence of emergent mycotoxins in all liver samples analyzed, specifically enniatins B, B1 and beauvericin were detected with concentrations up to 4.04 μg/kg.
Open Access
Fingerprinting of volatile organic compounds and discrimination of pear samples by gas chromatography-ion mobility spectrometry
(Elsevier, 2025-05-20) Giménez Campillo, Claudia; Pastor Belda, Marta; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Viñas López-Pelegrin, Pilar; Química Analítica
The pear contains many volatile organic compounds that are responsible for its distinctive aroma, flavour and texture. The aim of this work was to develop, optimise and validate an analytical method for the determination of volatile compounds in pears using headspace gas chromatography coupled to ion mobility spectrometry. A total of 254 samples from four cultivars were analysed, and a partial least squares discriminant analysis model using 93 markers allowed differentiation between cultivars with 100 % accuracy and a Q2 of 0.878. Additionally, a total of 227 Ercoline pears collected at different stages of ripening were analysed. For the first time, a predictive model based on 75 markers was used to determine pear ripeness, achieving 100 % accuracy and a Q2 of 0.856. A total of 22 compounds were identified and quantified in the samples and key compounds were determined for each cultivar and ripening stage.
Open Access
Fingerprinting of peach during the ripening process using an analytical platform with spectrometric and volatilome-based chromatographic techniques
(American Chemical Society , 2025-06-23) Giménez Campillo, Claudia; Arroyo Manzanares, Natalia; Pastor Belda, Marta; Campillo Seva, Natalia; Lukas Bodenbender; Weller, Philipp; Viñas López-Pelegrin, Pilar; Química Analítica
In recent years, the quality of peaches has been related to their early harvest, so this work has focused on the characterization of the spectral fingerprint using Fourier transform near-infrared spectroscopy, and headspace gas chromatography (HS-GC) coupled to ion mobility spectrometry (IMS) and mass spectrometry (MS) based on their volatilome or volatile organic compound content, with the aim of identifying the optimum ripening point of peaches. A total of 344 samples of two different varieties at all ripening stages were analyzed. The principal component analysis (PCA) showed a clear tendency for samples at the same stage of ripening to form visible clusters. The groups identified by PCA were used to construct partial least-squares discriminant analysis models that allowed differentiation according to ripening and variety. The overall results were very promising, especially for the volatilomes measured by HS-GC−IMS and HS-GC−MS.
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.
Open Access
Metabolomics study of the formation of genotoxic molecules based on the fecal volatile metabolites profile using an in vivo animal model
(Elsevier, 2024-02-09) Giménez Campillo, Claudia; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Torre-Minguela, Carlos de; Viñas López-Pelegrin, Pilar; Martínez Cáceres, Carlos Manuel; Química Analítica
Epidemiological studies have shown that haem iron from processed meat is a key element involved in the colon carcinogenesis. The haem iron induces lipid peroxidation in the colon lumen during digestion, enabling the formation of cytotoxic molecules derived from these reactions. The cytotoxic molecules generated are highly dependent on dietary factors such as lipid sources, calcium levels or the presence of antioxidants during digestion. Here, we investigated whether nitrite substitution by polyphenols as a food additive could modulate the in vivo luminal lipid peroxidation in the colon and consequently, reduce the formation of mucin-depleted foci in a chemical-induced colon cancer rat model. The addition of polyphenols to the cooked ham diet reduces the lipid peroxidation in the rats. A reduction in cytotoxic aldehydes in fecal water from animals fed with polyphenols as well as a decrease in the formation of mucin-depleted foci is observed. The antioxidant capacity derived from polyphenols modifies the luminal environment of the colon, allowing the identification of a specific molecular signature derived from the analysis of fecal volatile organic compounds. In this molecular signature is included the reduction in the abundance of (2E,4E)-2,4-hexadienal, a carcinogenic aldehyde derived from lipid peroxidation.
Open Access
Ultrasound assisted extraction approach to test the effect of elastic rubber nettings on the N-nitrosamines content of ham meat samples
(MDPI, 2021-10-24) Giménez Campillo, Claudia; Pastor Belda, Marta; Campillo Seva, Natalia; Hernández, Juan de Dios; Guillén, Isidro; Vizcaíno, Pascuala; López García, Ignacio Francisco; Hernández Córdoba, Manuel; Arroyo Manzanares, Natalia; Viñas López-Pelegrin, Pilar; Química Analítica
Nitrosamines (NAs), which are catalogued as carcinogenic compounds, may be present in meat products due to the conversion of nitrites and as result of migration from elastic rubber nettings used. A method based on ultrasonic assisted extraction coupled with dispersive liquid–liquid microextraction as sample treatment and gas chromatography-mass spectrometry as separation and detection technique was proposed for the determination of twelve NAs in cooked ham samples. The method was validated by evaluating linearity (0.5–1000 ng g−1), matrix effect, sensitivity (detection limits were between 0.15 and 1.4 ng g−1) and precision, which was below 12%. Five NAs were found in the samples with levels ranging from not quantifiable to 40 ng g−1. The effect of the elastic rubber nettings on the nitrosamine content of meat was evaluated by comparing the levels found in products made with several plastics or thread in the presence of additives.
Open Access
Monitorization of ibuprofen, diclofenac and triclosan and their photolytic transformation products
(Elsevier, 2025-06-03) León Morán, Lixy Olinda; Pastor Belda, Marta; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Viñas López-Pelegrin, Pilar; Martínez-Escudero, Carmen Maria; Garrido, Isabel; Contreras, Fulgencio; Hellín, Pilar; Flores, Pilar; Aliste, Marina; Fenoll, José; Química Analítica; Facultades de la UMU::Facultad de Química
The presence of contaminants of emerging concern (CECs) in wastewater treatment plant (WWTP) effluents poses a significant risk to human health and the environment. The application of photolytic processes in remediation of WWTP effluents results in the formation of transformation products (TPs) with unknown environmental impact. Thus, the identification of TPs and the monitoring of their evolution during the remediation process is of great interest. This study presents a new analytical method for the determination of three CECs (ibuprofen, IBU; diclofenac, DCF; triclosan, TCS) and their respective TPs in water subjected to direct photolysis by ultraviolet A irradiation with light emitting diode lamps. The analytes were extracted using in situ ionic liquid dispersive liquid–liquid microextraction and analysed by liquid chromatography with high resolution mass spectrometry (LC-HRMS) for the identification of known and unknown TPs. The identification of TPs was conducted through two untargeted strategies: a suspect screening based on the utilization of a home-made database created from the TPs previously described, and a screening for novel TPs based on the spectral investigation of a deconvoluted and aligned list of peaks with suitable degradation trends. The proposed analytical strategy allowed up to 39 TPs being identified, with 10 of them being structurally proposed for the first time in this study. In addition, verification of the identified TPs was carried out by LC with triple quadrupole. Moreover, the three CECs and their TPs were monitored in four WWTP samples subjected to degradation trials and two TPs (DCF-TP296C and TCS-TP303C) were found.
Open Access
Discrimination of the geographical origin of peaches by the monitoring of volatile organic compounds by gas chromatography with mass spectrometry and chemometric tools
(Elsevier, 2024-02-24) Giménez Campillo, Claudia; Arroyo Manzanares, Natalia; Pastor Belda, Marta; Campillo Seva, Natalia; Viñas López-Pelegrin, Pilar; Química Analítica
The peach is one of the most popular and widely consumed fruits in Europe. Spain is the largest peach-producing country in the world with several growing areas recognised by consumers. This work focuses on the development, optimisation and validation of a non-targeted metabolomics strategy for the determination of peach volatile organic compounds from different origins by headspace gas chromatography coupled to mass spectrometry (HS–GC–MS). The volatil profile found in each sample is used to classify peaches according to their origin. The results obtained were processed using MS-DIAL software and 279 features were detected, of which 102 volatile compounds were tentatively identified and 30 of them could also be quantified. In addition, the areas of all the features were used to build models based on orthogonal partial least squares discriminant analysis (OPLS-DA) to differentiate peaches according to their geographical origin. A very promising model was obtained, with a validation rate of 90.32%, which means that it could be used to guarantee the Protected Designation of Origin of different peaches with a simple analysis.
Open Access
Evaluation of the potential use of protoporphyrins as biomarkers of anemic disease in human urine from inflammatory bowel disease patients
(Elsevier, 2024-09-02) Giménez Campillo, Claudia; Montoya Méndez, Isabel; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; Val Oliver, Blanca del; Zarauz García, José; Sáenz, Luis; Viñas López-Pelegrin, Pilar; Química Analítica
Protoporphyrins are organic compounds with cyclic structure that are synthesised by a wide variety of organisms. In humans, these compounds are detected in blood and urine, with significantly higher levels in blood. Their potential as biomarkers of anemia and other diseases is currently being investigated, as their levels change according to the biochemical processes associated with the disease. The most widely used biomarker of anemia is serum ferritin, but it is unreliable in patients with inflammatory bowel disease (IBD) because its levels can be altered by acute inflammation and/or infections. There is therefore a need to look for new markers to help diagnose anemia in IBD patients. This work develops and validates a method for the determination of three protoporphyrins in human urine: protoporphyrin IX (PPIX), protoporphyrin IX complex with Zn (ZnPPIX) and protoporphyrin IX complex with Fe (II) (FePPIX), the latter also known as heme. The aim is to evaluate their potential as biomarkers of anemic disease in patients diagnosed with IBD. The proposed analytical method is based on high performance liquid chromatography (HPLC) with dual detection based on photodiode array (PDA) and fluorescence (FD). Quantification of the analytes at very low concentrations is possible due to the efficient preconcentration provided by dispersive liquid-liquid microextraction (DLLME) and the sensitivity of the detection systems. The method was validated by evaluating linearity (25–1000 ng mL􀀀 1), matrix effect, sensitivity (limits of quantification were between 5 and 11 ng mL􀀀 1), selectivity, accuracy, carry-over, dilution integrity, stability and precision (< 12.1 %). Finally, statistical analyses applied to the sample quantification results showed these three markers, together with five clinical markers, were significantly different between anemic and non-anemic IBD patients.
Open Access
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.