RESUMO
An on-line solid phase extraction coupled to liquid chromatography with UV detection (SPE/LC-UV) method was automated by the multisyringe flow-injection analysis (MSFIA) system for the determination of three phthalic acid esters (PAEs). The PAEs determined in drinking water stored in polyethylene terephthalate (PET) bottles of ten commercial brands were dimethyl phthalate (DMP), diethyl phthalate (DEP) and dibutyl phthalate (DBP). C18-bonded silica membrane was used for isolation and enrichment of the PAEs in water samples. The calibration range of the SPE/LC-UV method was 2.5-100µgL-1 for DMP and DEP and 10-100µgL-1 for DBP with correlation coefficients (r) ranging from 0.9970 to 0.9975. Limits of detection (LODs) were between 0.7 and 2.4µgL-1. Inter-day reproducibility performed at two concentration levels (10 and 100µgL-1) expressed as relative standard deviation (%RSD) were found in the range of 0.9-4.0%. The solvent volume was reduced to 18mL with a total analysis time of 48min per sample. The major species detected in bottled water samples was DBP reaching concentrations between 20.5 and 82.8µgL-1. The recovery percentages for the three analytes in drinking water were 80-115%. The migration test showed a great variation in the sum of migrated PAEs level (10.2-50.6µgL-1) among the PET bottle brands analyzed indicating that the presence of these contaminants in the plastic containers may depend on raw materials and the conditions used during their production process.
Assuntos
Cromatografia Líquida/instrumentação , Cromatografia Líquida/métodos , Água Potável/análise , Ácidos Ftálicos/análise , Ácidos Ftálicos/isolamento & purificação , Plásticos/química , Poluentes Químicos da Água/análise , Humanos , Extração em Fase Sólida , Raios Ultravioleta , Poluentes Químicos da Água/isolamento & purificaçãoRESUMO
A novel and fast method based on the solid phase extraction (SPE) coupled to a flow injection system for the determination of caffeine in coffee beans was developed. The caffeine extraction of coffee beans was carried out with hot water. A C18 reverse-phase mini-column was coupled to a continuous flow manifold to carry out the on-line SPE and the quantification of caffeine from aqueous extracts. Column length, retention time, elution volume, extracting solution and injection volume were evaluated. The retention time was of 90s and the elution was carried out with 400 µL of a methanol:water mixture (25:75). The proposed on-line SPE was compared against a chloroform extraction from aqueous extracts. With the proposed method the sample preparation was minimised and the sample throughput was increased (10 determination/h) because no dilution was required. Green coffee beans and beans with different roasting degree were analyzed.
Assuntos
Cafeína/análise , Cafeína/isolamento & purificação , Coffea/química , Análise de Injeção de Fluxo/métodos , Sementes/química , Extração em Fase Sólida/métodos , Automação , Cromatografia Líquida de Alta Pressão/métodos , Culinária , Análise de Injeção de Fluxo/instrumentaçãoRESUMO
Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV). An automated system using on-line solid extraction and High Performance Liquid Chromatography (HPLC) with ultraviolet (UV) detection was developed and validated for pharmacokinetic analysis of didanosine in dog plasma. Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma. Extraction was carried out on C18 cartridges, with high extraction yield as stationary phase, whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer, acetonitrile (KH2PO4: acetonitrile: 96:4, v/v) and 0.5% (w/v) of heptane sulphonic acid. The pH was adjusted to 6.5 with triethylamine. All samples and standard solutions were chromatographed at 28 °C. For an isocratic run, the flux was 1.0 mL/min, detection was at 250 nm and injected volume was 20 µL. The method was selective and linear for concentrations between 50 and 5000 ng/mL. Drug stability data ranged from 96% to 98%, and limit of quantification was 25 ng/mL. Extraction yield was up to 95%. Drug stability in dog plasma was kept frozen at -20 °C for one month after three freeze-thaw cycles, and for 24 h after processing in the auto sampler. Assay was successfully applied to measure didanosine concentrations in plasma dogs.