O presente trabalho descreve a aplicação bem sucedida da microextração em sorvente empacotado e cromatografia líquida com detecção de arranjo de diodos (MEPS/LC-DAD) para a determinação simultânea das sulfonamidas (sulfacetamida, sulfadiazina, sulfatiazol, sulfametazina sulfametoxipiridazina e sulfametoxazol) em amostras de ovos. As variáveis MEPS (pH da amostra, número de ciclos aspirar/dispensar, força iônica e procedimento de dessorção) foram otimizados para aumentar a sensibilidade analítica do método. O método apresentou linearidade na faixa de concentração de 30 ng g -1 (limite de quantificação, LOQ) a 300 ng g -1. Este valor de LOQ é inferior ao limite máximo de resíduo (LMR) preconizado para sulfonamidas em amostras de ovos (100 µg kg -1 ). As taxas de recuperação foram adequadas para todos os analitos (> 94%), bem como os dados de precisão inter-ensaio, com coeficientes de variação inferiores a 10%. Com base na validação analítica, a metodologia MEPS/LC é adequada para a determinação de sulfonamidas em amostras de ovos.The present work describes a successful application of microextraction packed sorbent and liquid chromatography with diode array detection (MEPS/LC-DAD) for simultaneous determination of the sulfonamides (sulfacetamide, sulfadiazine, sulfathiazole, sulfamethazine, sulfamethoxypiridazine and sulfamethoxazole) in egg samples. The MEPS variables (pH of the sample, draw-eject cycles, ionic strength, and desorption procedure) were optimized, in order to improve the sensitivity of the proposed method. The method was shown to be linear at concentrations ranging from 30 ng g -1 (limit of quantification, LOQ) to 300 ng g -1 . This LOQ value is lower than those established as the maximum residue limit (MRL) for egg samples (100 µg kg -1 ). The accuracy values were adequate for all analytes (> 94%), as well as the inter-day precision data, with coefficient of variation lower than 10%. On the basis of analytical validation, the MEPS/LC methodology has been shown to be a promising alternative for analysis of sulfonamides in egg samples.
Keywords: MEPS, sulfonamides, liquid chromatography, egg
IntroductionSulfonamides (SAs) are a group of synthetic antibiotics that have played an important role as effective chemotherapeutics in bacterial and protozoan infections in veterinary medicine practice. Subtherapeutic doses of more than ten SAs are routinely used in food-producing animals for prophylactic and growth-promoting purposes. SAs residues could be potentially toxic to aquatic organisms and humans because of their carcinogenic potency and possible antibiotic resistance. [1][2][3][4] There are no sulfonamides approved for use in laying hens. The use of veterinary drugs for medicinal purposes in laying hens could result in violative drug residues in food meant for human consumption. Of all the marketed SAs, only sulfamethazine and sulfadimethoxine have been approved for use in chickens. Furthermore, this approval extends to broilers only, not laying hens. 4,5 To safeguard human health, many countries ...