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
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
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
Reddish colour in cooked ham is developed by a mixture of protoporphyrins including Zn-Protoporphyrin and Protoporphyrin IX
(MDPI, 2022-12-15) Giménez Campillo, Claudia; Hernández, Juan de Dios; Guillén, Isidro; Campillo Seva, Natalia; Arroyo Manzanares, Natalia; TorreMinguela, Carlos de; Viñas López-Pelegrin, Pilar; Química Analítica
The nitrosyl–heme complex is considered the pigment responsible for the development of reddish colour in cooked hams. However, the same reddish colour was observed in a nitrite-free product elaborated with polyphenols, suggesting the presence of other red pigments that can contribute to generate this colour. In this study, the protoporphyrins composition of the pigment solution obtained from nitrite and nitrite-free cooked hams was analysed using 80% (v/v) acetone/water solution for extraction. Chromatographic analysis using a combination of diode array and fluorescence detectors revealed the presence of protoporphyrin IX and Zn-protoporphyrin IX in this solution, and these protoporphyrins were subsequently identified with complete certainty by mass spectrometry. These results show how the colour of cooked hams can be developed by a mixture of different protoporphyrins and also demonstrate the absence of selectivity of acetone/water extraction for measuring the content of nitrosyl–heme in cooked hams.
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.
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
Reliable and sensitive analytical platform to assess dietary exposure of pigs to mycotoxins and explore potential urinary biomarkers
(Elsevier, 2024-12-24) Castell Martínez, Ana; Arroyo Manzanares, Natalia; Campillo Seva, Natalia; Sanz Fernández, Santos; Rodríguez Estévez, Vicente; Roquet, Josep; González, Antonio; Fenoll, José; Viñas López-Pelegrin, Pilar; Química Analítica
A reliable and sensitive analytical platform is proposed for the assessment of pig exposure to mycotoxins through the consumption of commercial feed. A total of 48 naturally contaminated feed and 55 urine samples collected from eight Spanish farms were analyzed using a fast and simple methodology based on solid-liquid extraction (SLE) or liquid-liquid extraction (LLE) and dispersive liquid-liquid microextraction (DLLME). High-performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) was used for the targeted analysis of 27 mycotoxins from different families in both matrices achieving limits of quantification in a range of 0.019–73.5 ng/g in feed and 0.011–31.7 ng/mL in urine. All feed samples showed contamination with at least 7 mycotoxins. Enniatins (A, A1, B and B1) and beauvericin were quantified in 100 % of feed samples. ENNB, tenuazonic acid (TeA) and deoxynivalenol (DON) were the mycotoxins with the highest mean total concentrations (1.0 ± 1.9 μg/g, 155 ± 209 ng/g and 81 ± 94 ng/g, respectively). In urine samples, DON, TeA, ENNB1 and ENNA were the most prevalent mycotoxins; and TeA, fumonisin B1 and alternariol had the highest mean total concentration (133 ± 199 ng/mg, 0.43 ± 1.3 μg/mg and 0.29 ± 1.3 μg/mg creatinine, respectively). Statistical tests revealed the correlation of DON and TeA occurrence in feed and urine. Untargeted analysis byHPLC coupled to quadrupole-time-of-flight mass spectrometer (Q-TOF-MS) yielded some urinary biomarkers of mycotoxin exposure and other relevant compounds such as certain antibiotic residues in urine.
Open Access
Dilute-and-shoot-liquid chromatography-quadrupole time of flight-mass spectrometry for pteridine profiling in human urine and its association with different pathologies
(MDPI, 2023-06-01) Giménez Campillo, Claudia; Pastor Belda, Marta; Arroyo Manzanares, Natalia; Campillo Seva, Natalia; Val Oliver, Blanca del; Zarauz García, José; Sáenz, Luis; Viñas López-Pelegrin, Pilar; Química Analítica
Pteridines are a group of compounds synthesised by many living organisms that are involved in the metabolism of many cofactors and vitamins. Their concentration in biological fluids may be altered by various pathologies such as cancer or inflammatory bowel disease, urine being the main route of excretion. In this study, three lumazines and ten pterins were analysed in their native oxidation state using high-performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry. Their high concentration in urine samples and their good ionisation behaviour allow the use of the dilute-and-shoot method by simple filtration of the urine prior to chromatographic analysis. The final method offers excellent linearity, sensitivity and precision parameters, and a total of 135 urine samples were analysed from patients with some relevant information such as faecal calprotectin (FCP) levels, common diseases such as diabetes, hypertension and dyslipidaemia and immunological diseases such as inflammatory bowel disease (IBD). The pteridine profile was related to FCP levels without showing any correlation. In addition, pteridine levels were compared between healthy subjects and IBD, diabetic, hypertensive and dyslipidaemic patients, and significant differences were found between the two groups for some of the pteridines.
Open Access
Advanced materials for magnetic solid-phase extraction of mycotoxins: a review
(Elsevier, 2024-06-20) Castell Martínez, Ana; Arroyo Manzanares, Natalia; Viñas López-Pelegrin, Pilar; López García, Ignacio Francisco; Campillo Seva, Natalia; Química Analítica
Mycotoxins can occur at various stages of the food production process. Due to the toxicity of many of these compounds for human health, the development of analytical methodologies that allow their detection and remediation in food is of great interest. However, food analysis is challenging due to the complexity of the matrices, so sample treatment is a crucial step. Magnetic solid-phase extraction (MSPE) has become one of the most popular green approaches for the isolation of mycotoxins from complex matrices. Furthermore, advanced magnetic materials as molecularly imprinted polymers, metal-organic frameworks and covalent organic frameworks have emerged as promising candidates for MSPE, as they offer a simple and efficient application for mycotoxin extraction due to the possibility to modify and functionalize their surface according to specific requirements. This review provides an overview of the synthesis and recent applications of these sorbents for the MSPE isolation of mycotoxins from complex matrices.
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
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.