RESUMO
Phthalates have been used extensively as plasticizers to improve the flexibility of polymers, and they also have found many industrial applications. They are ubiquitous in the environment and have been detected in a variety of environmental and biological matrices. The goal of this study was to develop a method for the determination of 17 phthalate esters in house dust. This method involved sonication extraction, sample cleanup using solid phase extraction, and isotope dilution GC/MS/MS analysis. Method detection limits (MDLs) and recoveries ranged from 0.04 to 2.93 µg/g and from 84 to 117%, respectively. The method was applied to the analysis of phthalates in 38 paired household vacuum samples (HD) and fresh dust (FD) samples. HD and FD samples compared well for the majority of phthalates detected in house dust. Data obtained from 126 household dust samples confirmed the historical widespread use of bis(2-ethylhexyl) phthalate (DEHP), with a concentration range of 36 µg/g to 3840 µg/g. Dibutyl phthalate (DBP), benzyl butyl phthalate (BzBP), diisononyl phthalate (DINP), and diisodecyl phthalate (DIDP) were also found in most samples at relatively high concentrations. Another important phthalate, diisobutyl phthalate (DIBP), was detected at a frequency of 98.4% with concentrations ranging from below its MDL of 0.51 µg/g to 69 µg/g.
Assuntos
Poeira/análise , Ácidos Ftálicos/análise , Cromatografia Gasosa-Espectrometria de Massas , Habitação , Controle de Qualidade , Extração em Fase SólidaRESUMO
ISO/CD 18857-2 (International Organization for Standardization, Geneva) describes a new international standard method for the determination of octylphenol, nonylphenol, their mono- and diethyoxylates, and bisphenol A in nonfiltered samples of drinking, ground, surface, and wastewater. The method is based on the extraction of the analytes from an acidified water sample by solid phase extraction, solvent elution, derivatization, and determination by gas chromatography with mass spectrometric detection. For validation of this method, 14 laboratories from 4 different countries in Europe and Canada participated in an interlaboratory trial to determine the performance characteristics of the method, which are intended for publication in the corresponding standard. The interlaboratory trial was evaluated according to ISO 5725-2 and included two duplicate nonfiltered water samples: surface water containing the target compounds in an analyte concentration range from 0.05 to 0.4 microg/L and wastewater containing the target compounds in a concentration ranged from 0.1 to 5 microg/L. The repeatability variation coefficients (within-laboratory precision) varied for all samples and compounds between 1.9 and 7.8%, showing a sufficiently high repeatability of the method. The reproducibility variation coefficients (between-laboratory precision) were found to vary within a satisfactory range of 10.0-29.5% for surface water and 10.8-22.5% for wastewater. The recoveries as a measure of accuracy varied from 98.0 to 144.1% for surface water and from 95.4 to 108.6% for wastewater. The determined concentrations of the samples compared well to the "true" values, thus showing very satisfactory accuracy of the method. In the chromatogram of the surface water sample, a high unresolved background made up of coextractable matrix compounds was apparent. It is conceivable that compounds from this background may be responsible for enhanced recoveries of 144.1% for 4-nonylphenol (mixture of isomers) and of 123.4% for 4-nonylphenol monoethoxylate (mixture of isomers) in the surface water samples. The isotope-marked standard compounds developed in this context proved to be reliable internal standards that allow a precise and accurate quantitation of all compounds specified in ISO/CD 18857-2. The results of the interlaboratory trial confirmed that the analytical method is robust and reliable and can be used as a standard method to analyze the target compounds in water samples.
Assuntos
Cromatografia Gasosa-Espectrometria de Massas/métodos , Fenóis/análise , Poluentes da Água/análise , Compostos Benzidrílicos , Cromatografia Gasosa-Espectrometria de Massas/normas , Limite de DetecçãoRESUMO
Human exposure to bisphenol A (BPA) has recently received special attention. It has been shown that exposure to BPA may occur through the consumption of beverages or foods that have been in contact with polycarbonate (PC) plastic containers or epoxy resins in food packaging. A BPA migration study was conducted using a variety of plastic containers, including polycarbonate baby bottles, non-PC baby bottles, baby bottle liners, and reusable PC drinking bottles. Water was used to simulate migration into aqueous and acidic foods; 10% ethanol solution to simulate migration to low- and high-alcoholic foods; and 50% ethanol solution to simulate migration to fatty foods. By combining solid-phase extraction, BPA derivatization and analysis by GC-EI/MS/MS, a very low detection limit at the ng l(-1) level was obtained. Migration of BPA at 40 degrees C ranged from 0.11 microg l(-1) in water incubated for 8 h to 2.39 microg l(-1) in 50% ethanol incubated for 240 h. Residual BPA leaching from PC bottles increased with temperature and incubation time. In comparison with the migration observed from PC bottles, non-PC baby bottles and baby bottle liners showed only trace levels of BPA. Tests for leachable lead and cadmium were also conducted on glass baby bottles since these represent a potential alternative to plastic bottles. No detectable lead or cadmium was found to leach from the glass. This study indicated that non-PC plastic baby bottles, baby bottle liners and glass baby bottles might be good alternatives for polycarbonate bottles.
Assuntos
Estrogênios não Esteroides/análise , Contaminação de Alimentos/análise , Embalagem de Alimentos , Fenóis/análise , Cimento de Policarboxilato/análise , Compostos Benzidrílicos , Alimentação com Mamadeira , Utensílios de Alimentação e Culinária , Humanos , Lactente , Recém-Nascido , Limite de Detecção , Fenóis/química , Cimento de Policarboxilato/química , Esterilização/métodos , Temperatura , Água/análise , Água/químicaRESUMO
The alkaloid composition of the aerial parts and roots of PHYSALIS PERUVIANA was analysed by capillary GC (GC (2)), GC (2)-MS and GC (2)-FTIR. Eight alkaloids were identified, three of those alkaloids are 3beta-acetoxytropane and two N-methylpyrrolidinylhygrine isomers, which were not previously found in the genus PHYSALIS. A reproduction of the identification of alkaloids detected in the plant by the use of retention indices has been proposed.