Examinando por Autor "Morante-Zarcero, Sonia"

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2-Mercaptopyrimidine-functionalized mesostructured silicas to develop electrochemical sensors for a rapid control of scopolamine in tea and herbal tea infusions
(Elsevier, 2020) Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
Mesostructured silicas were synthesized and chemically functionalized with a 2- mercaptopyrimidine (MPY)-derivative. Bare and functionalized silicas (MSU-2, HMS, SBA-15, MSU-2-MPY, HMS-MPY and SBA-15-MPY) were characterized by powder X-ray diffraction, nitrogen adsorption-desorption isotherms, transmission electron and scanning electron microscopy, 29Si and 13C cross-polarization magic-angle spinning NMR spectroscopy and elemental analysis, and used to prepare modified carbon paste electrodes (CPEs). The electrodes properties were studied using potassium ferrocyanide and scopolamine as probes employing cyclic voltammetry (CV) and differential pulse voltammetry (DPV). Results proved that MPY groups on the silica surface were necessary to improve the sensitivity in the voltammetric determination of scopolamine. CPE modified with HMS-MPY exhibited higher peak current toward the oxidation of scopolamine, with a well-defined oxidation peak at + 1.1 V (vs. Ag/AgCl) in DPV. This fact can be attributed to the high electroactive area of this material, with 3 D wormholelike channel structure that favored the scopolamine diffusion. Under optimum conditions, HMS-MPY-CPE exhibited a wider linearity range, from 0.9 to 200 μM, with a detection limit of 0.3 μM and good reproducibility by DPV. The developed sensor was successfully applied for a rapid determination of scopolamine in spiked tea and herbal tea infusion samples with good recoveries (between 83 ± 5 and 101 ± 1%).
A comparative study of phenolic composition and antioxidant activity in commercial and experimental seedless table grapes cultivated in a Mediterranean climate
(Springer, 2021-01) Izcara, Sergio; Morante-Zarcero, Sonia; Andrés, María Teresa de; Arroyo, Teresa; Sierra, Isabel
Grapes are important sources of phenolic compounds, which have multiple beneficial effects on human health. Scientific advances in the field of genetics have allowed the production of seedless table grape varieties, which are highly demanded by consumers because of their nutritional value and their easy consumption. In this study, total phenolic content (TPC), radical scavenging activity (RSA) and total anthocyanin content (TAC), were determined in 65 seedless table grape varieties (41 experimental and 24 commercial varieties). Ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) was used to identify and quantify some phenolic acids, flavan-3-ols, flavonols and stilbenes in 14 experimental varieties. TPC ranged from 17 to 250 mg gallic acid equivalents/100 g fresh weight (FW), RSA ranged from 15 to 269 mg Trolox equivalents/100 g FW and TAC ranged from 0 to 168 mg cyanidin-3-glucoside/100 g FW. The RSA assay showed high correlation (R2 = 0.90) between the TPC and the antioxidant activity of the 65 seedless table grapes analyzed. In the vast majority of the new experimental varieties analyzed, the TPC and TAC were similar to those of some common table grapes with seeds, indicating promising perspectives for their commercialization as potential sources of these bioactive compounds. In 6 grape varieties, high concentrations of catechin, procyanidin B2, epicatechin, quercetin 3-β-D-glucoside, 4-hydroxybenzoic acid, vanillic acid, caftaric acid and rutin were found, which would indicate that the regular intake of these varieties would be highly recommended.
A disposable electrochemical sensor based on bifunctional periodic mesoporous organosilica for the determination of lead in drinking waters
(Springer Verlag, 2015-07) Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
A new bifunctional disulfide- and tetrasulfide-bridged periodic mesoporous organosilica (PMO) with mercaptothiazoline ligand was synthesized and employed to prepare chemically modified carbon paste electrodes for Pb(II) detection in aqueous media by square wave adsorptive stripping voltammetry. To demonstrate the real interest of bifunctionalization, carbon paste electrodes were prepared with disulfide- and tetrasulfide-bridged PMO without mercaptothiazoline ligand. Results showed the importance of bifunctionalization of PMOs to improve the sensitivity for the determination of Pb(II) in water samples. To achieve the most accurate and sensitive Pb(II) measurements, optimization of the operating parameters in preconcentration and detection steps was performed. Finally, the modified carbon paste electrode prepared with bifunctional disulfide-bridged PMO with mercaptothiazoline ligand was applied to determine Pb(II) in different water samples without any pre-treatment. Using this electrode, the optimal operating conditions were 120 s of electrolysis time in HCl 0.4 M. In these conditions, the voltammetric signal increased linearly with the preconcentration time from 1 to 10 min. Under optimized conditions, the linear range was 2 - 100 ¿g/L (R2 = 0.9943) with a detection limit of 0.5 ¿g/L (for 5 min preconcentration time). Good reproducibility was achieved on both single and equally prepared electrodes. The accuracy of the method was validated by analysing Pb(II) in different drinking and natural water samples, with spiked recoveries in the range of 95 ¿ 105 ± 10%. The results demonstrated that the prepared electrochemical sensor exhibited selectivity, fast response time and exceptional long-time stability.
A Miniaturized QuEChERS Method Combined with Ultrahigh Liquid Chromatography Coupled to Tandem Mass Spectrometry for the Analysis of Pyrrolizidine Alkaloids in Oregano Samples
(MDPI, 2020) Izcara, Sergio; Casado, Natalia; Morante-Zarcero, Sonia; Sierra, Isabel
Recent and unexpected food alerts about relatively high amounts of pyrrolizidine alkaloids in oregano samples have stressed the need to develop analytical strategies to ensure food safety in this type of foodstu . Accordingly, this work presents the development of a miniaturized strategy based on the QuEChERS (quick, easy, cheap, e ective, rugged and safe) method combined with ultrahigh liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) for the determination of 21 pyrrolizidine alkaloids suggested by the European Food Safety Authority to be monitored in food. The analytical method was properly validated, with overall average recoveries from 77 to 96% and relative standard deviations <13% (n = 9). The method proved to be a sustainable analytical strategy which meets green analytical chemistry principles as it showed good performance by using small amounts of sample (0.2 g), organic solvents (1000 L), clean-up sorbents (175 mg) and partitioning salts (0.65 g). Its feasibility was verified through the analysis of 23 oregano samples. Of the samples analyzed, 100% were contaminated, with an average concentration of 1254 g/kg. Lasiocarpine, lasiocarpine N-oxide, europine, europine N-oxide, senecivernine, senecionine, echimidine N-oxide, lycopsamine N-oxide and intermedine N-oxide were the alkaloids which significantly contributed to the contamination of the samples.
A novel hybrid mesostructured silica for the solid-phase extraction of estrogenic hormones from waters
(Royal Society of Chemistry, 2015-04) Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
Mesoporous silica functionalized with octadecyl groups (denoted as SBA-15-C18) was prepared and characterized. The adsorption capacity of the prepared SBA-15-C18 for a mixture of twelve endocrine disrupting compounds (synthetic and natural estrogenic hormones) in aqueous media was evaluated by off-line solid-phase extraction (SPE) and compared with a commercial phase for SPE (ExtraBondR C18). Analytes were determined by high performance liquid chromatography with UV-Vis detection. Under optimized conditions (100 mg of SBA-15-C18 sorbent; conditioning: 2 mL methanol and 2 mL Milli-Q water; loading: 150 mL water sample; washing: 5 mL Milli-Q water; elution: 2 mL methanol; flow rate 0.5 mL min-1) the preconcentration factor achieved was 103. The analytical characteristics of this methodology were evaluated, showing good precision, accuracy and linerarity, with method quantification limits (MQL) between 0.16 and 3-00 ¿g L-1. The SBA-15-C18 material enabled the extraction of the twelve estrogenic hormones in tap water (pH 6.6), mineral water (pH 5.0), ground water (pH 7.3), river water (pH 5.0) and effluent wastewater (pH 5.0) with recoveries between 71 and 112% at the lower level studied (MQL).
A simple and sensitive portable system for a rapid evaluation of bisphenol A contamination in potable and environmental waters using a mesoporous silica-modified carbon paste electrode
(Taylor & Francis, 2019-04-29) Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Gañán, Judith; Sierra, Isabel
In this work, two ordered mesoporous silicas (HMS and SBA-15) were prepared and incorporated into carbon paste electrodes (CPEs) to obtain mesostructured sensors for a rapid determination of bisphenol A (BPA) in waters by voltammetric techniques. The materials were characterised by nitrogen adsorption-desorption measurements, transmission electron microscopy and scanning electron microscopy. The electrochemical properties of the modified carbon paste electrodes were studied by differential pulse voltammetry (DPV) and cyclic voltammetry (CV). Results showed that the sensor modified with HMS (HMS-CPE) exhibited strong adsorption activity toward the oxidation of BPA, with a welldefined voltammetric peak at +0.6 V. Moreover, the HMS-CPE exhibited a wider linearity range, from 0.44 to 3.5 μM BPA, with a detection limit of 61 nM (S/N = 3) and good reproducibility by DPV. The enhanced performance of the HMS-CPE could be attributed to its high surface area, with a 3 D wormhole-like channel structure that favoured an excellent accessibility, high adsorption capacity and faster adsorption rate of BPA. This novel sensor was coupled to a portable system and successfully applied for a rapid determination of BPA in tap, mineral, well and river water samples with good recovery, ranging from 98 ± 12 to 103 ± 7%.
Active digital learning to enhance practical skills and motivation of students in a coordinated manner across subjects related to food analysis
(IATED, 2024) Morante-Zarcero, Sonia; Casado, Natalia; Casado-Hidalgo, Gema; Fernández-Pintor, Begoña; Gañán, Judith; González-Gómez, Lorena; Martínez-García, Gonzalo; Martínez-García, Isabel; Pérez-Quintanilla, Damián; Rodríguez-Castaño, Jesús; Sierra, Isabel; Vera-Baquero, Fernando L.
Nowadays, the task of inspiring student engagement and motivation remains a challenge in the field of higher education. For this reason, active learning methodologies are becoming increasingly common, especially in the science and technology educational field, which requires practical demands and a wide range of skills. In this context gamification stands out as an interesting innovative educational tool, which promotes active student participation, amplifies the practical application of knowledge, boosts motivation and offers a more accurate assessment of student understanding. Moreover, this educational resource combines the use of information and communication technologies (ICTs), teamwork and learning [1]. This study describes an active digital learning initiative implemented through virtual education at the Rey Juan Carlos University during the 2023-2024 academic year. The experience was carried out in a coordinated way between two different subjects of 2nd course of the Food Science and Technology degree: Food Analysis Techniques and Food Chemistry. Nonetheless, the learning acquired with the activity can be useful for other interrelated subjects, such as: Analysis and Quality Control of Foods (3rd course), Analytical Control of Contaminants in Food and Technology and Characterization of Dairy Products (4th course). The experience was designed as a mandatory activity prior to the laboratory practices. It involved a virtual tour performed through the Genially online tool. This tour encompassed a detailed exploration of the facilities and key equipment within the three laboratories where the students conduct their laboratory practices. It also included fundamental procedures which are essential for conducting experiments in food analysis. Likewise, throughout the tour, the students had to overcome different challenges and quizzes related to the information displayed on the tour (i.e., identify primary glassware and instrumental equipment, quality and types of chemical reagents degrees, chemical waste disposal management, recognize the arrangement of a sensory analysis laboratory, etc.). There was a total of 34 challenges within the tour which scored up to 9 points. Once the activity was finished, a satisfaction survey was conducted to the students. Filling out this survey added one more point to the score. The average score obtained by the students in the activity was a 7.8, what reveals that most of the students were able to successfully complete the activity and achieve a good score. Additionally, the students valued the activity positively, highlighting it usefulness and its ability to improve motivation for practical work. Finally, once the laboratory practices were performed, a new survey was conducted to assess the impact of the activity in the students. 71% of the students believed the activity has helped them to face the laboratory practices since they had a better understanding of the organization in the laboratory. The laboratory teachers also observed an improvement and recommended conducting the activity before entering the laboratories in other subjects or programs. Overall, the positive grades and evaluations obtained from both students and teachers confirm that the proposed activity enhances practical skills and student motivation.
Advances in Greener and Sustainable Sample Preparation for Tropane Alkaloid Analysis in Foods
(Springer, 2025-02-07) González-Gómez, Lorena; Fernández-Pintor, Begoña; Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
In the current context, Green Analytical Chemistry (GAC) focuses on promoting analytical methods that are more efficient and environmentally friendly. One of the fundamental principles of GAC is to reduce or eliminate the use of hazardous substances and minimize waste generation. One of the ways to achieve this is through the adoption of direct analytical techniques that can omit the sample preparation step. However, in the case of the determination of natural toxins, such as tropane alkaloids (TAs), carrying out direct analysis can be difficult due to several factors. For example, these compounds are often present in foods of plant origin with very complex matrices, in low concentrations, which makes their direct detection and quantification difficult. Therefore, in this context, sample preparation remains essential to clean up extracts and to concentrate analytes prior to their analysis. This chapter highlights the crucial importance of sample preparation in the determination of TAs. It emphasizes the fundamental role of miniaturized techniques and new materials applied in such techniques, which can contribute significantly to the search for more sustainable analytical practices. In this sense, an evaluation is carried out using the AGREEprep metric to analyze the miniaturized methods already published. This metric allows for a systematic evaluation of sample preparation methods in terms of their efficiency, sustainability, and compliance with the principles of Green Sample Preparation (GSP), which arises to better the principles of GAC. Positive and negative points of existing methods are identified, and possible modifications are suggested to improve their performance and make sample preparation greener.
Analytical Strategies for Green Extraction, Characterization, and Bioactive Evaluation of Polyphenols, Tocopherols, Carotenoids, and Fatty Acids in Agri-Food Bio-Residues
(MDPI, 2025-03-15) Vicente-Zurdo, David; Gómez-Mejía, Esther; Morante-Zarcero, Sonia; Rosales-Conrado, Noelia; Sierra, Isabel
Recent advancements in analytical strategies have enabled the efficient extraction and characterization of bioactive compounds from agri-food bio-residues, emphasizing green chemistry and circular economy principles. This review highlights the valorization of several agri-food bio-residues for the extraction of high-value-added bioactive compounds, particularly polyphenols, tocopherols, carotenoids, and fatty acids, as a biorefinery approach. To this end, the adoption of environmentally friendly extraction technologies is essential to improve performance, reduce energy consumption, and minimize costs. This study therefore examines emerging methodologies such as supercritical fluid extraction, pressurized liquid extraction, pulsed electric fields, and matrix solid-phase dispersion, highlighting their advantages and limitations. Additionally, the chemical characterization of these bioactive compounds is explored through spectrophotometric and high-resolution chromatographic techniques, crucial for their accurate identification and quantification. This is complemented by an analysis of bioactivity assays evaluating antioxidant, antimicrobial, anticancer, neuroprotective, and anti-inflammatory properties, with a focus on their applications in the food, pharmaceutical, and cosmetic industries. However, the analytical control of toxic compounds, such as alkaloids, in these bio-residues is undoubtedly needed. Ultimately, this approach not only promotes sustainability but also contributes to the development of eco-friendly solutions in various industries
Application of a hybrid large pore mesoporous silica functionalized with β-cyclodextrin as sorbent in dispersive solid-phase extraction. Toward sustainable sample preparation protocols to determine polyphenolic compounds in Arbutus unedo L. fruits by UHPLC-IT-MS/MS
(Elsevier, 2023-01) Izcara, Sergio; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
A quick, sensitive and selective analytical reversed-phase method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) was employed for the simultaneous determination of nine phenolic compounds (PCs) in strawberry tree (SBT) berries. The sample treatment included a solid-liquid extraction followed by a dispersive solid-phase extraction (dSPE) procedure using a hybrid large pore mesoporous silica (LP-MS) functionalized with β-cyclodextrin (β-CD) as sorbent material. For this purpose, the initial synthesized LP-MS was modified with β-CD following three different synthetic routes, obtaining three new functionalized materials (denoted LP-MS-β-CD-R1, LP-MS-β-CD-R2 and LP-MS-β-CD-R3). All synthesized materials were comprehensively characterized, showing excellent textural properties, and they were also tested as sorbent materials in the extraction of PCs by comparison of SPE and dSPE procedures. The LP-MS- β-CD-R2 as sorbent material in the dSPE procedure showed the best potential to extract and purify the target PCs, being more effective than the other materials and compared with the SPE procedure. The performance of the proposed dSPE-UHPLC-IT-MS/MS method was validated in terms of selectivity, linearity, LOD, LOQ, trueness, precision, and matrix effect, achieving good analytical method performance and demonstrating its feasibility and practicality for the quantification of PCs in SBT fruits. The analysis of the investigated SBT berries revealed, mainly, high contents of arbutin reaching concentrations up to 5979 μg/g dry weight, followed by catechin (661 μg/g dry weight). Arbutin was, undoubtedly, the major PC determined in all SBT berry samples analyzed, being the most prominent and showing a high concentration compared to that of other polyphenols determined in other red berries.
Application of a hybrid ordered mesoporous silica as sorbent for solid-phase multi-residue extraction of veterinary drugs in meat by ultra-high-performance liquid chromatography coupled to ion-trap tandem mass spectrometry
(Elsevier, 2016-06) Casado, Natalia; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
A quick, sensitive and selective analytical reversed-phase multi-residue method using ultra-high performance liquid chromatography coupled to an ion-trap mass spectrometry detector (UHPLC-IT-MS/MS) operating in both positive and negative ion mode was developed for the simultaneous determination of 23 veterinary drug residues (ß-blockers, ß-agonists and Non-Steroidal Anti-inflammatory Drugs (NSAIDs)) in meat samples. The sample treatment involved a liquid-solid extraction followed by a solid-phase extraction (SPE) procedure. SBA-15 type mesoporous silica was synthetized and modified with octadecylsilane, and the resulting hybrid material (denoted as SBA-15-C18) was applied and evaluated as SPE sorbent in the purification of samples. The materials were comprehensively characterized, and they showed a high surface area, high pore volume and a homogeneous distribution of the pores. Chromatographic conditions and extraction procedure were optimized, and the method was validated according to the Commission Decision 2002/657/EC. The method detection limits (MDLs) and the method quantification limits (MQLs) were determined for all the analytes in meat samples and found to range between 0.01-18.75 ¿g/Kg and 0.02-62.50 ¿g/Kg, respectively. Recoveries for 15 of the target analytes ranged from 71-98%. In addition, for comparative purpose SBA-15-C18 was evaluated towards commercial C18 amorphous silica. Results revealed that SBA-15-C18 was clearly more successful in the multi-residue extraction of the 23 mentioned analytes with higher recovery values. The method was successfully tested to analyze prepacked preparations of mince bovine meat. Traces of propranolol, ketoprofen and diclofenac were detected in some samples.
Application of the QuEChERS Strategy as a Useful Sample Preparation Tool for the Multiresidue Determination of Pyrrolizidine Alkaloids in Food and Feed Samples: A Critical Overview
(MDPI, 2022) Casado, Natalia; Morante-Zarcero, Sonia; Sierra, Isabel
The identification of concerning high levels of pyrrolizidine alkaloids (PAs) in a wide variety of food products has raised the occurrence of these natural toxins as one of the main current issues of the food safety field. Consequently, a regulation with maximum concentration levels of these alkaloids has recently been published to monitor their occurrence in several foodstuffs. According to legislation, the analytical methodologies developed for their determination must include multiresidue extractions with high selectivity and sensitivity, as a set of 21 + 14 PAs should be simultaneously monitored. However, the multiresidue extraction of these alkaloids is a difficult task due to the high complexity of food and feed samples. Accordingly, although solid-phase extraction is still the technique most widely used for sample preparation, the QuEChERS method can be a suitable alternative for the simultaneous determination of multiple analytes, providing green extraction and clean-up of samples in a quick and cost-effective way. Hence, this review proposes an overview about the QuEChERS concept and its evolution through different modifications that have broadened its applicability over time, focusing mainly on its application regarding the determination of PAs in food and feed, including the revision of published works within the last 11 years.
Assessment of atropine and scopolamine in commercial multigrain cereal-based baby products using UHPLC-TQ-MS/MS and solid phase extraction with MCM-41 mesostructured silica as sorbent
(Elsevier, 2025-04-30) Vera-Baquero, Fernando L.; Pérez-Quintanilla , Damián; Morante-Zarcero, Sonia; Sierra, Isabel
A sample preparation procedure for the analysis of tropane alkaloids (atropine and scopolamine) in multigrain cereal-based baby products (MGBP) has been optimized in this study. The protocol was based on a solid-liquid extraction, followed by purification by solid-phase extraction with MCM-41 functionalised with sulphonic acid groups as sorbent, before the analysis by ultra-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The method was successfully validated with limits of quantification of 0.005 and 0.05 μg/kg for atropine and scopolamine, respectively. The analysis of a quality control material (TAs in baby food multigrain) demonstrated the suitability for the purpose of the methodology. The analysis of twenty commercial MGBP (mixtures of 2 to 10 cereal flours, with honey, milk, fruit pulp or juices) purchased between 2016 and 2024, revealed the presence of atropine (between 0.07 and 1.0 μg/kg) and scopolamine (between 0.15 and 12 μg/kg) in all the MGBP analysed.
Atropine and scopolamine occurrence in spices and fennel infusions
(Elsevier, 2022-12-03) González-Gómez, Lorena; Gañán, Judith; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
Tropane alkaloids (TAs) are toxic anticholinergic compounds that appear due to accidental contamination of foods with TA-producing plants. Atropine and scopolamine are the most common TAs and their maximum levels in certain foodstuffs have been recently regulated, including food supplements. TAs occurrence in commercial products and the transfer ratio to herbal infusions prepared from contaminated spices are of interest for exposure assessment of consumers. In this study, the occurrence of atropine and scopolamine was investigated in a total of 51 commercial spices of 6 types (ginger, cloves, fennel, cumin, aniseed, coriander) and a mix of spices and herbs (curry) purchased in Portugal (19 samples) and Spain (32 samples) in 2021. Results evidenced that more than half of the samples analysed (67%) were contaminated with one or both analytes. Fennel, cloves and coriander showed the highest concentrations ranging between 5-31 μg/kg, 8–28 μg/kg and 5–45 μg/kg, respectively, for the sum of atropine and scopolamine. On the other hand, the transfer ratio of the target analytes found in four naturally contaminated fennel samples was studied. Infusions were prepared according to International Standard ISO 3103 protocol, and a transfer ratio between 64 and 88% for atropine and between 47 and 57% for scopolamine was found.
Bi-functionalized mesostructured silicas as reversed-phase/strong anion-exchange sorbents. Application to extraction of polyphenols prior to their quantitation by UHPLC with ion-trap mass spectrometry detection
(SpringerLink, 2019-02-06) Casado, Natalia; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel
Hybrid mesostructured silicas with wormhole-like pore structure were synthesized and bi-functionalized with n-octyl (C8) and quaternary ammonium (NR4+) groups to obtain new sorbent materials for dispersive solid-phase extraction (dSPE) of polyphenols. Due to their nature of being both a reversed-phase and a strong anion-exchanger, the materials display mixed mode retention mechanism. During the synthesis, the functionalization conditions were varied to obtain materials with different functionalization degree. The resulting materials (denoted as HMS-RPC8-SAX-1, HMS-RPC8-SAX-2 and HMS-RPC8-SAX-3) show high surface area, wormhole-like framework and controlled pore size. They were evaluated for multicomponent extraction of 22 polyphenols, including phenolic acids, flavonoids and stilbenes, from spiked juice samples. The sample extracts were analyzed by ultra-high performance liquid chromatography coupled to ion-trap tandem mass spectrometry. The adsorption capability, the amount of sorbent, the eluent and the elution volume were optimized. Best performance was achieved by using HMS-RPC8-SAX-2, which is the material with the highest fraction of NR4+ groups. This material has a large extraction capability and provides high recovery values of the target analytes (70–101%) as a result of its hydrophobic and anion-exchange interactions. The detection limits for polyphenols in juice range from 1 to 560 ng mL−1.
Creación de un diario de misión digital basado en la superación de distintos retos para mejorar el rendimiento académico de los estudiantes del grado en Ciencia y Tecnología de los Alimentos
(Universitat Politècnica de València, 2023-07-13) Casado, Natalia; Gañán, Judith; González-Gómez, Lorena; Casado-Hidalgo, Gema; Morante-Zarcero, Sonia
Este trabajo describe la implantación de una actividad de innovación docente basada en la metodología activa de la gamificación dentro del grado en Ciencia y Tecnología de los Alimentos de la Universidad Rey Juan Carlos durante el curso académico 2022-2023. La actividad se realizó en la asignatura de Análisis y Control de la Calidad de los Alimentos de 3º curso de forma voluntaria para conseguir una puntuación extra en la calificación final. El principal objetivo fue incentivar el estudio, la motivación y el trabajo autónomo de los estudiantes. Para ello, la actividad consistió en la creación de un diario de misión digital por parte de cada estudiante basado en la superación de un conjunto de retos relacionados con la técnica de extracción en fase sólida en el análisis de alimentos. Estos retos formaban parte de un itinerario formativo con distintos niveles que debían ir superando semana a semana. Los resultados obtenidos demuestran una mejora del rendimiento académico de los estudiantes participantes, los cuales al realizar la actividad también han desarrollado competencias generales y específicas útiles para mejorar la compresión de otras asignaturas del grado y para abordar su Trabajo Fin de Grado.
Current development and applications of ordered mesoporous silicas and other sol-gel silica-based materials in food sample preparation for xenobiotics analysis
(Elsevier, 2017) Casado, Natalia; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel
In the last years, sample preparation has been playing an important role in the analysis of xenobiotics in complex matrices, such as food samples. Recent advances in the development of new materials, such as ordered mesoporous silicas (OMSs) and other sol-gel silica-based materials, have gained increasing research interest in sample preparation and analytical chemistry due to their desirable characteristics and advantages versus traditional and commercial sorbents, since they enhance the analytical performance of many existing techniques or allow new ones to be developed. The aim of this review is to provide an overview with the most relevant achievements in the preparation and functionalization of OMSs and other sol-gel organic-inorganic hybrid silicas, and to give some recent examples from the last six years (from 2010 to 2016) regarding the analytical applications of these materials in sample preparation and extraction of xenobiotics from food products, including beverages and drinking water samples.
Design and Optimisation of Sustainable Sample Treatments Based on Ultrasound-Assisted Extraction and Strong Cation-Exchange Purification with Functionalised SBA-15 for Opium Alkaloids in Ground Poppy Seeds
(MDPI, 2023-11-24) Casado-Hidalgo, Gema; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Sierra, Isabel
An analysis methodology was optimised and validated for the quantification of opium alkaloids (OAs) in ground poppy seeds. This involved ultrasound-assisted extraction (UAE) and solid-phase extraction (SPE) purification before analysis using a high-performance liquid chromatography mass spectrometry detector (HPLC-MS/MS). UAE was optimised through the design of experiments with three factors and a three-level full factorial design. For SPE optimisation, a commercial material was compared with a previously synthesised material of SBA-15 silica functionalised with sulfonic groups (SBA-15-SO3-). The synthesised material demonstrated superior efficiency with only 25 mg and proved to be reusable for up to four cycles. The methodology was properly validated in terms of linearity, limits of detection and quantification, and selectivity. Matrix effects were negligible; adequate recovery values (85–100%) and inter-day and intra-day precision (<15%) were obtained. The greenness of the method was evaluated with the AGREEprep metric scale, being more environmentally friendly compared to OA analysis methods. Finally, the method was applied to different samples of ground poppy seeds and revealed a concentration of 140 mg/kg of morphine equivalents in one of the samples, surpassing the legislatively established limits by seven fold. This highlights the need to analyse these types of samples to mitigate potential public health issues.
Determination of atropine and scopolamine in honey using a miniaturized polymer-based solid-phase extraction protocol prior to the analysis by HPLC-MS/MS
(Elsevier, 2024-03-10) Fernández-Pintor, Begoña; Paniagua, Gema; Gañán, Judith; Morante-Zarcero, Sonia; Garcinuño, Rosa María; Fernández, Pilar; Sierra, Isabel
Two homopolymers have been prepared employing methacrylic acid and 4-vynylpiridine as functional monomers (p-MAA, p-4-VP) through an easy and quick precipitation polymerization method for application as sorbents in solid-phase extraction (SPE) to determine atropine and scopolamine in honey. The optimized SPE conditions were as follows: 25 mg of p-MAA, 4 mL of sample loading volume (diluted honey 1:10 with water), 4 mL of elution solvent (methanol/water with 1 % formic acid, 80/20, v/v). The extracts were analyzed by HPLC-MS/MS. The cartridges were reusable for forty cycles demonstrating an environmentally friendly approach. The methodology was validated in terms of linearity, accuracy, precision, selectivity, matrix effect and sensibility, highlighting the absence of matrix effect. The miniaturized polymer-based SPE was successfully applied to fifteen honeys, showing concentrations up to 7.23 ng/g in the most contaminated honey. All quantified honey samples (5 in total) were of multifloral type.
Development and Characterization of SBA-15 Imprinted Polymers for Spiramycin Analysis
(MDPI, 2024-08-15) González-Gómez, Lorena; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Paniagua González, Gema; Garcinuño, Rosa M.; Fernández Hernando, Pilar; Sierra, Isabel
This work focuses on the development of a hybrid material based on SBA-15 silica with a molecularly imprinted polymer (MIP), using spiramycin (SPI) as a template, for use as sorbent in solid-phase extraction (SPE). Characterization techniques such as nitrogen gas adsorption–desorption isotherms, infrared spectroscopy and scanning electron microscopy confirmed the structure and properties of the SBA-15@MIP-SPI material. SPE conditions using SBA-15@MIP-SPI as sorbent were optimized, which allowed us to demonstrate the high selectivity and adsorption capacity of SPI on the synthesized material. The best conditions were 50 mg of sorbent, loading with 1 mL of standard solution or sample of cow milk previously extracted in acetonitrile and eluting with 3 mL of methanol with 1% acetic acid. After the optimization process, the material demonstrated recovery percentages of 81 ± 3% in SPI standard solutions and showed its potential in cow milk samples (71 ± 6%). The novelty of the research consists of the combination of MIPs with SBA-15, which could offer important advantages in terms of specific surface area and porous structure, thus improving performance and reducing the amount of sorbent compared to other traditional methods.