Systematic Study of the Content of Phytochemicals in Fresh and Fresh-Cut Vegetables

Vegetables and fruits have beneficial properties for human health, because of the presence of phytochemicals, but their concentration can fluctuate throughout the year. A systematic study of the phytochemical content in tomato, eggplant, carrot, broccoli and grape (fresh and fresh-cut) has been performed at different seasons, using liquid chromatography coupled to triple quadrupole mass spectrometry. It was observed that phenolic acids (the predominant group in carrot, eggplant and tomato) were found at higher concentrations in fresh carrot than in fresh-cut carrot. However, in the case of eggplant, they were detected at a higher content in fresh-cut than in fresh samples. Regarding tomato, the differences in the content of phenolic acids between fresh and fresh-cut were lower than in other matrices, except in winter sampling, where this family was detected at the highest concentration in fresh tomato. In grape, the flavonols content (predominant group) was higher in fresh grape than in fresh-cut during all samplings. The content of glucosinolates was lower in fresh-cut broccoli than in fresh samples in winter and spring sampling, although this trend changes in summer and autumn. In summary, phytochemical concentration did show significant differences during one-year monitoring, and the families of phytochemicals presented different behaviors depending on the matrix studied

Monitoring of Volatile Additives from Plant Protection Products in Tomatoes Using HS-SPME-GC-HRMS: Targeted and Suspect Approaches

Additives present in plant protection products (PPPs) are normally not monitored after sample treatments. In this study, the fate of additives detected by targeted and nontargeted analysis in tomato samples treated with two PPPs was carried out. The study was carried out in a greenhouse for 12 days, in which two applications with each PPP were made. Compounds were extracted by applying a headspace solid phase microextraction (HS-SPME) and analyzed by gas chromatography coupled to high resolution mass spectrometry (GC-HRMS), performing targeted and suspect approaches. Three targeted and 15 nontargeted compounds were identified at concentration levels of up to 150 μg/kg. Compounds detected encompassed benzene, toluene, indene, and naphthalene derivatives, as well as conservatives and flavouring compounds. Most of them degraded in less than 7 days after the second application, following first-order kinetic. This study aims to reduce knowledge gaps regarding additives and their fate under real climatic conditions of greenhouses cultivations.Spanish Ministry of Economy and Competitiveness (MINECO)FEDER-EU (project PID2019-106201RB-I00)Regional Government of Andalusia, SpainEuropean funds for financial support (project P18- RT-2329)Andalusian Ministry of Economic Transformation, Industry, Knowledge and Universities for financial support from “Ayudas para Captación, Incorporación y Movilidad de Capital Humano de I+D+i (PAIDI 2020)”University of Almería for his “Convocatoria de Recualificación do Sistema Universitario Español-Margarita Salas”“Plan de Recuperación Transformación” program funded by the Spanish Ministry of UniversitiesEuropean Union’s NextGenerationEU fund

ESTUDIO DE LA INFLUENCIA DE pH Y TEMPERATURA EN LA RACEMIZACIÓN DE (-)-HIOSCIAMINA A (+)-HIOSCIAMINA EN SEMILLAS DE ESTRAMONIO

El estramonio es una planta de la familia de las Solenaceaes, del género Daturae, que crece como maleza junto a campos de cultivo. Debido a su toxicidad y sus efectos sobre la alimentación y la seguridad de los piensos animales y alimentos para los humanos, la determinación de sustancias tóxicas en estas plantas está ganado interés. Los principales componentes tóxicos son la escopolamina y la atropina (mezcla racémica de (+) y (-)-hiosciamina). Aunque la atropina sea una mezcla racémica, solo el enantiómero encontrado naturalmente, la (-)-hiosciamina, tiene actividad farmacológica, siendo un potente anticolinérgico [1,2]. La racemización ocurre en el proceso de extracción de la (-)-hiosciamina, con temperaturas elevadas y prolongadas y pH básico, siendo muy escasos los estudios realizados en este sentido [3]. Así mismo resulta de interés conocer las condiciones en las que se produce la racemización de un compuesto en otro, ya que las mismas son también de aplicación en procesos del cocinado (cocción u horneado) de alimentos que contengan pequeñas cantidades de semillas de plantas de la familia de las Solenaceaes. En la presente comunicación se realiza un estudio de la influencia del pH y la temperatura en dicho proceso. A tal fin se realizaron experiencias a valores de pH de 3, 5, 7 y 9 y temperaturas de 30, 50 y 80ºC. Así mismo se estudió la influencia del mantenimiento de algunas condiciones (pH 5 y 9 a 80ºC) en el proceso de conversión de racemización. Para estudiar estos factores se hace uso de un método basado en cromatografía de líquidos de alto rendimiento acoplada a espectrometría de masas en tándem (HPLCMS/ MS), empleando una columna quiral, Chiralpak-AY3. La separación se realiza en modo isocrático usando etanol al 0,1% dietanolamina como fase móvil, en un tiempo de 10 minutos. La extracción de la hiosciamina de las semillas de estramonio se realiza mediante el método QuEChERS

Persistence of transferred fragrance on fabrics for forensic reconstruction applications

It has recently been established that volatile organic compounds (VOCs) successfully transfer between clothing even with a short contact of 10 s, highlighting the potential to use VOCs in forensic reconstruction scenarios, such as sexual assault cases. The mid and low volatility compounds transferred in greater amounts than high volatility compounds. This study presents empirical data addressing the persistence of transferred VOCs on clothing for the first time. A series of experiments were carried out to determine the persistence of VOCs on clothing for time periods of up 4 weeks, on natural and synthetic fibres, and at three different environmental temperatures. The data indicate that the highest VOC amounts are generally obtained for shorter persistence times of up to 1 d. Whilst high volatility compounds were not recovered in sufficient amounts to allow quantification, the four other transferred VOCs were successfully quantified for persistence times of up to 4 weeks. The persistence for mid-volatility compounds follows decay curve trends in line with those previously obtained for fibres, glass and pollen. When comparing the persistence of VOCs on a natural and a synthetic fibre, for a persistence time of 1 h, the transferred VOCs were retained on a natural fibre in higher amounts than on a synthetic fibre. However, for longer persistence times the concentration of VOCs was similar between the two fabrics. Lastly, lower environmental temperatures resulted in higher recoveries for most VOCs, especially for short persistence times. These findings demonstrate that optimal recovery of VOCs from clothing occurs when the fabric is kept at cooler temperatures and analysed soon after the fragrance transfer occurred, although VOC recovery was possible at higher temperatures and after longer persistence times. Given the transfer and persistence characteristics of VOCs from fragrance, there is potential for fragrance to be used as a form of trace in forensic reconstruction approaches

Determination of atropine and scopolamine in bluckwheat and related products using modified QuEChERS and liquid chromatography tándem mass spectrometry

Buckwheat is a healthy pseudo cereal widely cultivated over the world as an important raw material used for functional food because it becomes a dietary source of bioactive compounds, such as nutritionally valuable protein, phenolic compounds, starch and dietary fiber, essential minerals and trace elements. However, buckwheat can be contaminated by stramonium (Datura stramonium), which can contain high concentration of tropane alkaloids, and therefore, these toxic substances can be found in buckwheat and related matrices at concentrations higher than 100 μg/kg [1]. Tropane alkaloids are synthesized by the plants of the genus from Solanaceae family, although they are also produced in smaller quantities in plants from other families. They can affect human and animal health due to their high toxicity and intake of contaminated food or animal feed. Although there are more than 200 tropane alkaloids, atropine and scopolamine are the most common compounds of this family. According to the EFSA scientific opinion in 2013 [1] more attention must be focused on the contaminated levels of atropine and scopolamine in food from plant origin, such as cereal products, grain-based baby-food, buckwheat grain and food products and tea and herbal infusions. Therefore, the development of quick, easy and reliable analytical methods for the trace analysis of tropane alkaloids at trace levels in food from plant origin is desirable. Therefore the aim of this study is the development and validation of an analytical method for the simultaneous determination of atropine and scopolamine residues in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction method with acidified acetonitrile (1% formic acid v/v) followed by a clean-up step using graphitized black carbon (GBC) and primary secondary amine (PSA) was applied. For the separation and quantification of the target compounds, ultra high performance liquid chromatography (UHPLC)-coupled to tandem mass spectrometry (MS/MS), utilizing triple quadrupole (QqQ) as analyzer, was used. The method was validated, determining linearity, trueness, precision, limits of detection (LODs) and quantification (LOQs). Recoveries ranged from 75 to 92% with precision below 17% (RSD values) for all the compounds studied. Both LODs and LOQs were below 2 μg kg-1. The validated method was tested in eight commercial samples (buckwheat, wheat, soy, buckwheat flour, buckwheat noodle, amaranth grain, chia seeds and peeled millet). Target compounds were not found above the detection limits of the method

Enantiomeric separation of (-) and (+)- hyosciamine by high performance liquid chromatography-tandem mass spectrometry

Interest in natural toxins produced by fungi or plants has grown in recent years due to its toxicity and its impact on feeding and animal feed and human food safety. Among these toxins, alkaloids and more specifically tropane alkaloids, are very significant and they are characterized by presenting anticholinergic activity. Tropane alkaloids are synthesized by the plants from Solanaceae family and in smaller quantities from plants from other families. This family of compounds involves more than 200 compounds, although the compounds most studied are scopolamine, atropine and (-)-hyoscyamine [1]. In the case of atropine, which is a racemic mixture of (-) and (+)-hyoscyamine, it is well known that (-)-hyoscyamine exhibit stronger anticholinergic effects than the (+)-hyoscyamine. Moreover, racemization occurs during the treatment process of the raw material and cooking procedures due to pH and temperature modifications, since only the (-)-hyoscyamine is naturally formed. For this reason, according to the EFSA interest in 2013 [1] it is necessary to develop methods which allows the separation of these two chiral enantiomers to elucidate the conditions that favor the transformation between both enantiomers, because there are not many studies that evaluate these processes. Therefore the aim of this study is the optimization of the enantioselective separation of (-) and (+)-hyoscyamine with a Chiralpak-AY3 (150x4.6 mm, 3 μm) analytical column in combination with high performance liquid chromatography (HPLC)-coupled to tandem mass spectrometry (MS/MS) has been used. The developed method allowed the separation of the two target compounds in 10 min, using ethanol 0.1% diethanolamine as mobile phase. In addition, the influence of differents parameters, such as pH apparent or temperature, in the signal of the (-) and (+)-hyoscyamine was studied. Finally the method was applied to the determination of the target compounds in buckwheat samples. Performance characteristics, such as trueness (in terms of recovery), precision, linearity, detection limits (LODs) and quantification limits (LOQs) were studied. Suitable performance characteristics were obtained for a reliable determination of both enantiomers in the selected samples

Compuesto deuterados de flonicamida, procedimiento de preparación y uso de los mismos

ES2644163 A1 (27.11.2017) P201600466 (27.05.2016)Compuestos deuterados de flonicamida, procedimiento de preparación y uso de los mismos. La invención se refiere a un compuesto deuterado de flonicamida, de fórmula (I) en la que R1 es un grupo seleccionado entre -CH2-CN y -CH2-COOH; y R2 es H, y en la que al menos un átomo de hidrógeno en R1 o en R2 está sustituido por deuterio; a su procedimiento de obtención y a su uso como patrón para la detección y cuantificación de flonicamida y derivados mediante técnicas cromatográficas acopladas a espectrometría de masas.UNIVERSIDAD DE ALMERÍ