Institute for State Control of Veterinary Biologicals and Medicines, Brno, Czech Republic.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(6):983-6. doi: 10.1080/19440049.2013.787651. Epub 2013 May 17.
A sensitive and selective analytical method for the determination of four thyreostats (tapazol, thiouracil, methylthiouracil and propylthiouracil) in cow's milk, lamb's milk, and goat's milk was developed and validated according to 2002/657/EC criteria. Proteins in milk samples were precipitated by acetonitrile and analytes were derivatised with 3-iodobenzylbromide. Afterwards, derivatives were separated from the matrix by liquid-liquid extraction with ethyl acetate as an organic solvent and analysis was carried out using LC-MS/MS in a positive electrospray mode. The method provides, for all determined analytes, decision limits CCα below 1 ng ml(-1) and a detection capability CCβ value below 1.5 ng ml(-1). The stability of analytes in sample extracts stored at various conditions was also tested and evaluated.
建立并验证了 2002/657/EC 准则下的一种可同时测定牛奶、羊奶和羊乳中四种甲状腺抑制剂（他巴唑、硫尿嘧啶、甲巯咪唑和丙基硫氧嘧啶）的灵敏且专一的分析方法。牛奶样品中的蛋白质通过乙腈沉淀，用 3-碘苄基溴衍生化。随后，用乙酸乙酯作为有机溶剂进行液液萃取，将衍生物与基质分离，采用 LC-MS/MS 在正电喷雾模式下进行分析。该方法为所有被测定的分析物提供了决定限 CCα 低于 1ng/ml(-1) 和检测能力 CCβ 值低于 1.5ng/ml(-1)。还测试和评估了在不同条件下保存的样品提取物中分析物的稳定性。
