Ministério da Agricultura, Pecuária e Abastecimento, Laboratório Federal de Defesa Agropecuária - LFDA/RS, Seção Laboratorial Avançada - SLAV/SC, São José, SC, Brazil.
Anal Biochem. 2020 Dec 15;611:114011. doi: 10.1016/j.ab.2020.114011. Epub 2020 Nov 6.
A new procedure for direct extraction and analysis of sulfonamides residues in bovine liver was developed. Briefly, an amount of homogenized sample was mixed with sand and incubated in an ultrasonic bath to promote tissue disruption. After, samples are centrifuged in an empty cartridge with a fritted glass filter. The filtrate was diluted with acetonitrile to precipitate proteins and centrifuged again. The final supernatant was diluted with HPLC mobile phase (ammonium acetate 10 mM: methanol, 85:15) and analyzed with a LC-MS/MS system with electrospray ionization in positive mode. Six sulfonamides were studied, and the procedure showed good recoveries values for all analytes, except for sulfamethoxazole and sulfaquinoxaline. Sulfapirydine was used as internal standard. Consumption of organic solvents was restricted to 2 mL of acetonitrile per sample.
建立了一种用于直接提取和分析牛肝中磺胺类残留的新方法。简要地说，将一定量的匀浆样品与沙子混合，并在超声波浴中孵育以促进组织破碎。然后，将样品在带有玻璃纤维滤板的空柱中离心。将滤液用乙腈稀释以沉淀蛋白质，然后再次离心。最后，将上清液用 HPLC 流动相（10mM 乙酸铵：甲醇，85：15）稀释，并用电喷雾电离正模式的 LC-MS/MS 系统进行分析。研究了 6 种磺胺类药物，除了磺胺甲恶唑和磺胺喹噁啉外，该方法对所有分析物均显示出良好的回收率。磺胺嘧啶被用作内标。每种样品消耗的有机溶剂限制在 2 毫升乙腈。
