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1.
J Chromatogr A ; 1625: 461307, 2020 Aug 16.
Artículo en Inglés | MEDLINE | ID: mdl-32709350

RESUMEN

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%.


Asunto(s)
Compuestos de Anilina/química , Bebidas/análisis , Grafito/química , Hidróxidos/química , Ácidos Ftálicos/aislamiento & purificación , Extracción en Fase Sólida/métodos , Ácidos Sulfónicos/química , Ultrasonido/métodos , Adsorción , Ésteres/análisis , Cromatografía de Gases y Espectrometría de Masas , Concentración de Iones de Hidrógeno , Nanocompuestos/química , Concentración Osmolar , Ácidos Ftálicos/análisis , Preparaciones de Plantas/química , Reproducibilidad de los Resultados , Solventes/química , Espectroscopía Infrarroja por Transformada de Fourier , Factores de Tiempo , Difracción de Rayos X
2.
Food Chem ; 321: 126720, 2020 Aug 15.
Artículo en Inglés | MEDLINE | ID: mdl-32276149

RESUMEN

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.


Asunto(s)
Cápsulas/química , Café/química , Embalaje de Alimentos , Extracción Líquido-Líquido/métodos , Polímeros/química , Polipropilenos/química , Cromatografía Líquida de Alta Presión/métodos , Cromatografía Liquida , Análisis de los Alimentos/métodos , Concentración de Iones de Hidrógeno , Límite de Detección , Cloruro de Sodio/química , Espectrometría de Masas en Tándem/métodos
3.
J Chromatogr A ; 1602: 56-63, 2019 Sep 27.
Artículo en Inglés | MEDLINE | ID: mdl-31155144

RESUMEN

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 (0.1-1.9 ng g-1, 0.1-1.2 ng g-1, 0.2-2.3 ng 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.


Asunto(s)
Acrilatos/análisis , Adhesivos/química , Técnicas de Química Analítica/métodos , Cromatografía Líquida de Alta Presión , Tereftalatos Polietilenos/química , Espectrometría de Masas en Tándem , Adhesivos/aislamiento & purificación , Contaminación de Alimentos/prevención & control , Embalaje de Alimentos/normas , Tereftalatos Polietilenos/aislamiento & purificación , Reciclaje , Contaminantes Químicos del Agua/análisis
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