RESUMO
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.
Assuntos
Alcaloides , Mel , Alcaloides de Pirrolizidina , Mel/análise , Espectrometria de Massas em Tandem/métodos , Alcaloides de Pirrolizidina/química , Tropanos , Cromatografia Líquida/métodos , Alcaloides/análise , Contaminação de Alimentos/análise , Cromatografia Líquida de Alta Pressão/métodosRESUMO
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.
RESUMO
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.
RESUMO
The exponential number of food alerts about concerning levels of some plant-alkaloids, such as pyrrolizidine, tropane and opium alkaloids, have stressed the need to monitor their occurrence in foods to avoid toxic health effects derived from their intake. Therefore, analytical strategies to simultaneously monitor the occurrence of these alkaloids should be developed to ensure food safety an comply with regulations. Accordingly, this work proposes an efficient multicomponent analytical strategy for the simultaneous extraction of these alkaloids from commercial bakery products. The analytical method was validated and applied to the analysis of 15 samples, revealing that 100% of them contained at least one of the target alkaloids, in some cases exceeding the maximum limits legislated. Moreover, in two samples the 3 different alkaloid families were detected. These results confirm the importance of simultaneously monitoring these alkaloids in food and highlight also considering some opium alkaloids in current legislation.
RESUMO
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.
Assuntos
Papaver , Papaver/química , Ópio , Espectrometria de Massas em Tandem/métodos , Morfina , Dióxido de Silício/química , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão/métodosRESUMO
Resumo Neste artigo, investigamos o nível de aderência dos serviços de cuidado de crianças de zero a três anos à agenda feminista de políticas públicas. Para isso, realizamos um estudo de casos qualitativo de três países latino-americanos (Brasil, Argentina e Uruguai), durante o "giro à esquerda". Analisando três indicadores parametrizados (elegibilidade, cobertura e tipo de jornada), identificamos avanços maiores no Uruguai, mais restritos na Argentina e intermediários no Brasil. A variação positiva foi maior para elegibilidade e cobertura, do que para tipo de jornada. Concluímos que essa assimetria na variação dos indicadores sugere que os avanços decorrem principalmente do reconhecimento dos direitos das crianças à educação, e, secundariamente, do compromisso com a igualdade de gênero.
Résumé Cet article examine le niveau d'adhésion à l'agenda féministe des politiques publiques concernant les services de garde d'enfants de zéro à trois ans. A ce fin, nous avons mené une étude de cas qualitative dans trois pays d'Amérique latine (Brésil, Argentine et Uruguay) à l'époque de leur "tournant à gauche". En analysant trois indicateurs paramétrés (éligibilité), couverture et modalités d'accueil), nous avons constaté que les progrès les plus importants concernaient l'Uruguay et les moindres l'Argentine alors qu'au Brésil ils étaient. La variation positive était plus significative. Pour l'égibilité et la couverture que pour les modalités d'accueil. Nous avons conclu que cette asymétrie dans la variation des indicateurs suggère que les progrès découlent plutôt de la reconnaissance des droits de l'enfant à l'éducation, et, secondairement, de l'engagement en faveur de l'égalité de genre.
Resumen En este artículo, investigamos el nivel de adhesión de los servicios de cuidado infantil (cero a tres años) a la agenda feminista de políticas públicas. Para esto, realizamos un estudio de casos cualitativo de tres países latinoamericanos (Brasil, Argentina y Uruguay), durante el "giro a la izquierda". Analizando tres indicadores parametrizados (elegibilidad, cobertura y tipo de jornada), logramos encontrar avances mayores en Uruguay, más restrictos en Argentina e intermedios en Brasil. Además, los resultados fueron más positivos para a elegibilidad y cobertura que para el tipo de jornada. Concluimos que esa diferencia apunta que los avances que ocurrieron están, primero, relacionados al reconocimiento de los derechos de la infancia y, secundariamente, al compromiso con la igualdad de género.
Abstract In this article, we investigate the level of adherence of childcare services (zero to three years of age) to the feminist public policy agenda. To do so, we conducted a qualitative case study of three Latin American countries (Brazil, Argentina, and Uruguay), during the "left turn". Analyzing three parameterized indicators (eligibility, coverage, and type of school day), we identified greater progress in Uruguay, more restricted in Argentina and intermediate in Brazil. The positive variation was greater for eligibility and coverage, than for type of school day. We concluded that the results are related with the recognition of the right to childhood, firstly, and with commitment to gender equality, secondly.
RESUMO
Teniendo en cuenta que no existe una normativa actualizada nacional para el control de calidad de los envases metálicos de aerosol que se utilizan en la industria farmacéutica y la cosmética, en este trabajo se desarrolló una guía de análisis para aplicarla de forma rutinaria a los envases con boca de 25,4 mm de diámetro. El primer paso consistió en realizar una revisión documental de las normativas del Instituto Colombiano de Normas Técnicas (Icontec), la Consumer Specialty Products Associations Aerosol Guide (CSPA), la Federación Europea de Aerosoles (FEA), la European Standards (EN) y el Instituto Argentino de Normalización (IRAM). Luego se seleccionaron los análisis de mayor criticidad y practicidad que fueran aplicables a la industria del llenado de aerosoles y se confirmó su viabilidad técnica en diferentes envases metálicos con un diámetro de boca de 25,4 mm, con el fin de desarrollar un protocolo unificado para llevar a cabo el control de calidad de estos envases metálicos.
This study was conducted with the objective of developing an analysis guide for quality control of metal containers used for filling of aerosols in the pharmaceutical and cosmetic industry, taking into account that at the national level there are no regulations for quality control of containers metal for aerosol. First, we conducted a literature review of the regulations of Instituto Colombiano de Normas Técnicas (Icontec), Consumer Specialty Products Association Guide (CSPA), European Aerosol Federation (FEA), European Standards EN, and Instituto Argentino de Normalización (IRAM). Subsequently, more critical analysis and practicality that are applicable to aerosol filling industry were selected and technical feasibility was confi rmed for various metal packaging with a mouth diameter of 25.4 mm, to develop a unified protocol quality control of these metal containers.
RESUMO
O Empowerment Psicológico é um constructo motivacional pela garantia de condições que aumentem a motivação para a realização das tarefas, com um forte sentido de autoeficácia. O presente estudo tem como objetivo analisar a estrutura fatorial da escala de Empowerment Psicológico numa amostra portuguesa de 230 indivíduos, funcionários de universidade pública portuguesa. Os resultados da análise fatorial confirmatória, da escala de 12 itens, mostram uma estrutura de quatro fatores, com elevada consistência interna, o que sugere a sua pertinência para aplicação à população portuguesa. Reitera-se a premência em continuar a estudar esta temática, sobretudo a sua relação com os demais processos organizacionais...
Psychological empowerment is a motivational construct, by ensuring conditions that increase motivation to perform tasks, with a strong sense of self-efficacy. The present study aimed to examine the factor structure of the psychological empowerment scale in a Portuguese sample of 230 individuals, employees of a public university in Portugal. The results of the confirmatory factor analysis of the 12 items on the scale show a structure of four factors, with high internal consistency, which suggests appropriateness for application to a Portuguese population. We reiterate the urgent need to further examine this issue, namely, its relationship with other organizational processes...
El Empowerment Psicológico es un constructo motivacional, garantizando las condiciones que aumentan la motivación para llevar a cabo las tareas, con un fuerte sentido de auto-eficacia. El objetivo de este estudio es analizar la estructura factorial de la escala de Empowerment Psicológico en una muestra portuguesa de 230 trabajadores de una universidad pública portuguesa. Los resultados del análisis factorial confirmatorio, de la escala de 12 ítems, mostraron una estructura de cuatro dimensiones y una elevada fiabilidad, por lo que puede ser considerada apropiada para su aplicación en el contexto portugués. Del mismo modo, nuevos estudios son necesarios sobre esta temática especialmente por su relación con aspectos organizacionales significativos en las empresas...
Assuntos
Humanos , Feminino , Adulto , Pessoa de Meia-Idade , Adaptação Psicológica , Análise Fatorial , Local de Trabalho/psicologia , Motivação , Poder Psicológico , UniversidadesRESUMO
El crecimiento progresivo de la industria de los aerosoles, se debe en gran medida a la efectividad de este tipo de envase para contener, proteger, conservar y dosificar el producto. Actualmente, se le han agregado algunos elementos que influyen notablemente en la decisión final, pues permiten que estos envases sean económicos, ergonómicos, amigables con el medioambiente y con buena apariencia. La tendencia del crecimiento de la industria del aerosol se ha extendido a todos los sectores de consumo, principalmente para el cuidado personal, el cuidado del hogar, productos farmacéuticos para uso humano y veterinario y productos alimenticios. Gracias al esfuerzo de empresas maquiladoras en búsqueda de nuevas oportunidades, hoy Colombia cuenta con maquinaria e insumos para producir aerosoles con calidad internacional. Dada la diversidad de proveedores de envases, necesarios para cubrir la demanda, es indispensable establecer pautas para el control de la calidad de los envases, pues ello incide directamente en la calidad del producto final. En el presente trabajo se revisaron y evaluaron las normas más representativas, del ámbito nacional e internacional, para el control de calidad de envases metálicos para aerosol, con el fin de identificar las pruebas aplicables al sector industrial tanto farmacéutico como cosmético.
The progressive growth of the aerosol industry is due largely to the effectiveness of this type of packaging to contain, protect, preserve and dispense the product. Currently, some elements have been added in order to influence the final decision, they allow these containers are economical, ergonomic, environmentally friendly and good looking. The growth trend of the aerosol industry has spread to all sectors of consumption, mainly for personal care, home care, pharmaceuticals for human and veterinary use, and food products. Thanks to the efforts of industries maquiladoras in search of new opportunities, Colombia currently has machinery and inputs to produce aerosols with international quality. Given the diversity of packaging suppliers, needed to meet demand, it is essential to establishing guidelines for quality control of packaging as this directly impacts the quality of the final product. In this paper we reviewed and assessed most representative standards, nationally and internationally, for the quality control of metal aerosol containers, in order to identify the tests applicable to both pharmaceutical industry as a cosmetic.