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1.
Foods ; 13(11)2024 Jun 01.
Artículo en Inglés | MEDLINE | ID: mdl-38890967

RESUMEN

A miniaturized solid-phase extraction of two tropane alkaloids (TAs) and twenty-one pyrrolizidine alkaloids (PAs) from infusions of dry edible flowers using optimized µSPEed® technique was developed. The optimization of the µSPEed® methodology involved testing different cartridges and comparing various volumes and numbers of loading cycles. The final conditions allowed for a rapid extraction, taking only 3.5 min. This was achieved using a C18-ODS cartridge, conditioning with 100 µL of methanol (two cycles), loading 100 µL of the infusion sample (seven cycles), and eluting the analytes with 100 µL of methanol (two cycles). Prior to their analysis by UHPLC-IT-MS/MS, the extracts were evaporated and reconstituted in 100 µL of water (0.2% formic acid)/methanol (0.2% ammonia) 95:5 (v/v), allowing for a preconcentration factor of seven times. The methodology was successfully validated obtaining recoveries ranging between 87 and 97%, RSD of less than 12%, and MQL between 0.09 and 0.2 µg/L. The validated methodology was applied to twenty samples of edible flower infusions to evaluate the safety of these products. Two infusion samples obtained from Acmella oleracea and Viola tricolor were contaminated with 0.16 and 0.2 µg/L of scopolamine (TA), respectively, while the infusion of Citrus aurantium was contaminated with intermedine and lycopsamine (PAs) below the MQL.

2.
Foods ; 13(5)2024 Feb 21.
Artículo en Inglés | MEDLINE | ID: mdl-38472764

RESUMEN

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.

3.
J Agric Food Chem ; 72(1): 819-832, 2024 Jan 10.
Artículo en Inglés | MEDLINE | ID: mdl-38109357

RESUMEN

Currently, the analysis of trace-level contaminants in food must be addressed following green analytical chemistry principles and with a commitment to the sustainable development goals. Accordingly, a sustainable and ecofriendly microextraction procedure based on µ-SPEed followed by ultrahigh liquid chromatography coupled to ion-trap tandem mass spectrometry analysis was developed to determine the occurrence of pyrrolizidine and tropane alkaloids in honey samples. The µ-SPEed procedure took approximately 3 min per sample, using only 100 µL of organic solvent and 300 µL of diluted sample. The method was properly validated (overall recoveries 72-100% and precision RSD values ≤15%), and its greenness was scored at 0.61 out of 1. The method was applied to different honey samples, showing overall contamination levels from 32 to 177 µg/kg of these alkaloids. Atropine was found in all the samples, whereas retrorsine N-oxide, lasiocarpine, echimidine, and echimidine N-oxide were the main pyrrolizidine alkaloids in the samples analyzed.


Asunto(s)
Alcaloides , Miel , Alcaloides de Pirrolicidina , Miel/análisis , Espectrometría de Masas en Tándem/métodos , Alcaloides de Pirrolicidina/química , Tropanos , Cromatografía Liquida/métodos , Alcaloides/análisis , Contaminación de Alimentos/análisis , Cromatografía Líquida de Alta Presión/métodos
4.
Toxins (Basel) ; 15(12)2023 11 24.
Artículo en Inglés | MEDLINE | ID: mdl-38133176

RESUMEN

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 sevenfold. This highlights the need to analyse these types of samples to mitigate potential public health issues.


Asunto(s)
Papaver , Papaver/química , Opio , Espectrometría de Masas en Tándem/métodos , Morfina , Dióxido de Silicio/química , Extracción en Fase Sólida/métodos , Cromatografía Líquida de Alta Presión/métodos
5.
Toxins (Basel) ; 15(6)2023 05 27.
Artículo en Inglés | MEDLINE | ID: mdl-37368663

RESUMEN

Atropine and scopolamine belong to the tropane alkaloid (TA) family of natural toxins. They can contaminate teas and herbal teas and appear in infusions. Therefore, this study focused on analyzing atropine and scopolamine in 33 samples of tea and herbal tea infusions purchased in Spain and Portugal to determine the presence of these compounds in infusions brewed at 97 °C for 5 min. A rapid microextraction technique (µSPEed®) followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was used to analyze the selected TAs. The results showed that 64% of the analyzed samples were contaminated by one or both toxins. White and green teas were generally more contaminated than black and other herbal teas. Of the 21 contaminated samples, 15 had concentrations above the maximum limit for liquid herbal infusions (0.2 ng/mL) set by Commission Regulation (EU) 2021/1408. In addition, the effects of heating conditions (time and temperature) on atropine and scopolamine standards and naturally contaminated samples of white, green, and black teas were evaluated. The results showed that at the concentrations studied (0.2 and 4 ng/mL), there was no degradation in the standard solutions. Brewing with boiling water (decoction) for 5 and 10 min allowed for higher extraction of TAs from dry tea to infusion water.


Asunto(s)
Atropina , Tés de Hierbas , Escopolamina/análisis , Tés de Hierbas/análisis , Espectrometría de Masas en Tándem/métodos , Temperatura , Tropanos/análisis , Té/química , Agua
6.
Stem Cell Reports ; 18(2): 489-502, 2023 02 14.
Artículo en Inglés | MEDLINE | ID: mdl-36638790

RESUMEN

Sex differences exist for many lung pathologies, including COVID-19 and pulmonary fibrosis, but the mechanistic basis for this remains unclear. Alveolar type 2 cells (AT2s), which play a key role in alveolar lung regeneration, express the X-linked Ace2 gene that has roles in lung repair and SARS-CoV-2 pathogenesis, suggesting that X chromosome inactivation (XCI) in AT2s might impact sex-biased lung pathology. Here we investigate XCI maintenance and sex-specific gene expression profiles using male and female AT2s. Remarkably, the inactive X chromosome (Xi) lacks robust canonical Xist RNA "clouds" and less enrichment of heterochromatic modifications in human and mouse AT2s. We demonstrate that about 68% of expressed X-linked genes in mouse AT2s, including Ace2, escape XCI. There are genome-wide expression differences between male and female AT2s, likely influencing both lung physiology and pathophysiologic responses. These studies support a renewed focus on AT2s as a potential contributor to sex-biased differences in lung disease.


Asunto(s)
COVID-19 , ARN Largo no Codificante , Femenino , Masculino , Humanos , Ratones , Animales , Inactivación del Cromosoma X/genética , Enzima Convertidora de Angiotensina 2/genética , Enzima Convertidora de Angiotensina 2/metabolismo , Genes Ligados a X , COVID-19/genética , SARS-CoV-2/genética , ARN Largo no Codificante/genética , ARN Largo no Codificante/metabolismo , Transcriptoma
7.
Int J Gynaecol Obstet ; 160(1): 345-350, 2023 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-36404724

RESUMEN

On February 21, 2022, the Colombian Constitutional Court decided that the existing regulation of abortion was unconstitutional and repealed it (Sentencia C-055/2022). The new abortion law, as per the Court's decision, considers the voluntary interruption of a pregnancy a crime only when it happens after week 24 and does not fall under the health, rape, or malformation indications developed through precedent from 2006 to 2022. The decision is generally binding and of immediate application. The decision's rationale builds on the right to health, substantive equality, and freedom of conscience. It acknowledges severe restrictions in access to abortion faced by Colombian women and the costs these restrictions have on their lives. It also recognizes that the indications model forces women to obtain permission from medical doctors to access abortion, and thus fails to recognize women's freedom of conscience.


Asunto(s)
Aborto Inducido , Femenino , Humanos , Embarazo , Aborto Legal , Colombia , Crimen
8.
Acta Derm Venereol ; 102: adv00825, 2022 Nov 29.
Artículo en Inglés | MEDLINE | ID: mdl-36444563

RESUMEN

Hidradenitis suppurativa (HS) is a chronic inflammatory disease of the hair follicles. The aim of this case-control study was to assess whether HS is associated with disturbances in trabecular bone score, bone mineral density, bone remodelling markers, and calciotropic hormones. A total of 81 patients and 79 controls of similar age and sex were included. Demographic, anthropometric, laboratory data, trabecular bone score, bone mineral density, serum 25-hydroxyvitamin D (25OHD), serum amino-terminal pro-peptide of type 1 collagen (PINP), and C-terminal telopeptide of type 1 collagen (CTX) concentrations were assessed in both groups. Patients with HS had lower serum 25OHD levels than controls, and approximately 62% of them had vitamin D deficiency. Serum PINP was increased and CTX was decreased in patients with HS. Fully adjusted trabecular bone score values were lower in patients with HS compared with controls. Adjusted lumbar bone mineral density was similar in HS and controls, whilst total hip bone mineral density was lower in patients with HS. There were no statistical differences regarding disease severity in terms of 25OHD, serum turnover markers, bone mineral density, or trabecular bone score values. This study shows that patients with HS have lower trabecular bone score and total hip bone mineral density values than population-based controls. In addition, the prevalence of vitamin D deficiency is high in subjects with HS.


Asunto(s)
Hidradenitis Supurativa , Deficiencia de Vitamina D , Humanos , Estudios de Casos y Controles , Colágeno Tipo I , Deficiencia de Vitamina D/diagnóstico , Deficiencia de Vitamina D/epidemiología , Folículo Piloso
9.
Molecules ; 27(19)2022 Sep 28.
Artículo en Inglés | MEDLINE | ID: mdl-36234940

RESUMEN

Volatile organic metabolites (VOMs) present in different spices can provide distinct analytical biosignatures related to organoleptic properties and health benefits. This study aimed to establish the volatilomic fingerprint of six of the most consumed spices all over the world (saffron (Crocus sativus L.), cinnamon (Cinnamomum verum), cumin (Cuminum cyminum L.), black pepper, (Piper nigrum L.), sweet paprika (Capsicum annuum L.), and curry (a mix of different herbs and spices)). Based on headspace solid phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis, this is a powerful strategy to explore and establish the spice's volatile pattern and unravel the potential health benefits related to the most important VOMs identified in each spice. This comprehensive knowledge will help in the definition of their authenticity, while simultaneously protecting against potential frauds and adulterations. A total of 162 VOMs were identified. Semi-quantitative assessments revealed that terpenoids and sesquiterpenoids amounted to the major volatile class in the investigated spices, except for cinnamon, where carbonyl compounds are the major group. Most of the studied spices comprised key characteristics of aroma and health bioactive compounds, e.g., dihydrojuneol in saffron, cinnamaldehyde in cinnamon, cuminaldehyde in cumin and curry, and caryophyllene in black pepper. The principal component analysis (PCA) and partial least-squares discriminant analysis (PLS-DA) successfully discriminated the investigated spices, being α-cubebene, 3-methyl butanal, ß-patchoulene and ß-selinene, the most important VOMs (highest VIP's) that contributed to its discrimination. Moreover, some VOMs have a high influence on the spice's bioactive potential, helping to prevent certain diseases including cancer, inflammatory-related diseases, diabetes, and cardiovascular diseases.


Asunto(s)
Capsicum , Crocus , Cuminum , Piper nigrum , Compuestos Orgánicos Volátiles , Crocus/química , Cuminum/química , Cromatografía de Gases y Espectrometría de Masas/métodos , Piper nigrum/química , Especias/análisis , Terpenos/análisis , Compuestos Orgánicos Volátiles/análisis
10.
Toxins (Basel) ; 14(10)2022 Sep 20.
Artículo en Inglés | MEDLINE | ID: mdl-36287919

RESUMEN

This work presents an optimized methodology based on the miniaturization of the original QuEChERS (µ-QuEChERS) followed by liquid chromatography coupled to mass spectrometry (HPLC-MS/MS) for the determination of tropane alkaloids (TAs), atropine, and scopolamine in leafy vegetable samples. The analytical methodology was successfully validated, demonstrating quantitation limits (MQL) ≤ 2.3 ng/g, good accuracy, and precision, with recoveries between 90-100% and RSD ≤ 13% for both analytes. The method was applied to the analysis of TA-producing plants (Brugmansia versicolor, Solandra maxima, and Convolvulus arvensis). High concentrations of scopolamine were found in flowers (1771 mg/kg) and leaves (297 mg/kg) of B. versicolor. The highest concentration of atropine was found in flowers of S. maxima (10.4 mg/kg). Commercial mixed leafy vegetables contaminated with B. versicolor and S. maxima were analysed to verify the efficacy of the method, showing recoveries between 82 and 110% for both analytes. Finally, the method was applied to the analysis of eighteen samples of leafy vegetables, finding atropine in three samples of mixed leafy vegetables, with concentrations of 2.7, 3.2, and 3.4 ng/g, and in nine samples with concentrations ≤MQL. In turn, scopolamine was only found in a sample of chopped Swiss chard with a concentration ≤MQL.


Asunto(s)
Espectrometría de Masas en Tándem , Verduras , Cromatografía Líquida de Alta Presión , Verduras/química , Espectrometría de Masas en Tándem/métodos , Tropanos/análisis , Atropina , Escopolamina/análisis , Hojas de la Planta/química
11.
Foods ; 11(15)2022 Jul 23.
Artículo en Inglés | MEDLINE | ID: mdl-35892780

RESUMEN

In this work, the thermal degradation of tropane and opium alkaloids was studied in samples of breadsticks prepared with corn flour, contaminated with seeds of Datura stramonium, and containing seeds of Papaver somniferum L. A total of seven different samples were prepared and eight alkaloids were studied, three tropane (atropine, scopolamine, and anisodamine) and five opium (morphine, codeine, thebaine, papaverine, and noscapine) alkaloids. For this purpose, a fast, easy and efficient method based on solid-liquid extraction (SLE) prior to the analysis by high-performance liquid chromatography with a diode array detector (HPLC-DAD) was developed and validated. Thermal degradation studies showed a decrease in the TAs and OAs content under baking (180 °C for 20 min) that was between 7-65% for atropine, depending on the preparation conditions used, between 35-49% for scopolamine and anisodamine, up to 100% for morphine and codeine and between 14-58% for thebaine, papaverine, and noscapine. Results also evidenced that degradation of morphine and codeine was higher when the seeds were added as topping to the breadsticks.

12.
J Agric Food Chem ; 70(24): 7594-7606, 2022 Jun 22.
Artículo en Inglés | MEDLINE | ID: mdl-35674269

RESUMEN

Bakery products containing poppy seeds are increasingly being commercialized. These seeds may be contaminated with latex from the Papaver somniferum L. plant rich in opium alkaloids (OAs). Therefore, health authorities demand the development of analytical methods to control them. In this study, an efficient and simple method was developed and validated for the first time to analyze six OAs in bakery products by high-performance liquid chromatography-tandem mass spectrometry. For this purpose, a solid-liquid extraction was optimized, and then a magnetic material [magnetite surface-modified with Fe(III) terephthalate, denoted as Fe3O4@TPA-Fe] was used for a fast magnetic solid-phase extraction. The method has been validated with adequate recoveries (70-110%) and relative standard deviations (<20%) and without matrix effects. Nine bakery samples (five breadsticks and four sliced bread) were analyzed; breadsticks showed low amounts of OAs, but two sliced bread showed higher amounts of OAs than the new amount (1.5 mg/kg) set by the Commission Regulation (EU) 2021/2142.


Asunto(s)
Alcaloides Opiáceos , Papaver , Cromatografía Líquida de Alta Presión/métodos , Compuestos Férricos , Fenómenos Magnéticos , Opio/análisis , Papaver/química , Semillas/química , Extracción en Fase Sólida , Espectrometría de Masas en Tándem/métodos
13.
Food Chem ; 393: 133371, 2022 Nov 01.
Artículo en Inglés | MEDLINE | ID: mdl-35661599

RESUMEN

Mallow blue (Malva sylvestris L.), hibiscus (Hibiscus rosa-sinensis L.) and nasturtium (Tropaeolum majus L.), are common edible flowers rich in bioactive secondary metabolites (BASMs) whose use in sophisticated gastronomy present currently as increasing trend. In this study the BASMs profile of these edible flowers was established using an emerging green extraction technique, µQuEChERS followed by ultra-high performance liquid chromatography coupled to a photodiode array detection system (UHPLC-PDA). After validation the µQuEChERS/UHPLC-PDA methodology allow to identify that apigenin and epigallocatechin gallate are the most abundant BASMs in mallow blue flowers, while catechin and dicaffeoylquinic acid are predominant in hibiscus flowers, and myricitrin and dicaffeoylquinic acid in nasturtium flowers. Total polyphenol content is the highest in the extract of hibiscus. Nasturtium shows the greatest radical scavenging activity. The results revealed that these flowers constitute a potential source of BASMs with different bioactive properties suggesting its use in design of new functional foods.


Asunto(s)
Hibiscus , Tropaeolum , Antioxidantes/química , Cromatografía Líquida de Alta Presión/métodos , Flores/química , Extractos Vegetales/química , Polifenoles/análisis , Tropaeolum/química
14.
Food Chem ; 394: 133512, 2022 Nov 15.
Artículo en Inglés | MEDLINE | ID: mdl-35728464

RESUMEN

A high throught methododology based on a green extraction technique, µSPEed®, followed by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been proposed for the analysis of atropine and scopolamine in tea and herbal tea infusions. For this, a digiVOL® Digital Syringe was used with different sorbents and working conditions to obtain a fast and efficient µSPEed® extraction. The best performance was achieved with a PS/DVB sorbent phase, sample loading of 5 × 500 µL and elution with 2 × 100 µL aliquots of methanol. The strategy based on µSPEed® followed by HPLC-MS/MS was validated, attaining quantitation limits lower than 0.15 ng mL-1 and recoveries between 94 and 106% for both analytes and applied to seventeen tea and herbal tea infusions. Fourteen infusions showed contamination with one or both analytes above the maximum content legislated (sum of atropine and scopolamine < 0.2 ng mL-1).


Asunto(s)
Tés de Hierbas , Atropina/análisis , Cromatografía Líquida de Alta Presión/métodos , Límite de Detección , Escopolamina/análisis , Espectrometría de Masas en Tándem/métodos , Té/química , Tés de Hierbas/análisis
15.
J Agric Food Chem ; 70(25): 7826-7841, 2022 Jun 29.
Artículo en Inglés | MEDLINE | ID: mdl-35714998

RESUMEN

A sustainable microextraction of pyrrolizidine alkaloids (PAs) from edible flower infusions using the innovative µSPEed technique is proposed. Different sorbents and extraction conditions were tested, achieving the highest extraction efficiency with an octadecylsilane sorbent (4 mg). The extraction procedure just took 1 min per sample, and only 300 µL of methanol and 300 µL of the sample were used per extraction. Ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry was used for analysis. The method was properly validated, providing suitable linearity, selectivity, sensitivity (quantification limits 0.3-1 µg/L), overall recoveries (79-97%), and precision (≤17% relative standard deviation). Its application to the analysis of different infusions of mallow, calendula, and hibiscus flowers revealed similar total PA values (23-41 µg/L) and contamination profile among the mallow and hibiscus samples, with predominance of senecionine-type and heliotrine-type PAs, respectively. Conversely, calendula samples showed more variations (23-113 µg/L), highlighting the occurrence of intermedine N-oxide and europine N-oxide on them.


Asunto(s)
Calendula , Hibiscus , Alcaloides de Pirrolicidina , Cromatografía Líquida de Alta Presión/métodos , Cromatografía Liquida , Flores/química , Óxidos , Alcaloides de Pirrolicidina/química , Espectrometría de Masas en Tándem/métodos
16.
Toxins (Basel) ; 14(3)2022 03 17.
Artículo en Inglés | MEDLINE | ID: mdl-35324716

RESUMEN

In this work, Hexagonal Mesoporous Silica (HMS) and Santa Barbara Amorphous-15 (SBA-15) mesostructured silicas were synthesized and functionalized with sulfonic acid groups. The materials (HMS-SO3− and SBA-15-SO3−) were evaluated as strong cation exchange sorbents for sample extract clean-up, by solid phase extraction (SPE) and dispersive solid phase extraction, to determine atropine (At) and scopolamine (Sc) in commercial culinary aromatic herbs. Under optimized conditions, 0.25 g of sample was subject to solid−liquid extraction with acidified water (pH 1.0), and good recovery percentages were achieved for At and Sc using 75 mg of HMS-SO3− in SPE as the clean-up stage, prior to their determination by HPLC-MS/MS. The proposed method was validated in a thyme sample showing recoveries in the range of 70−92%, good linearity (R2 > 0.999), adequate precision (RSD ≤ 14%) and low limits (MDL 0.8−2.2 µg/kg and MQL 2.6−7.2 µg/kg for both analytes). Sixteen aromatic herbs samples (dried thyme, basil and coriander leaves) were analysed and At was found in fourteen samples over an interval of <5−42 µg/kg, whereas Sc was found in three of the sixteen samples studied (between <5−34 µg/kg). The amount of At and Sc found in some analysed samples confirms the importance of setting maximum levels of At and Sc in culinary aromatic herbs.


Asunto(s)
Extracción en Fase Sólida , Espectrometría de Masas en Tándem , Cationes , Cromatografía Líquida de Alta Presión/métodos , Dióxido de Silicio , Extracción en Fase Sólida/métodos , Espectrometría de Masas en Tándem/métodos , Tropanos
17.
Foods ; 11(3)2022 Jan 30.
Artículo en Inglés | MEDLINE | ID: mdl-35159558

RESUMEN

Tropane alkaloids (TAs) are natural toxins produced by different plants, mainly from the Solanaceae family. The interest in TAs analysis is due to the serious cases of poisoning that are produced due to the presence of TA-producing plants in a variety of foods. For this reason, in recent years, different analytical methods have been reported for their control. However, the complexity of the matrices makes the sample preparation a critical step for this task. Therefore, this review has focused on (a) collecting the available data in relation to the occurrence of TAs in foods for human consumption and (b) providing the state of the art in food sample preparation (from 2015 to today). Regarding the different food categories, cereals and related products and teas and herbal teas have been the most analyzed. Solid-liquid extraction is still the technique most widely used for sample preparation, although other extraction and purification techniques such as solid-phase extraction or QuEChERS procedure, based on the use of sorbents for extract or clean-up step, are being applied since they allow cleaner extracts. On the other hand, new materials (molecularly imprinted polymers, mesostructured silica-based materials, metal-organic frameworks) are emerging as sorbents to develop effective extraction and purification methods that allow lower limits and matrix effects, being a future trend for the analysis of TAs.

18.
Food Chem ; 380: 132189, 2022 Jun 30.
Artículo en Inglés | MEDLINE | ID: mdl-35086011

RESUMEN

This work proposes the miniaturization and modification of the QuEChERS strategy using different large pore mesostructured silicas, non-modified and modified with amino groups (NH2), as dispersive clean-up sorbents for multi-component extraction of 21 pyrrolizidine alkaloids from different aromatic herbs, combined with ultra-high performance liquid chromatography coupled to tandem mass spectrometry analysis. The procedure was miniaturized by reducing the amounts of sample (0.2 g), solvents (2 mL), clean-up sorbents (25 mg sorbent + 150 mg MgSO4) and partitioning salts (0.65 g) employed. Best results were achieved using mesostructured silicas (LP-MS-NH2) than conventional PSA. The method was validated (overall recoveries 73-105%) and applied to the analysis of 17 samples. All the samples were contaminated with PAs (average concentration 262 µg/Kg). Thyme and basil samples were the most contaminated, whereas rosemary was the least. Lasiocarpine, senecivernine N-oxide and europine N-oxide were the main PAs that contributed to their contamination.


Asunto(s)
Alcaloides de Pirrolicidina , Extracción en Fase Sólida , Cromatografía Líquida de Alta Presión , Dióxido de Silicio , Espectrometría de Masas en Tándem
19.
Foods ; 10(7)2021 Jul 05.
Artículo en Inglés | MEDLINE | ID: mdl-34359430

RESUMEN

Insect-based products are novel foods (NF) that merit careful study. For this reason, in this work a method has been developed for the simultaneous analysis of four food processing contaminants (FPC), acrylamide (AA), 5-hydroxymethylfurfural, (HMF), 5-methylfurfural (MF) and furfural (F), in insect-based products (bars, crackers and flours) by high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (HPLC-QqQ-MS/MS). The method consisted of a solid-liquid extraction (SLE) with acidified water, followed by solid-phase extraction (SPE), using 100 mg of a sorbent based on mesostructured silica with a large pore functionalized with amino groups (SBA-15-LP-NH2). The analytical method was properly optimized and validated in a representative bar sample of pineapple & coconut with cricket flour (Ins-B-Pine-Coco) showing good accuracy, with recoveries ranging from 70-101% for the four analytes and adequate precision (RSD < 9%). Good linearity (R2 ≥ 0.995) and low method quantification limits for AA (between 1.3-1.4 µg/g), F (between 7.9-8.8 µg/g), MF (between 3.1-6.5 µg/g) and HMF (between 1.5-3.3 µg/g) were also obtained in all samples studied. The proposed method was successfully applied in eleven insect-based foods. Results revealed that insect-based bars can be a good alternative to traditional cereal bars to reduce dietary exposure to HMF; but, in order to reduce the exposure to AA, alternative formulations must be evaluated in the design of innovative insect-based crackers.

20.
Foods ; 10(7)2021 Jul 08.
Artículo en Inglés | MEDLINE | ID: mdl-34359458

RESUMEN

In recent years, health authorities have become increasingly concerned about preventing consumer exposure to opium alkaloids present in Papaver somniferum L. poppy seeds. In this study, a simple, rapid and efficient method has been optimised to determine all main opioids in poppy seeds (morphine, codeine, thebaine, papaverine, noscapine and oripavine) by UHPLC-QqQ-MS/MS. For this purpose, solid-liquid extraction (SLE) of samples was optimised and six magnetic adsorbent materials with a core of Fe3O4 coated with amorphous and mesostructured silica, both functionalised with octadecyl-silane or octyl-silane were characterised and evaluated for magnetic solid-phase extraction (MSPE). The material with the best results was non-functionalised mesostructured silica and, with it, the MSPE procedure was optimised. This method was validated and used to quantify six opioids in 14 edible seed samples (eleven poppy seeds and three seed mixes). Considerable amounts were found (1.5-249.0 mg/kg morphine, <0.2 µg/kg-45.8 mg/kg codeine, <2.4 µg/kg-136.2 mg/kg thebaine, <0.2 µg/kg-27.1 mg/kg papaverine, <0.2 µg/kg-108.7 mg/kg noscapine and <240 µg/kg-33.4 mg/kg oripavine), exceeding maximum limits established in some EU countries and the reference level of morphine in the EU. Furthermore, in some commercial samples for human consumption, inadequate labelling was found because significant amounts of alkaloids were detected even though Papaver rhoeas L. seeds were declared on the product label.

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