RESUMO
In this study, the ultrasonic-assisted dispersive solid phase extraction (UA-d-SPE) method coupled to gas chromatography-mass spectrometry (GC-MS) was applied for the analysis of phthalate esters in drinking water and distilled herbal beverages (Rosa, Mentha, Cichorium). A new nanocomposite based on layered double hydroxide supported on graphene oxide was synthesized and modified by sulfonated polyaniline via a simple one-pot in-situ polymerization method. The structure and morphology of the nanocomposite was confirmed by means of complementary techniques: Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, and transmission electron microscopy. The effects of key parameters including adsorbent mass, type and amount of back extraction solvent, extraction and desorption time, pH of the solution and ionic strength were optimized and good precision and sensitivity were achieved. Under the optimum conditions, the limits of detection were between 0.06-0.3 ng mL-1 in aqueous solutions. The hybrid nanomaterial exhibited good adsorption ability toward phthalates in drinking water and distilled herbal beverages. The relative standard deviations (RSD%) for beverage samples varied from 0.1% to 9.9% (n = 3). The relative recoveries varied from 54.5% to 112.6%.
Assuntos
Compostos de Anilina/química , Bebidas/análise , Grafite/química , Hidróxidos/química , Ácidos Ftálicos/isolamento & purificação , Extração em Fase Sólida/métodos , Ácidos Sulfônicos/química , Ultrassom/métodos , Adsorção , Ésteres/análise , Cromatografia Gasosa-Espectrometria de Massas , Concentração de Íons de Hidrogênio , Nanocompostos/química , Concentração Osmolar , Ácidos Ftálicos/análise , Preparações de Plantas/química , Reprodutibilidade dos Testes , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier , Fatores de Tempo , Difração de Raios XRESUMO
Migration of N,N-Bis(2-hydroxyethyl) alkyl(C8-C18)amines from five different polypropylene capsules to Tenax® and coffee powder have been studied. A single step extraction-cleanup procedure using salting out liquid-liquid extraction (SALLE) method followed by ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was applied. The critical parameters on the SALLE procedure such as extracting solvent, extracting volume, sample pH, salt and its concentration were optimized. The recovery values were in the range of 87.5%-106.5%. The %RSD were lower than 3.7%. The limit of detection was improved from 2.3 ng/g in Tenax® to 0.8 ng/g in coffee. The results indicated that the analyzed compounds have the potential to migrate from the polypropylene capsule containers to the coffee. In most of the cases, the migrated values were higher in Tenax® than in coffee in a range between 1.8 and 61%. One sample did not comply with the specific migration limit established by the European Commission.
Assuntos
Cápsulas/química , Café/química , Embalagem de Alimentos , Extração Líquido-Líquido/métodos , Polímeros/química , Polipropilenos/química , Cromatografia Líquida de Alta Pressão/métodos , Cromatografia Líquida , Análise de Alimentos/métodos , Concentração de Íons de Hidrogênio , Limite de Detecção , Cloreto de Sódio/química , Espectrometria de Massas em Tandem/métodosRESUMO
This article presents fabric phase sorptive extraction (FPSE) as a simple and effective pre-concentration method for the enrichment of acrylate compounds in different food simulants and subsequent analysis of the extracts by ultra-high-performance liquid chromatography with mass spectrometric detection (UPLC-MS). Acrylate compounds come from acrylic adhesives used commonly for sticking the paper labels on polyethylene terephthalate (PET) bottles and therefore, they may exist in recycled polyethylene terephthalate (rPET). Four acrylates were studied: ethylene glycol dimethacrylate (EGDM), pentaerythritol triacrylate (PETA), triethylene glycol diacrylate (TEGDA) and trimethylolpropane triacrylate (TMPTA). Five different types of FPSE media coated with different sol-gel sorbents were studied and finally sol-gel polyethylene glycol- polypropylene glycol-polyethylene glycol triblock copolymer (PEG-PPG-PEG) coated FPSE media was chosen for its satisfactory results. The optimal conditions affecting the extraction efficiency of compounds were determined in three different food simulants. Statistical evaluation of this method reveals good linearity and precision. Under the optimized conditions, the method provided limits of detection of the compounds in the range of (0.1-1.9â¯ngâ¯g-1, 0.1-1.2â¯ngâ¯g-1, 0.2-2.3â¯ngâ¯g-1) in EtOH 10%, HAc 3% and EtOH 20% and the enrichment factor values (EFs) after applying N2 were in the range of 11.1-25.0, 13.8-26.3, 8.3-21.9, in simulants A, B and C respectively. The optimized method was applied successfully to analyze thirteen types of recycled PET samples. Acrylates were found in some of the samples at ng g-1 levels.