RESUMO
BACKGROUND: DBS cards have been a big promise for decades. However, blood with low hematocrit (Ht) values results on regular cellulose-based DBS cards in larger spot sizes, compared with blood with high Ht-values. A new material has been developed to solve this problem. RESULTS: This material, based on hydrophilic-coated woven polyester fibers, shows spot sizes independent of the Ht-value of blood. Homogeneity over the spot is within 10% RSD. CONCLUSION: Quantitative measurements over a broad Ht range show nonbiased results compared with whole spot analysis. The cards are experienced as reproducible, robust and easy to use on aspects of punchability and extractability.
Assuntos
Teste em Amostras de Sangue Seco/instrumentação , Teste em Amostras de Sangue Seco/métodos , Hematócrito , Acetaminofen/sangue , Cromatografia Líquida/métodos , Codeína/sangue , Desenho de Equipamento , Humanos , Morfina/sangue , N-Metil-3,4-Metilenodioxianfetamina/sangue , Poliésteres/química , Espectrometria de Massas em Tandem/métodosRESUMO
A method based on liquid chromatography (LC)-mass spectrometry (MS)/MS was developed for sensitive determination of a number of less gas chromatography (GC)-amenable organophosphorus pesticides (OPs; acephate, methamidophos, monocrotophos, omethoate, oxydemeton-methyl and vamidothion) in cabbage and grapes. For extraction, several solvents were evaluated with respect to the possibility of direct injection, matrix-induced suppression or enhancement of response, and extraction efficiency. Overall, ethyl acetate was the most favourable solvent for extraction, although a solvent switch was required. For some pesticide/matrix combinations, reconstitution of the residue after evaporation required special attention. Extracts were analysed on a C18 column with polar endcapping. The pesticides were ionised using atmospheric pressure chemical ionisation on a tandem mass spectrometer in multiple reaction monitoring mode. The final method is straightforward and involves extraction with ethyl acetate and a solvent switch to 0.1% acetic acid/water without further cleanup. The method was validated at the 0.01 and 0.5 mg/kg level, for both cabbage and grapes. Recoveries were between 80 and 101% with R.S.D. < 11% (n = 5). The limit of quantification was 0.01 mg/kg and limits of detection were between 0.001 and 0.004 mg/kg.