RESUMO
For the first time, structural analogues to bisphenol A were investigated in infant formulas marketed in Brazil. A fast and high throughput UPLC-MS/MS method was established for simultaneous analysis of bisphenol A, B, E, F, and S in complex infant formula matrices. The influence of mobile phase composition on electrospray ionization response in negative mode was studied to improve the detectability of the method. As also, the main sample preparation variables that could affect the extraction and cleanup were screened by the Plackett-Burman design. The method performance characteristics were adequate, including reliable limits of detection (5-10 µg kg-1) and quantification (10-20 µg kg-1) with suitable recoveries (84.2-108.9 %) and precision (≤18 %). Sixty-one infant formulas were analyzed, and 36 % of total samples contained at least one bisphenol analogue, whose levels ranged between 10.9 and 198.9 µg kg-1. Based on a deterministic approach, the estimated daily intakes for babies up to 6 months old, fed exclusively with infant formula, were below the temporary tolerable daily intake of 4 µg kg-1 body weight set for bisphenol A by the European Food Safety Authority.
Assuntos
Fórmulas Infantis , Espectrometria de Massas em Tandem , Compostos Benzidrílicos , Brasil , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida , Exposição Dietética , Humanos , Lactente , Fórmulas Infantis/química , FenóisRESUMO
During the burning of the organic material (firewood) in the drying, combustion may occur incompletely, thus generating smoke contaminants such as polycyclic aromatic hydrocarbons (PAHs) in the furnaces. This study aimed to identify possible contamination by PAHs in soybean grains from storage units in municipalities in the Midwest region that have undergone drying in a direct-fired furnace with firewood as fuel. The soybean grains were collected in different municipalities of the Midwest region of Brazil, totaling 22 samples. A survey of possible contamination of soybean grains by PAHs was carried out using High-Performance Liquid Chromatography. The experiment was carried out in a completely randomized design with three replicates, and the data were subjected to analysis of variance, with means compared by Tukey test. The sum of the groups was: PAH4 - 1.45 µg kg-1 for Edéia (2), PAH8 - 2.97 µg kg-1 for Catalão (19) and PAHT - 5.06 µg kg-1 for Edéia (2); for benzo(a)pyrene, the sum was below 2.0 µg kg-1, not exceeded by the value of 0.64 µg kg-1 for Edéia (1). The values found of PAHs did not exceed the maximum limits established by the European Union, except for infant food.
RESUMO
Polycyclic aromatic hydrocarbons (PAHs) are food-processing contaminants considered to be carcinogenic and genotoxic. Due to its drying process stage, teas may be contaminated with PAHs. The aim of the study was to validate an analytical method involving QuEChERS and HPLC-FLD for the determination of PAH4 in teas and evaluate the contamination levels in 10 different types of teas from Brazil. Recoveries varied from 54% to 99% and relative standard deviations from 1% to 21%. Limits of detection and quantification were from 0.03 to 0.3 µg/kg and 0.1 to 0.5 µg/kg, respectively. Mate tea presented the highest PAH levels, with PAH4 varying from 194 to 1795 µg/kg; followed by black (1.8-186 µg/kg), white (24-119 µg/kg), and green teas (3.1-92 µg/kg). Teas with lowest PAH4 were strawberry, lemongrass, peppermint, and boldo. Only trace levels of PAHs were detected in tea infusions, so apparently it would not affect PAH intake by Brazilian population.
Assuntos
Carcinógenos Ambientais/análise , Contaminação de Alimentos , Hidrocarbonetos Policíclicos Aromáticos/análise , Chá/química , Chás de Ervas/análise , Métodos Analíticos de Preparação de Amostras , Benzo(a)Antracenos/análise , Benzo(a)Antracenos/isolamento & purificação , Benzo(a)pireno/análise , Benzo(a)pireno/isolamento & purificação , Brasil , Carcinógenos Ambientais/isolamento & purificação , Cromatografia Líquida de Alta Pressão , Crisenos/análise , Crisenos/isolamento & purificação , Fluorenos/análise , Fluorenos/isolamento & purificação , Manipulação de Alimentos , Inspeção de Alimentos/métodos , Ilex paraguariensis/química , Limite de Detecção , Oxirredução , Folhas de Planta/química , Hidrocarbonetos Policíclicos Aromáticos/isolamento & purificação , Reprodutibilidade dos Testes , Espectrometria de Fluorescência , Chá/economia , Chás de Ervas/economiaRESUMO
A total of 13 polycyclic aromatic hydrocarbons (PAHs) were surveyed in dry whole soybeans (Glycine max L.) sold for human consumption. The analysed samples were commercialised in vegetarian shops and food stores in Southern Brazil regions. The determination of PAHs levels was carried out by high performance liquid chromatography (HPLC)with fluorescence detection. PAHs were present in 89.7% of the samples. Chrysene (Chy) and 5 methyl chrysene (5MeChy) were the main PAHs detected (76.9% and 71.8%, respectively) followed by dibenzo(ai)pyrene (DaiP), however in a much less percentage of samples (23.1%). Apart from those PAHs, also benzo(a)antracene (BaA), benzo(b)fluoranthene (BbF), benzo(k)fluoranthene (BkF) and benzo(a)pyrene(BaP) were found. The ΣPAH levels in the positive samples ranged from 0.80 to 38.78 µg kg-1, with exception of one sample that reached 204.46 µg kg-1 (ΣPAHs of six compounds). Despite the present contamination there are no maximum limits set for PAHs in soybeans.
Assuntos
Dieta , Exposição Ambiental/análise , Contaminação de Alimentos/análise , Abastecimento de Alimentos/normas , Glycine max , Hidrocarbonetos Policíclicos Aromáticos/análise , Sementes/química , Benzo(a)Antracenos/análise , Benzo(a)pireno/análise , Brasil , Cromatografia Líquida de Alta Pressão , Crisenos/análise , Comércio , Fluorenos/análise , HumanosRESUMO
Brazilian green coffee beans of Coffea arabica and Coffea canephora species were roasted to light, medium, and dark roast degrees and analyzed in relation to furan content by using an in-house validated method based on gas chromatography coupled to mass spectrometry preceded by headspace solid-phase microextraction. Furan was not detected in green coffees, whereas levels between 911 and 5852 µg/kg were found in the roasted samples. Higher concentrations were found in Coffea canephora species and darker ground coffees. Some of the potential furan precursors were observed in significant amounts in green coffee, especially sucrose and linoleic acid, but their concentrations could not be correlated to furan formation. Additionally, coffee brews were prepared from roasted ground coffees by using two different procedures, and furan levels in the beverages varied from <10 to 288 µg/kg. The factor that most influenced the furan content in coffee brew was the brewing procedure.
Assuntos
Coffea/química , Café/química , Contaminação de Alimentos/análise , Manipulação de Alimentos/métodos , Furanos/análise , Temperatura Alta , Contaminação de Alimentos/prevenção & controle , Cromatografia Gasosa-Espectrometria de Massas , Reprodutibilidade dos Testes , Sementes/química , Especificidade da EspécieRESUMO
O diflubenzurom é um pesticida que pode ser utilizado na pecuária como regulador do crescimento de insetos, entre eles a mosca-do-chifre. Esse composto é usualmente administrado oralmente ao gado e é efetivo contra larvas de Díptera que crescem no estrume. O objetivo do presente estudo foi de avaliar a presença de diflubenzurom em amostras de leite cru coletadas de seis vacas leiteiras da raça Girolanda tratadas com uma marca comercial de diflubenzurom em pó. A determinação dos resíduos envolveu a extração do composto com acetato de etila, remoção da gordura com hexano e análise cromatográfica por CLAE com detector UV-Visível (254nm). O princípio ativo diflubenzurom não foi detectado nas seis amostras analisadas (<0,01mg/kg). Dessa forma, os resultados fornecem indicativos de que a utilização do princípio ativo, em níveis suficientes para se obter o efeito inseticida desejado, pode resultar em um leite considerado seguro para o consumo em termos da presença de resíduos de diflubenzurom.
Assuntos
Praguicidas , Resíduos de Praguicidas , Substitutos do LeiteRESUMO
OBJETIVO: Este estudo teve como objetivo determinar os teores de cafeína em diferentes marcas de guaraná em pó disponíveis comercialmente. MÉTODOS: A metodologia analítica utilizada envolveu as etapas de extração com água, limpeza da amostra com acetato de chumbo e determinação por cromatografia líquida de alta eficiência com detector de arranjo de diodos (200-400nm). Foram analisadas 39 amostras adquiridas nas cidades de Campinas e Ribeirão Preto, SP, entre dezembro de 2003 e janeiro de 2004. RESULTADOS: Os teores de cafeína nas amostras apresentaram grande variabilidade, situando-se na faixa de 9,52 a 36,71mg/g de pó, isso se deve, possivelmente, às diferenças de procedência e processo a que a matéria-prima foi submetida. Comparando-se com o pó de café, fonte tradicional de cafeína na dieta, verifica-se que o teor médio de cafeína encontrado no guaraná em pó, dependendo da marca considerada, pode ser até quatro vezes maior. CONCLUSÃO: Entre os consumidores de guaraná em pó esse produto pode ser considerado uma importante fonte de cafeína na dieta, e sua associação com demais produtos que contêm cafeína sugere que seu consumo deve ser controlado, uma vez que controvérsias persistem quanto à dose segura de ingestão da cafeína.
OBJECTIVE: The present study was conducted in order to determine the caffeine levels in different brands of commercially available guaraná powder. METHODS: The analytical methodology involved extraction with water, clean-up with saturated basic lead acetate solution and determination by high performance liquid chromatography with diode array detector (200-400nm). 39 samples were purchased in the cities of Campinas and Ribeirão Preto, SP, between December 2003 and January 2004 and analyzed. RESULTS: The caffeine levels in the samples varied widely ranging from 9.52 to 36.71mg/g, probably due to differences in the origin of the raw material and to the types of processing that the guaraná seeds are submitted to. In comparison to coffee, traditional source of caffeine in the diet, it is possible to verify that the average caffeine content in guaraná powder is about four times higher than the quantities present in coffee. CONCLUSION: Among guaraná powder consumers, this product may be considered as an important source of caffeine in the diet. The association with other products containing caffeine suggests that the guaraná powder consumption should be controlled as the debate regarding caffeine's safe dose of intake remains.
Assuntos
Cafeína/análise , Cromatografia Líquida/métodos , PaulliniaRESUMO
Diflubenzuron has been a pesticide that can be used in cattle breeding as insect growth regulator, and the horn fly has been an insect that can be controlled by the use of this compound. Diflubenzuron has usually been orally administered to cows, and it has been effective against Diptera larvae growing in manure. The objective of the present study was to evaluate the occurrence of diflubenzuron in milk samples collected from six Girolanda dairy cows treated with a commercial brand of diflubenzuron powder. The pesticide residues determination included the compound extraction with ethyl acetate, fat removal with hexane, and chromatography analysis by HPLC with UV detection (254nm). Diflubenzuron was not detected ( 0.01 mg/kg) in any of the six analysed samples. These data indicate that the use of this compound, in adequate doses for achieving a proper insecticide effect, may result in milk considered safe regarding to the presence of diflubenzuron residues.
O diflubenzurom é um pesticida que pode ser utilizado na pecuária como regulador do crescimento de insetos, entre eles a mosca-do-chifre. Esse composto é usualmente administrado oralmente ao gado e é efetivo contra larvas de Díptera que crescem no estrume. O objetivo do presente estudo foi de avaliar a presença de diflubenzurom em amostras de leite cru coletadas de seis vacas leiteiras da raça Girolanda tratadas com uma marca comercial de diflubenzurom em pó. A determinação dos resíduos envolveu a extração do composto com acetato de etila, remoção da gordura com hexano e análise cromatográfica por CLAE com detector UV-Visível (254nm). O princípio ativo diflubenzurom não foi detectado nas seis amostras analisadas ( 0,01mg/kg). Dessa forma, os resultados fornecem indicativos de que a utilização do princípio ativo, em níveis suficientes para se obter o efeito inseticida desejado, pode resultar em um leite considerado seguro para o consumo em termos da presença de resíduos de diflubenzurom.