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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.
Rosa Peñalver; Alberto Ortiz; Natalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Pilar Viñas. Non-targeted analysis by DLLME-GC-MS for the monitoring of pollutants in the Mar Menor lagoon. Chemosphere 2021, 286, 131588 .
AMA StyleRosa Peñalver, Alberto Ortiz, Natalia Arroyo-Manzanares, Natalia Campillo, Ignacio López-García, Pilar Viñas. Non-targeted analysis by DLLME-GC-MS for the monitoring of pollutants in the Mar Menor lagoon. Chemosphere. 2021; 286 ():131588.
Chicago/Turabian StyleRosa Peñalver; Alberto Ortiz; Natalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Pilar Viñas. 2021. "Non-targeted analysis by DLLME-GC-MS for the monitoring of pollutants in the Mar Menor lagoon." Chemosphere 286, no. : 131588.
Dry-cured Iberian ham is officially classified into different commercial categories according to the pig’s breed and feeding regime. These reach very different prices, thus promoting labelling fraud and causing great damage to the food sector. In this work, a method based on Raman spectroscopy was explored as a rapid in situ screening tool for Iberian ham samples. A total of 110 samples were analyzed to assess the potential of this technique to differentiate purebred, crossbred, acorn-fed and feed-fed dry-cured Iberian ham. A continuous signal probably due to sample fluorescence was obtained, which hid the Raman scattering signal. Therefore, chemometric treatment was applied in order to extract non-apparent information. High validated classification rates were obtained for feeding regime (83.3%) and breed (86.7%). In addition, an interlaboratory study was carried out to confirm the applicability of the method with 52 samples, obtaining a validated rate above 80%.
Andrés Martín-Gómez; Natalia Arroyo-Manzanares; María García-Nicolás; Ángela López-Lorente; Soledad Cárdenas; Ignacio López-García; Pilar Viñas; Manuel Hernández-Córdoba; Lourdes Arce. Portable Raman Spectrometer as a Screening Tool for Characterization of Iberian Dry-Cured Ham. Foods 2021, 10, 1177 .
AMA StyleAndrés Martín-Gómez, Natalia Arroyo-Manzanares, María García-Nicolás, Ángela López-Lorente, Soledad Cárdenas, Ignacio López-García, Pilar Viñas, Manuel Hernández-Córdoba, Lourdes Arce. Portable Raman Spectrometer as a Screening Tool for Characterization of Iberian Dry-Cured Ham. Foods. 2021; 10 (6):1177.
Chicago/Turabian StyleAndrés Martín-Gómez; Natalia Arroyo-Manzanares; María García-Nicolás; Ángela López-Lorente; Soledad Cárdenas; Ignacio López-García; Pilar Viñas; Manuel Hernández-Córdoba; Lourdes Arce. 2021. "Portable Raman Spectrometer as a Screening Tool for Characterization of Iberian Dry-Cured Ham." Foods 10, no. 6: 1177.
The most common mycotoxins are aflatoxins (AFs), which are produced by strains of various species of molds in the genus Aspergillus (A. flavus, A. parasiticus, A. nomius and A. tamarii) and can grow on many foods, mainly peanuts, maize and cottonseed. AFs are currently considered to be the most hazardous mycotoxins to health, in particular because of their hepatocellular carcinogenic potential. The main aflatoxins are B1 (AFB1), B2 (AFB2), G1 (AFG1) and G2 (AFG2) although many other derivatives have been described. In addition, animals consuming contaminated feeds are able to metabolize them by hydroxylation in a certain position, yield for example aflatoxin M1 (AFM1) and aflatoxin M2 (AFM2) from AFB1 and AFB2, respectively. Nowadays, only the four main AFs and one hydroxylated metabolite (AFM1) are routinely analyzed. High resolution mass spectrometry (HRMS) using Orbitrap or time-of-flight (TOF) mass analysers is a trend for AFs determination, allowing to determine AFs and their derivatives for which there are no commercial standards available, in order to carry out metabolization studies, exposure assessment or monitoring modified AFs in food. The aim of this study is to show the recent trends in analytical methods based on LC-HRMS for determination of AFs.
Natalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Pilar Viñas. Determination of Aflatoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry. Aflatoxins [Working Title] 2021, 1 .
AMA StyleNatalia Arroyo-Manzanares, Natalia Campillo, Ignacio López-García, Pilar Viñas. Determination of Aflatoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry. Aflatoxins [Working Title]. 2021; ():1.
Chicago/Turabian StyleNatalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Pilar Viñas. 2021. "Determination of Aflatoxins by Liquid Chromatography Coupled to High-Resolution Mass Spectrometry." Aflatoxins [Working Title] , no. : 1.
Mycotoxins are toxic secondary metabolites produced by some filamentous fungi from Aspergillus, Fusarium, Penicillium, Alternaria and Claviceps genera. These metabolites are stable chemical compounds and persist during processing and heat treatment, so they can contaminate food and animal feed causing a broad spectrum of adverse effects both in humans and animals. In addition, mycotoxins can bioaccumulate in organs, and tissues, thereby affecting the nervous, endocrine, and immune systems; or can be excreted by biological fluids or faeces, being able to use as biomarkers of mycotoxin exposure. The most common are aflatoxins (B1, B2, G1, and G2), ochratoxin A, fumonisins, trichothecenes, zearalenone and patulin, although approximately 400 different mycotoxins have been described to date. Moreover, unaltered mycotoxins are not the only source of exposure since, as part of their defence against xenobiotics, plant and living organisms may alter their chemical structure. Liquid chromatography (LC) coupled to tandem mass spectrometry (MS/MS) is commonly used for determining mycotoxins. However, not all mycotoxins or modified mycotoxins are commercially available as reference standards for use in monitoring, and, as a result, interest in high resolution mass spectrometry (HRMS) is increasing. More specifically, Orbitrap and time-of-flight (TOF) mass analysers have emerged as the most useful technique for mycotoxin determination. HRMS has important advantages over other methods, including the ability to record full scan spectra by measuring the accurate mass of analytes, the screening of untargeted compounds, a high degree of structural confirmation, and retrospective analysis data that offer the possibility of investigating analytes that were not considered at the time of spectral acquisition. This review discusses recent studies for the targeted and untargeted determination of mycotoxins in urine, blood and other relevant biological samples using strategies based on HRMS.
Natalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. High-resolution mass spectrometry for the determination of mycotoxins in biological samples. A review. Microchemical Journal 2021, 166, 106197 .
AMA StyleNatalia Arroyo-Manzanares, Natalia Campillo, Ignacio López-García, Manuel Hernández-Córdoba, Pilar Viñas. High-resolution mass spectrometry for the determination of mycotoxins in biological samples. A review. Microchemical Journal. 2021; 166 ():106197.
Chicago/Turabian StyleNatalia Arroyo-Manzanares; Natalia Campillo; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. 2021. "High-resolution mass spectrometry for the determination of mycotoxins in biological samples. A review." Microchemical Journal 166, no. : 106197.
After the International Agency for Research on Cancer (IARC) classified ingested nitrites and nitrates as “probably carcinogenic to humans” under conditions favoring endogenous nitrosation, several meat products labeled as “made without nitrite” were launched. In order to distinguish uncured products truly made without nitrite from cured products made with any nitrite source (vegetal or mineral), this article presents an approach to detect and quantify nitrite from different origins added to meat. The method consists on the determination of nitrous oxide as a target compound using headspace gas chromatography–mass spectrometry (HS-GC–MS). Nitrous oxide (N2O) is formed after two reduction steps: from nitrite to nitric oxide (NO) and then to N2O. The NO is bound to myoglobin (Mb) or metmyoglobin (Met-Mb), forming a complex, which is subsequently released using sulfuric acid, which also favors the reduction to N2O. The HS-GC–MS conditions were split ratio 1:10; injection temperature at 70 °C; incubation temperature at 30 °C and time 45 min; and injection volume 1 mL. As a result, a relationship was established between the concentration of nitrite in cooked ham samples and the area of the N2O peak generated, meaning that this method allows the quantification of added nitrite within a concentration range of 10 to 100 mg kg−1.
Juan Hernández; Ana Castell; Natalia Arroyo-Manzanares; Isidro Guillén; Pascuali Vizcaíno; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. Toward Nitrite-Free Curing: Evaluation of a New Approach to Distinguish Real Uncured Meat from Cured Meat Made with Nitrite. Foods 2021, 10, 313 .
AMA StyleJuan Hernández, Ana Castell, Natalia Arroyo-Manzanares, Isidro Guillén, Pascuali Vizcaíno, Ignacio López-García, Manuel Hernández-Córdoba, Pilar Viñas. Toward Nitrite-Free Curing: Evaluation of a New Approach to Distinguish Real Uncured Meat from Cured Meat Made with Nitrite. Foods. 2021; 10 (2):313.
Chicago/Turabian StyleJuan Hernández; Ana Castell; Natalia Arroyo-Manzanares; Isidro Guillén; Pascuali Vizcaíno; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. 2021. "Toward Nitrite-Free Curing: Evaluation of a New Approach to Distinguish Real Uncured Meat from Cured Meat Made with Nitrite." Foods 10, no. 2: 313.
Paprika is considered a high-quality product being one of the most consumed spices in the world. Contamination with mycotoxins may appear due to inappropriate practices during processing or resulting from invading mould in the final manufactured products. A sample treatment based on dispersive magnetic solid-phase extraction (DMSPE) has been proposed for emerging mycotoxin determination, enniatins (ENNs) and beauvericins (BEAs), in paprika. Different magnetic nanoparticles were tested, and cellulose-ferrite nanocomposite was selected for the extraction and preconcentration of the mycotoxins. Nanocomposite was characterised using field emission scanning electron microscopy and energy dispersive X-ray spectroscopy in terms of morphology and elemental composition. High-resolution mass spectrometry allowed the quantification of the five main emerging mycotoxins and the monitoring of unexpected members of this class of toxic fungal secondary metabolites. The method has been validated, obtaining limits of quantification between 9.5 and 9.9 μg kg−1 and testing its trueness through recovery studies, with satisfactory values of between 89.5 and 97.7%. Relative standard deviations were calculated to evaluate the intra- and inter-day precision and values lower than 8% were obtained in all cases. The analysis of 26 samples, including conventional and organic, demonstrated the presence of ENNB1 at 12.0 ± 0.6 μg kg−1 in one of the samples studied. Other analogues ENNs and BEAs were not detected.
María García-Nicolás; Natalia Arroyo-Manzanares; Natalia Campillo; Pilar Viñas. Cellulose-ferrite nanocomposite for monitoring enniatins and beauvericins in paprika by liquid chromatography and high-resolution mass spectrometry. Talanta 2021, 226, 122144 .
AMA StyleMaría García-Nicolás, Natalia Arroyo-Manzanares, Natalia Campillo, Pilar Viñas. Cellulose-ferrite nanocomposite for monitoring enniatins and beauvericins in paprika by liquid chromatography and high-resolution mass spectrometry. Talanta. 2021; 226 ():122144.
Chicago/Turabian StyleMaría García-Nicolás; Natalia Arroyo-Manzanares; Natalia Campillo; Pilar Viñas. 2021. "Cellulose-ferrite nanocomposite for monitoring enniatins and beauvericins in paprika by liquid chromatography and high-resolution mass spectrometry." Talanta 226, no. : 122144.
The use of dispersive liquid–liquid microextraction (DLLME) is proposed for the preconcentration of thirteen lipophilic marine toxins in seawater samples. For this purpose, 0.5 mL of methanol and 440 µL of chloroform were injected into 12 mL of sample. The enriched organic phase, once evaporated and reconstituted in methanol, was analyzed by reversed-phase liquid chromatography with triple-quadrupole tandem mass spectrometry. A central composite design multivariate method was used to optimize the interrelated parameters affecting DLLME efficiency. The absence of any matrix effect in the samples allowed them to be quantified against aqueous standards. The optimized procedure was validated by recovery studies, which provided values in the 82–123% range. The detection limits varied between 0.2 and 5.7 ng L−1, depending on the analyte, and the intraday precision values were in the 0.1–7.5% range in terms of relative standard deviation. Ten water samples taken from different points of the Mar Menor lagoon were analyzed and were found to be free of the studied toxins.
Ainhoa Oller-Ruiz; Natalia Campillo; Manuel Hernández-Córdoba; Javier Gilabert; Pilar Viñas. Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry. Toxins 2021, 13, 57 .
AMA StyleAinhoa Oller-Ruiz, Natalia Campillo, Manuel Hernández-Córdoba, Javier Gilabert, Pilar Viñas. Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry. Toxins. 2021; 13 (1):57.
Chicago/Turabian StyleAinhoa Oller-Ruiz; Natalia Campillo; Manuel Hernández-Córdoba; Javier Gilabert; Pilar Viñas. 2021. "Monitoring Lipophilic Toxins in Seawater Using Dispersive Liquid—Liquid Microextraction and Liquid Chromatography with Triple Quadrupole Mass Spectrometry." Toxins 13, no. 1: 57.
Ranitidine drug products were recently recalled because they contained carcinogenic nitrosamines (NAs), such as N-nitrosodimethylamine (NDMA) and N-nitrosodiethylamine (NDEA). This episode emphasises the importance of developing analytical methods to determine NAs in this type of product. This study describes the development and validation of an analytical method for the determination of nine NAs (NDMA, N-nitrosomethylethylamine (NEMA), NDEA, N-nitrosopyrrolidine (NPYR), N-nitrosomorpholine (NMOR) N-nitrosodi-n-propylamine (NDPA) N-nitrosopiperidine (NPIP), N-nitrosodi-n-butylamine (NDBA) and N-nitrosodiphenylamine (NDPhA)) in ranitidine drug samples using a combination of microextraction and gas chromatography-mass spectrometry. The procedure involved the dissolution of 1 g of sample in 10 mL of water. For the dispersive liquid-liquid microextraction, 0.5 g of NaCl was added to this aqueous solution, followed by a mixture containing 0.5 mL methanol as dispersant and 150 μL chloroform as extractant solvent. The recovered organic phase was injected into the GC-MS system and a 20 min oven programme was applied. Quantification limits were in the 0.21-21 ng g-1 range, corresponding to NDPhA and NDMA, respectively. Relative standard deviations lower than 12% were achieved in all cases, which indicates the adequate precision of the method. Seven pharmaceutical products containing two different amounts of ranitidine (150 and 300 mg) were analysed. None of the samples contained NEMA, NDEA, NPYR, NMOR, NDPA or NPIP, while NDMA, NDBA and NDPhA were found in three products.
Claudia Giménez-Campillo; Marta Pastor-Belda; Natalia Campillo; Manuel Hernández-Córdoba; Pilar Viñas. Development of a new methodology for the determination of N-nitrosamines impurities in ranitidine pharmaceuticals using microextraction and gas chromatography-mass spectrometry. Talanta 2020, 223, 121659 .
AMA StyleClaudia Giménez-Campillo, Marta Pastor-Belda, Natalia Campillo, Manuel Hernández-Córdoba, Pilar Viñas. Development of a new methodology for the determination of N-nitrosamines impurities in ranitidine pharmaceuticals using microextraction and gas chromatography-mass spectrometry. Talanta. 2020; 223 ():121659.
Chicago/Turabian StyleClaudia Giménez-Campillo; Marta Pastor-Belda; Natalia Campillo; Manuel Hernández-Córdoba; Pilar Viñas. 2020. "Development of a new methodology for the determination of N-nitrosamines impurities in ranitidine pharmaceuticals using microextraction and gas chromatography-mass spectrometry." Talanta 223, no. : 121659.
Due to its multiple advantages, ion mobility spectrometry (IMS) is being considered as a complementary technique to mass spectrometry (MS). The goal of this work is to investigate and compare the capacity of IMS and MS in the classification of olive oil according to its quality. For this purpose, two analytical methods based on headspace gas chromatography (HS-GC) coupled with MS or with IMS have been optimized and characterized for the determination of volatile organic compounds from olive oil samples. Both detectors were compared in terms of sensitivity and selectivity, demonstrating that complementary data were obtained and both detectors have proven to be complementary. MS and IMS showed similar selectivity (10 out of 38 compounds were detected by HS-GC-IMS, whereas twelve compounds were detected by HS-GC-MS). However, IMS presented slightly better sensitivity (Limits of quantification (LOQ) ranged between 0.08 and 0.8 µg g−1 for HS-GC-IMS, and between 0.2 and 2.1 µg g−1 for HS-GC-MS). Finally, the potential of both detectors coupled with HS-GC for classification of olive oil samples depending on its quality was investigated. In this case, similar results were obtained when using both HS-GC-MS and HS-GC-IMS equipment (85.71 % of samples of the external validation set were classified correctly (validation rate)) and, although both techniques were shown to be complementary, data fusion did not improve validation results (80.95% validation rate).
María García-Nicolás; Natalia Arroyo-Manzanares; Lourdes Arce; Manuel Hernández-Córdoba; Pilar Viñas. Headspace Gas Chromatography Coupled to Mass Spectrometry and Ion Mobility Spectrometry: Classification of Virgin Olive Oils as a Study Case. Foods 2020, 9, 1288 .
AMA StyleMaría García-Nicolás, Natalia Arroyo-Manzanares, Lourdes Arce, Manuel Hernández-Córdoba, Pilar Viñas. Headspace Gas Chromatography Coupled to Mass Spectrometry and Ion Mobility Spectrometry: Classification of Virgin Olive Oils as a Study Case. Foods. 2020; 9 (9):1288.
Chicago/Turabian StyleMaría García-Nicolás; Natalia Arroyo-Manzanares; Lourdes Arce; Manuel Hernández-Córdoba; Pilar Viñas. 2020. "Headspace Gas Chromatography Coupled to Mass Spectrometry and Ion Mobility Spectrometry: Classification of Virgin Olive Oils as a Study Case." Foods 9, no. 9: 1288.
The most commonly used technique for monitoring microbial contamination in cosmetic products is plate counting. In this contribution, headspace - gas chromatography (HS-GC) coupled to mass spectrometry (MS) or ion mobility spectrometry (IMS) is proposed as a technique to evaluate rapidly and accurately the state of microbial colonies in cosmetic creams using the volatile organic compounds produced by microorganisms (MVOC). The work focuses on monitoring two of the microorganisms that most frequently occur in such creams, Candida albicans and Staphylococcus aureus. In addition, two different types of ingredient with antimicrobial properties (a chemical preservative and a natural preservative) were added to study the behaviour of these microorganisms under different conditions. The facial creams were elaborated and inoculated with the two above microorganisms, and then sampled weekly for 4 weeks, analysing the evolution of the MVOCs by HS-GC-MS and HS-GC-IMS. In addition, microbial contamination was determined by the classical plate counting method. The pH, colour, viscosity and water activity parameters were also measured. The use of chemometric tools is essential because of the large amount of data generated, and different models based on discriminant analysis with an orthogonal projection on latent structures (OPLS-DA) were constructed. The optimal models obtained by both analytical techniques allowed differentiation between contaminated and non-contaminated creams, with a validation success rate of 94.4%. In addition, MVOC monitoring also allowed assessment of the microbial concentration.
María García-Nicolás; Natalia Arroyo-Manzanares; Juan De Dios Hernández; Isidro Guillén; Pascuala Vizcaíno; Marta Sánchez-Rubio; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. Ion mobility spectrometry and mass spectrometry coupled to gas chromatography for analysis of microbial contaminated cosmetic creams. Analytica Chimica Acta 2020, 1128, 52 -61.
AMA StyleMaría García-Nicolás, Natalia Arroyo-Manzanares, Juan De Dios Hernández, Isidro Guillén, Pascuala Vizcaíno, Marta Sánchez-Rubio, Ignacio López-García, Manuel Hernández-Córdoba, Pilar Viñas. Ion mobility spectrometry and mass spectrometry coupled to gas chromatography for analysis of microbial contaminated cosmetic creams. Analytica Chimica Acta. 2020; 1128 ():52-61.
Chicago/Turabian StyleMaría García-Nicolás; Natalia Arroyo-Manzanares; Juan De Dios Hernández; Isidro Guillén; Pascuala Vizcaíno; Marta Sánchez-Rubio; Ignacio López-García; Manuel Hernández-Córdoba; Pilar Viñas. 2020. "Ion mobility spectrometry and mass spectrometry coupled to gas chromatography for analysis of microbial contaminated cosmetic creams." Analytica Chimica Acta 1128, no. : 52-61.
Plastic food packages usually contain additives which may migrate from the package into the food and then be ingested by the consumer, representing a risk for their health. In this study, targeted and untargeted analysis by gas chromatography-mass spectrometry (GC–MS) is proposed to monitor any contaminants of this type in honey. The application of dispersive liquid–liquid microextraction (DLLME) as a preconcentration technique allowed very low detection limits to be reached for all the substances. Fifteen target compounds, including styrene, phthalates, fatty acids, alkylphenols and bisphenol A, were quantified. Untargeted analyses were also carried out, allowing other migrants in the honey samples to be identified, such as two phthalates, four acids, three esters, one aldehyde, one hydrocarbon and two alkyl phenol compounds. The proposed method was seen to be a useful approach for the quantification and identification of potential migrants from plastics in challenging samples such as honey.
Rosa Peñalver; Natalia Arroyo-Manzanares; Natalia Campillo; Pilar Viñas. Targeted and untargeted gas chromatography-mass spectrometry analysis of honey samples for determination of migrants from plastic packages. Food Chemistry 2020, 334, 127547 .
AMA StyleRosa Peñalver, Natalia Arroyo-Manzanares, Natalia Campillo, Pilar Viñas. Targeted and untargeted gas chromatography-mass spectrometry analysis of honey samples for determination of migrants from plastic packages. Food Chemistry. 2020; 334 ():127547.
Chicago/Turabian StyleRosa Peñalver; Natalia Arroyo-Manzanares; Natalia Campillo; Pilar Viñas. 2020. "Targeted and untargeted gas chromatography-mass spectrometry analysis of honey samples for determination of migrants from plastic packages." Food Chemistry 334, no. : 127547.
A rapid analytical procedure is proposed for determining two antimicrobial onion organosulfur compounds, propyl disulfide (PDS) and propyl propane thiosulfonate (PTSO), in animal feed.
Marta Pastor-Belda; Natalia Arroyo-Manzanares; Kateryna Yavir; Paloma Abad; Natalia Campillo; Manuel Hernández-Córdoba; Pilar Viñas. A rapid dispersive liquid–liquid microextraction of antimicrobial onion organosulfur compounds in animal feed coupled to gas chromatography-mass spectrometry. Analytical Methods 2020, 12, 2668 -2673.
AMA StyleMarta Pastor-Belda, Natalia Arroyo-Manzanares, Kateryna Yavir, Paloma Abad, Natalia Campillo, Manuel Hernández-Córdoba, Pilar Viñas. A rapid dispersive liquid–liquid microextraction of antimicrobial onion organosulfur compounds in animal feed coupled to gas chromatography-mass spectrometry. Analytical Methods. 2020; 12 (21):2668-2673.
Chicago/Turabian StyleMarta Pastor-Belda; Natalia Arroyo-Manzanares; Kateryna Yavir; Paloma Abad; Natalia Campillo; Manuel Hernández-Córdoba; Pilar Viñas. 2020. "A rapid dispersive liquid–liquid microextraction of antimicrobial onion organosulfur compounds in animal feed coupled to gas chromatography-mass spectrometry." Analytical Methods 12, no. 21: 2668-2673.
This work focuses on the development, validation and application of an analytical method for the determination of twenty organochlorine pesticides (OCPs) in human tissues using salting-out liquid–liquid extraction and dispersive liquid–liquid microextraction for sample preparation and gas chromatography–mass spectrometry to analyze the obtained extracts. Measurement of the concentration levels of these toxics in tissues can be used to assess the risk of the population to exposure. The linearity of the proposed method was verified in the 10–1,000 ng/g range. The sensitivity was evaluated calculating the limits of detection (LODs) for 20 OCPs (α-, β-, γ- and δ-hexachlorocyclohexane (HCH), α- and β-endosulfan, endosulfan sulfate, aldrin, dieldrin, endrin, endrin ketone, endrin aldehyde, α- and γ-chlordane, 4,4′-dichlorodiphenyltrichloroethane, 4,4′-dichlorodiphenyldichloroethylene (DDE), 4,4′-dichlorodiphenyldichloroethane, heptachlor, heptachlor epoxide and methoxychlor), most of them being found between 1.0 and 16 ng/g. The intra- and interday precisions were <12% for relative standard deviation values. The accuracy of the method was evaluated by recovery studies, which gave recovery percentages in the 85–109% range. Seven different tissues (liver, kidney, heart, spleen, lung, brain and abdominal fat) from eight autopsies were analyzed, and only three cases were seen to have β-HCH and 4,4′-DDE in abdominal fat, while 4,4′-DDE was also detected in the heart of one case. The rest of the samples were free of the studied OCPs at least above the corresponding LODs.
Marta Pastor Belda; José Antonio González-Franco; Ricardo Rubio; Natalia Campillo; Manuel Hernández-Córdoba; Carmen Torres; María Dolores Pérez-Cárceles; Pilar Viñas. Occurrence of Organochlorine Pesticides in Human Tissues Assessed Using a Microextraction Procedure and Gas Chromatography–Mass Spectrometry. Journal of Analytical Toxicology 2020, 45, 84 -92.
AMA StyleMarta Pastor Belda, José Antonio González-Franco, Ricardo Rubio, Natalia Campillo, Manuel Hernández-Córdoba, Carmen Torres, María Dolores Pérez-Cárceles, Pilar Viñas. Occurrence of Organochlorine Pesticides in Human Tissues Assessed Using a Microextraction Procedure and Gas Chromatography–Mass Spectrometry. Journal of Analytical Toxicology. 2020; 45 (1):84-92.
Chicago/Turabian StyleMarta Pastor Belda; José Antonio González-Franco; Ricardo Rubio; Natalia Campillo; Manuel Hernández-Córdoba; Carmen Torres; María Dolores Pérez-Cárceles; Pilar Viñas. 2020. "Occurrence of Organochlorine Pesticides in Human Tissues Assessed Using a Microextraction Procedure and Gas Chromatography–Mass Spectrometry." Journal of Analytical Toxicology 45, no. 1: 84-92.
A rapid procedure for the determination of amphenicol antibiotics in human urine by liquid chromatography with quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) is proposed. The presence of thiamphenicol (TAP), florfenicol (FF) and chloramphenicol (CAP) in the human body can be attributed to their administration to treat certain diseases or by eating food of animal origin. The TAP, FF and CAP excreted in urine is mainly in the form of glucuronide conjugates, although their free forms may also be excreted to a lesser extent. In the procedure described, the enzymatic hydrolysis of amphenicol glucuronide forms in urine was carried out using β-glucuronidase and sulfatase at pH 5 (37 °C, overnight) in order to discriminate the free and conjugated forms. Then, amphenicol antibiotics were submitted to dispersive liquid–liquid microextraction (DLLME) for preconcentration. All the parameters affecting DLLME efficiency were optimized, and the following conditions were selected: 0.9 g NaCl in 10 mL of urine, to which 1.2 mL methanol (as dispersant solvent) and 1 mL of 4-methyl-2-pentanone (as extractant solvent) were added. The absence of a matrix effect allowed quantification of the samples against aqueous standards. Detection limits were 29, 6 and 3 pg mL−1 for TAP, FF and CAP, respectively. Relative standard deviations were calculated to evaluate the intra- and inter-day precision and values lower than 10% were obtained in all cases. The trueness of the method was tested through recovery studies, obtaining satisfactory values (83–104%). Ten urine samples obtained from volunteers were analysed and all of them were free of the studied antibiotics.
Marta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Manuel Hernández-Córdoba; Pilar Viñas. Determination of amphenicol antibiotics and their glucuronide metabolites in urine samples using liquid chromatography with quadrupole time-of-flight mass spectrometry. Journal of Chromatography B 2020, 1146, 122122 .
AMA StyleMarta Pastor-Belda, Natalia Campillo, Natalia Arroyo-Manzanares, Manuel Hernández-Córdoba, Pilar Viñas. Determination of amphenicol antibiotics and their glucuronide metabolites in urine samples using liquid chromatography with quadrupole time-of-flight mass spectrometry. Journal of Chromatography B. 2020; 1146 ():122122.
Chicago/Turabian StyleMarta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Manuel Hernández-Córdoba; Pilar Viñas. 2020. "Determination of amphenicol antibiotics and their glucuronide metabolites in urine samples using liquid chromatography with quadrupole time-of-flight mass spectrometry." Journal of Chromatography B 1146, no. : 122122.
An ion-pair liquid–liquid microextraction procedure followed by LC tandem mass spectrometry allows a reliable and sensitive determination glyphosate, glufosinate y aminomethylphosphonic acid in agricultural samples.
Javier Marín; Natalia Campillo; Manuel Hernández-Córdoba; Isabel Garrido; José Fenoll; Pilar Viñas. Liquid–liquid microextraction of glyphosate, glufosinate and aminomethylphosphonic acid for the analysis of agricultural samples by liquid chromatography. Analytical Methods 2020, 12, 2039 -2045.
AMA StyleJavier Marín, Natalia Campillo, Manuel Hernández-Córdoba, Isabel Garrido, José Fenoll, Pilar Viñas. Liquid–liquid microextraction of glyphosate, glufosinate and aminomethylphosphonic acid for the analysis of agricultural samples by liquid chromatography. Analytical Methods. 2020; 12 (15):2039-2045.
Chicago/Turabian StyleJavier Marín; Natalia Campillo; Manuel Hernández-Córdoba; Isabel Garrido; José Fenoll; Pilar Viñas. 2020. "Liquid–liquid microextraction of glyphosate, glufosinate and aminomethylphosphonic acid for the analysis of agricultural samples by liquid chromatography." Analytical Methods 12, no. 15: 2039-2045.
Dispersive magnetic solid-phase extraction (DMSPE) has received growing attention for sample treatment preconcentration prior to the separation of analytes due to its many advantages. In the present work, the potential of DMSPE for the determination of emergent mycotoxins (enniatins A, A1, B and B1, and beauvericin) is investigated for the first time. Different magnetic nanoparticles were tested and a magnetic multiwalled carbon nanotube ([email protected]) composite was selected for the extraction and preconcentration of the five target mycotoxins in human urine samples before their analysis by ultrahigh performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS). The nanocomposite was characterized by energy dispersive X-ray spectrometry, scanning electron microscopy, Fourier transform infrared spectrophotometry, and X-ray diffraction. Several parameters affecting the adsorption and desorption of DMSPE steps were optimized and the method was fully validated. Due to a matrix effect, matrix-matched calibration curves were necessary to carry out quantification. In this way, limits of quantification of between 0.04 and 0.1 μg/L, relative standard deviation values lower than 12% and recoveries between 89.3% and 98.9% were obtained. Finally, a study of the reuse of the [email protected] composite was carried out, confirming that it can be reused at least four times.
Natalia Arroyo-Manzanares; Rosa Peñalver-Soler; Natalia Campillo; Pilar Viñas. Dispersive Solid-Phase Extraction using Magnetic Carbon Nanotube Composite for the Determination of Emergent Mycotoxins in Urine Samples. Toxins 2020, 12, 51 .
AMA StyleNatalia Arroyo-Manzanares, Rosa Peñalver-Soler, Natalia Campillo, Pilar Viñas. Dispersive Solid-Phase Extraction using Magnetic Carbon Nanotube Composite for the Determination of Emergent Mycotoxins in Urine Samples. Toxins. 2020; 12 (1):51.
Chicago/Turabian StyleNatalia Arroyo-Manzanares; Rosa Peñalver-Soler; Natalia Campillo; Pilar Viñas. 2020. "Dispersive Solid-Phase Extraction using Magnetic Carbon Nanotube Composite for the Determination of Emergent Mycotoxins in Urine Samples." Toxins 12, no. 1: 51.
An analytical procedure is proposed for determining three cyanotoxins (microcystin RR, microcystin LR, and nodularin) and two phycotoxins (domoic and okadaic acids) in seawater and algae-based food supplements. The toxins were first isolated by a salting out liquid extraction procedure. Since the concentration expected in the samples was very low, a dispersive liquid–liquid microextraction procedure was included for preconcentration. The ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate (80 mg) was used as green extractant solvent and acetonitrile as disperser solvent (0.5 mL) for a 10 mL sample volume at pH 1.5, following the principles of green analytical chemistry. Liquid chromatography with electrospray ionization and quadrupole time of flight-mass spectrometry (LC-Q-TOF-MS) was used. The selectivity of the detection system, based on accurate mass measurements, allowed the toxins to be unequivocally identified. Mass spectra for quadrupole time of flight-mass spectrometry (Q-TOF-MS) and Q-TOF-MS/MS were recorded in the positive ion mode and quantification was based on the protonated molecule. Retention times ranged between 6.2 and 17.9 min using a mobile phase composed by a mixture of methanol and formic acid (0.1%). None of the target toxins were detected in any of the seawater samples analyzed, above their corresponding detection limits. However, microcystin LR was detected in the blue green alga sample.
Claudia Giménez-Campillo; Marta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Manuel Hernández-Córdoba; Pilar Viñas. Determination of Cyanotoxins and Phycotoxins in Seawater and Algae-Based Food Supplements Using Ionic Liquids and Liquid Chromatography with Time-Of-Flight Mass Spectrometry. Toxins 2019, 11, 610 .
AMA StyleClaudia Giménez-Campillo, Marta Pastor-Belda, Natalia Campillo, Natalia Arroyo-Manzanares, Manuel Hernández-Córdoba, Pilar Viñas. Determination of Cyanotoxins and Phycotoxins in Seawater and Algae-Based Food Supplements Using Ionic Liquids and Liquid Chromatography with Time-Of-Flight Mass Spectrometry. Toxins. 2019; 11 (10):610.
Chicago/Turabian StyleClaudia Giménez-Campillo; Marta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Manuel Hernández-Córdoba; Pilar Viñas. 2019. "Determination of Cyanotoxins and Phycotoxins in Seawater and Algae-Based Food Supplements Using Ionic Liquids and Liquid Chromatography with Time-Of-Flight Mass Spectrometry." Toxins 11, no. 10: 610.
The validation of a procedure for the determination of six alkylphenols (APs), 4-tert-butylphenol, 4-pentylphenol, 4-tert-octylphenol, 4-hexylphenol, 4-octylphenol and 4-nonylphenol, and three bisphenols (BPs), bisphenol A, bisphenol F and bisphenol Z, in seven human organs and tissues (kidney, liver, heart, lung, spleen, brain and abdominal fat) obtained from eight autopsies is presented. Previously ground samples were treated by salt-assisted liquid-liquid extraction (SALLE) for isolation of the analytes and then pre-concentrated using dual stir bar sorptive extraction (SBSE), allowing two different extraction conditions for the same sample. Finally, thermal desorption was used as the injector system in combination with gas chromatography coupled to mass spectrometry (GC-MS). To determine BPs, derivatization using acetic anhydride was required, although this step was not necessary for the APs. Two parallel extractions of the contaminants with the stir bars were performed, followed by thermal desorption and chromatographic analysis. The procedure provided quantification limits between 0.050 and 4.0 ng g−1 for APs and from 0.26 to 2.6 ng g−1 for BPs. Repeatability and reproducibility values were lower than 15% in all cases. The accuracy of the procedure was established by a recovery study, which provided values in the 85.8–115% range for APs and 83.6–120% for BPs. Samples were analyzed with the proposed methodology and data were processed by ANOVA tests to study the behaviour and bioaccumulation of these compounds in human tissues or organs. In addition, discriminant analysis detected age- and sex-dependent differences in bioaccumulation.
Marta Pastor-Belda; Tamara Drauschke; Natalia Campillo; Natalia Arroyo-Manzanares; Carmen Torres; María Dolores Pérez-Cárceles; Manuel Hernández-Córdoba; Pilar Viñas. Dual stir bar sorptive extraction coupled to thermal desorption-gas chromatography-mass spectrometry for the determination of endocrine disruptors in human tissues. Talanta 2019, 207, 120331 .
AMA StyleMarta Pastor-Belda, Tamara Drauschke, Natalia Campillo, Natalia Arroyo-Manzanares, Carmen Torres, María Dolores Pérez-Cárceles, Manuel Hernández-Córdoba, Pilar Viñas. Dual stir bar sorptive extraction coupled to thermal desorption-gas chromatography-mass spectrometry for the determination of endocrine disruptors in human tissues. Talanta. 2019; 207 ():120331.
Chicago/Turabian StyleMarta Pastor-Belda; Tamara Drauschke; Natalia Campillo; Natalia Arroyo-Manzanares; Carmen Torres; María Dolores Pérez-Cárceles; Manuel Hernández-Córdoba; Pilar Viñas. 2019. "Dual stir bar sorptive extraction coupled to thermal desorption-gas chromatography-mass spectrometry for the determination of endocrine disruptors in human tissues." Talanta 207, no. : 120331.
Polycyclic aromatic hydrocarbons (PAHs) are considered xenobiotics of a potentially carcinogenic nature, being accumulated in the fatty tissue of the body. The objective of this work was the development and validation of a new analytical method to check the bioaccumulation of these toxic compounds in human organs obtained from autopsies. The contaminants were first isolated from the tissues by salt-assisted liquid-liquid extraction in acetonitrile. Because of the low concentrations of these compounds in the human body, a dispersive liquid-liquid microextraction procedure was included. The preconcentrated samples were analyzed by gas chromatography-mass spectrometry to identify the compounds. Principal component analysis was applied to show the natural clustering of forensic samples and orthogonal partial least-squares discriminant analysis to develop a multivariate regression method, which permitted the classification of samples. The quantification limits for the 13 PAHs (acenaphthylene, fluorene, phenanthrene, anthracene, pyrene, benzo(a)anthracene, chrysene, benzo(b)fluoranthene, benzo(k)fluoranthene, benzo(a)pyrene, dibenz(a,h)anthracene, benzo(g,h,i)perylene, and indeno(1,2,3-cd)pyrene) analyzed were in the 0.06-0.44 ng g-1 range, depending on the compound, while the mean intraday relative standard deviation of about 7% demonstrated the high precision of the method. Linearity was verified in the 0.5-200 ng g-1 range, and the enrichment factors were between 55 and 122. The results provided by the analysis of seven different human organs (brain, liver, kidney, lung, heart, spleen, and abdominal fat) from eight autopsies confirmed the PAH-bioaccumulation capacity of human body, fat showing the highest degree of bioaccumulation. The present work is the first study on PAH contamination in different organs obtained from autopsies, being PAH detected in most human samples at values ranged from 0 to 19 ng g-1.
Marta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Carmen Torres; María Dolores Pérez-Cárceles; Manuel Hernández-Córdoba; Pilar Viñas. Bioaccumulation of Polycyclic Aromatic Hydrocarbons for Forensic Assessment Using Gas Chromatography–Mass Spectrometry. Chemical Research in Toxicology 2019, 32, 1680 -1688.
AMA StyleMarta Pastor-Belda, Natalia Campillo, Natalia Arroyo-Manzanares, Carmen Torres, María Dolores Pérez-Cárceles, Manuel Hernández-Córdoba, Pilar Viñas. Bioaccumulation of Polycyclic Aromatic Hydrocarbons for Forensic Assessment Using Gas Chromatography–Mass Spectrometry. Chemical Research in Toxicology. 2019; 32 (8):1680-1688.
Chicago/Turabian StyleMarta Pastor-Belda; Natalia Campillo; Natalia Arroyo-Manzanares; Carmen Torres; María Dolores Pérez-Cárceles; Manuel Hernández-Córdoba; Pilar Viñas. 2019. "Bioaccumulation of Polycyclic Aromatic Hydrocarbons for Forensic Assessment Using Gas Chromatography–Mass Spectrometry." Chemical Research in Toxicology 32, no. 8: 1680-1688.
Head-space (HS) gas chromatography (GC) coupled to mass spectrometry (MS) is proposed for the assessment of the contamination of mayonnaise as an alternative to plate counting, which is the technique commonly used for evaluating microbial contamination. More specifically, this method was applied in the detection of Candida metapsilosis and Zygosaccharomyces bailii, both of great importance in term of food spoilage since they are resistant to many of the common methods of food preservation. Different chemometric models were investigated using the data obtained by GC-MS (m/z profile, area of the chromatographic peaks and entire chromatographic profile), in order to obtain the highest classification success. The best results were obtained using the chromatographic profile (success rate of 92%). Contaminated samples could also be classified according to the concentration of yeast, obtaining a success rate of 87.5%. Finally, a chemometric model was constructed in an attempt to differentiate between strains.
N. Arroyo-Manzanares; B. Markiv; J.D. Hernández; I. López-García; I. Guillén; P. Vizcaíno; M. Hernández-Córdoba; P. Viñas. Head-space gas chromatography coupled to mass spectrometry for the assessment of the contamination of mayonnaise by yeasts. Food Chemistry 2019, 289, 461 -467.
AMA StyleN. Arroyo-Manzanares, B. Markiv, J.D. Hernández, I. López-García, I. Guillén, P. Vizcaíno, M. Hernández-Córdoba, P. Viñas. Head-space gas chromatography coupled to mass spectrometry for the assessment of the contamination of mayonnaise by yeasts. Food Chemistry. 2019; 289 ():461-467.
Chicago/Turabian StyleN. Arroyo-Manzanares; B. Markiv; J.D. Hernández; I. López-García; I. Guillén; P. Vizcaíno; M. Hernández-Córdoba; P. Viñas. 2019. "Head-space gas chromatography coupled to mass spectrometry for the assessment of the contamination of mayonnaise by yeasts." Food Chemistry 289, no. : 461-467.