Validação de método analítico para determinar a migração de ε-caprolactama das embalagens para alimentos gordurosos

ε-Caprolactam (CAP) is a monomer of nylon 6 used as food packaging for bologna sausage, turkey blanquettes, fowl breast, pâtés and ham luncheon meat. After polymerization a part of the monomer can remain in the packaging and migrate into the food. The aim of this work was develop and validate a single laboratory method to determine CAP in ethanol 95% that simulates fatty food characteristics. Thus, linear range was 2 to 32 mg/L of CAP, detection and quantification limits were 0.83 and 1.63 mg/L, respectively. Repeatability showed Hor Rat values lower than 2 while recovery range was 97.5 to 106.5%. The method was considered adequate for purpose.

Determinação de arsênio em amostras da cadeia produtiva de frangos de corte por espectrometria de absorção atômica com forno de grafite

Chicken meat is largely consumed in human nutrition and it is produced in extremely large scale in some countries, including Brazil. In this work graphite furnace atomic absorption spectrometry was used for determination of arsenic in chicken and chicken production-related samples. These samples were digested employing a microwave-assisted procedure in closed vessels using a 7 mol L-1 nitric acid solution plus concentrated hydrogen peroxide. The concentration range of total As determined in chicken production-related samples varied from 1.30 to 29.8 mg kg-1 of As. The detection and quantification limits reached were 0.055 and 0.182 mg kg-1, respectively (n = 15).

Desenvolvimento e validação do método QuEChERS na determinação de resíduos de medicamentos veterinários em leite e carne de búfalo

Analytical methods were developed and validated to determine residues of veterinary drugs in buffalo milk and meat, using the QuEChERS method and gas chromatography-mass spectrometry. Both milk and meat, at 2 g of sample, 4 mL of acetonitrile, 0.8 g of MgSO4 and 0.2 g of NaCl, were used in the liquid-liquid partition, whereas 50 mg of C18, 50 mg of PSA and 150 mg of MgSO4 were employed in the dispersive solid-phase extraction (d-SPE). The methods showed sensitivity, precision and accuracy. The quantitation limits were in agreement with the maximum residue limit established by the Codex Alimentarius, FAO and WHO.

Avaliação de tratamentos da amostra em microescala para a determinação de K, Mg, Na e Zn em carnes por técnicas de espectrometria atômica

This paper describes the development of methods in micro-scale for the determination of K, Mg, Na and Zn in meat by atomic spectrometry techniques. The limits of detection (LOD) for K and Na by microdigestion were 0.18 and 0.20 mg g-1, respectively whereas LOD for Mg and Zn by microsolubilization with TMAH were 2.40 and 18.4 µg g-1, respectively. The RSD values were lower than 6.0% and the CRMs analyzed showed values with 95% agreement. The proposed methods are simple, fast and use small amounts of sample (around 10 mg) yet do not require special equipment for sample preparation.