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%.
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.
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.
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.
Development of a Green, Quick, and Efficient Method Based on Ultrasound-Assisted Extraction Followed by HPLC-DAD for the Analysis of Bioactive Glycoalkaloids in Potato Peel Waste
(MDPI, 2024-02-21) Martínez-García, Isabel; Gaona-Scheytt, Carlos; Morante-Zarcero, Sonia; Sierra, Isabel
α-Solanine and α-chaconine are the two most predominant glycoalkaloids (GAs) present in potato. Potato peel contains a high concentration of GAs, which are especially interesting for application in the pharmaceutical industry due to their different beneficial properties (such as anticarcinogenic, anti-inflammatory, antiallergic, antipyretic, antiviral, fungicide, and antibiotic activities, among others); so, potato peel waste can be valorized by extracting these biologically active compounds. For this, a green, quick, and efficient miniaturized analytical approach based on ultrasound-assisted extraction (UAE) combined with HPLC-DAD was developed to quantify α-solanine and α-chaconine in potato peel. Some parameters of the extraction were optimized, including the extraction method, the type of solvent, and the sample/solvent ratio, by a three-factor, three-level (33 ) full factorial experimental design. The optimal extraction conditions were obtained with UAE using methanol as a solvent and a sample/solvent ratio of 1:10 (w/v, g/mL). The analytical greenness metric for sample preparation (AGREEprep) tool was used to assess the greenness of the methods used. The tool revealed an acceptable green analysis, with 0.61 points. The method was validated and applied to the evaluation of GAs in the peel of 15 commercial varieties of potato. The amount of glycoalkaloids found in the samples evaluated ranged from 143 to 1273 mg/kg and from 117 to 1742 mg/kg dry weight for α-solanine and α-chaconine, respectively. These results reveal the important variability that exists between potato varieties; so, their analysis is of great importance to select the most suitable ones for biovalorization (e.g., the Amandine and Rudolph varieties, with around 3000 mg/kg, in total, of both GAs). To provide higher stability to the peel during storage, freeze-drying or a medium-temperature drying process resulted preferable to avoid GA degradation. Overall, this study will contribute to the expansion of the future biovalorization of potato peel waste as well as provide a powerful analytical tool for GA analysis.
Development of Gluten-Free Bread Based on Maize and Buckwheat and Enriched with Aromatic Herbs and Spices
(MDPI, 2024-04-16) Ruiz-Aceituno, Laura; Casado, Natalia; Arriero-Romo, Emma; Morante-Zarcero, Sonia; Lázaro, Almudena; Sierra, Isabel
This work aimed to develop high-quality gluten-free bread based on maize and buckwheat with good palatability and texture properties. Different aromatic herbs and spices were incorporated as ingredients to evaluate whether their addition could influence the acceptability of consumers by improving the sensory properties of the final product. The bread formulation was first optimized through a response surface methodology. Accordingly, high specific volume, high springiness, and low hardness provided the best theoretical bread quality. However, when developing the product, some sensory defects were detected. Therefore, the addition of other ingredients (e.g., oil, sugar, and yeast) was tested. Finally, five different gluten-free bread with different combinations of aromatic herbs and spices were obtained. They were nutritionally characterized and subjected to sensory analysis by a panel of 140 consumers. The chemical composition of all bread was very similar, with only slight differences among them. Likewise, all of them received acceptable sensory scores (>5) from consumers, and some combinations of herbs and spices obtained scores higher than in the control bread (without herbs and spices). Overall, the gluten-free bread formulated with the combination of basil and oregano was the one that consumers significantly liked the most.
Dispersive solid-phase extraction of polyphenols from juice and smoothie samples using hybrid mesostructured silica followed by ultra-high-performance liquid chromatography-ion-trap tandem mass spectrometry
(ACS publications, 2018-12-20) Casado, Natalia; Morante-Zarcero, Sonia; Perez-Quintanilla, Damián; S. Câmara, José; Sierra, Isabel
A wormhole-like mesostructured silica was synthesized and modified with octadecylsilane (C18) groups. The resulting hybrid material (HMS-C18) was characterized and evaluated as sorbent for simultaneous extraction of 20 polyphenols from mixed fruit-vegetables juices and smoothies by dispersive solid-phase extraction (dSPE). The samples were first subjected to solvent extraction followed by dSPE procedure. The extraction step was optimized and combined with a reversed-phase ultra-high-performance liquid chromatography method coupled to ion-trap tandem mass spectrometry (UHPLC-IT-MS/MS), which was also optimized. HMS-C18 showed high potential to extract and purify the target analytes, being more effective than commercial C18 amorphous silica. The proposed method was validated for both samples, obtaining average recoveries from 57-99% with relative standard deviations lower than 9%. Its applicability in the analysis of commercial mixed fruit-vegetables juices and smoothies revealed mainly contents of rutin, 4-hydroxybenzoic acid, chlorogenic acid, epicatechin, caffeic acid and naringin in the samples analyzed
Environmental chiral analysis of β-blockers: Evaluation of different n-alkyl-modified SBA-15 mesoporous silicas as sorbents in solid phase extraction
(CSIRO PUBLISHING, 2018) Silva, Mariana; Morante-Zarcero, Sonia; Pérez-Quintanilla, Damián; Marina, M.L.; Sierra, Isabel
The extraction and preconcentration of chiral β-blockers in environmental water was evaluated by solid-phase extraction (SPE) employing an SBA-15 ordered mesoporous silica functionalised with alkyl chains of different length. The materials were characterised by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption isotherm measurements and elemental analysis. Important parameters influencing extraction efficiency, including the type and amount of sorbent and the breakthrough volume, were optimised. The results obtained showed that the organic chain length played an important role in the behaviour of these sorbents. Under optimised conditions, using 200 mg SBA-15-C8 as sorbent, a simple analytical method based on off-line SPE coupled to chiral capillary electrophoresis with diode array detection (SPE-chiral CE-DAD) was developed. Method detection and quantification limits were lower than 0.6 and 1.9 µg L −1 respectively for all enantiomers, with a preconcentration factor of 500-fold. The method was successfully applied to the chiral analysis of atenolol, metoprolol, pindolol and propranolol in river and sewage water samples. Satisfactory recoveries (between 86 ± 2 and 98 ± 1 %) and repeatability (relative standard deviation (RSD) < 9 %, n = 3) were obtained. Metoprolol was detected in sewage water at a concentration of 10.7 and 9.9 µg L−1 and an enantiomeric fraction of 0.52 and 0.48 for the first- and the second-migrating enantiomers respectively. These results emphasise the importance of enantioselective analysis for environmental risk assessment.
Evaluating the stability of tropane and opium alkaloids during baking in homemade gluten-free poppy seed crackers
(Elsevier, 2024-12) González-Gómez, Lorena; Casado-Hidalgo, Gema; Gañán, Judith; Pérez-Quintanilla, Damián; Morante-Zarcero, Sonia; Sierra, Isabel
Nowadays, alternative flour to wheat, such as teff and corn are increasingly used in gluten-free bakery products, and seeds, such as poppy seeds (whole or ground) are added for their beneficial nutritional properties. However, these ingredients may be contaminated with natural toxins such as tropane (TAs) and opium (OAs) alkaloids. To reduce toxin exposure, it is essential to assess their thermal degradation during baking. The study aimed to quantify TAs and OAs in doughs before and after baking to evaluate their degradation while preparing homemade gluten-free ground poppy seed crackers. To achieve this, a novel methodology involving solid-liquid extraction (SLE) and solid-phase extraction (SPE) with a bifunctionalized mesostructured silica SBA-15 sorbent (50 mg), followed by UHPLC-MS/MS analysis, was developed and validated. The method validation showed good linearity (R2 ≥ 0.991), precision (%RSD ≤17%), accuracy (88–104% for TAs and 79–106% for OAs), and low quantification limits (0.6–1.1 μg/kg for TAs and 0.06–0.46 mg/kg for OAs). The results showed no significant reduction of the alkaloids in the homemade gluten-free ground poppy seed crackers, showing that both families of natural toxins can remain in foods even after intense heat treatments, highlighting the need for accurate monitoring of these natural toxins in processed food.