建立并验证了一种用于检测牛奶中 11 种抗球虫药的液相色谱-串联质谱法。
Development and validation of a liquid chromatographic-tandem mass spectrometric method for determination of eleven coccidiostats in milk.
机构信息
Joint Research and Training Laboratory on Separation Techniques, Eötvös Loránd University, 1117 Budapest, Pázmány Péter Sétány 1/A, Hungary.
Central Agricultural Office, Food and Feed Safety Directorate, Feed Investigation National Reference Laboratory, 1144 Budapest, Remény utca 42, Hungary.
出版信息
Food Chem. 2012 Jul 15;133(2):536-43. doi: 10.1016/j.foodchem.2012.01.022. Epub 2012 Jan 25.
A reversed phase liquid chromatographic-tandem mass spectrometric method with simple solvent extraction and purification by solid phase extraction (SPE) has been developed for the determination of coccidiostats in milk. For sample preparation matrix solid phase dispersion, extraction by organic solvent and SPE with different cartridges were also tested. The compounds determined include lasalocid, narasin, salinomycin, monensin, semduramicin, maduramicin, robenidine, decoquinate, halofuginone, nicarbazin and diclazuril. Main steps of the method are addition of acetonitrile to the milk samples, centrifugation, removal of matrix by SPE, concentration by evaporation and LC-MS-MS determination. During a 15 min time segmented chromatographic run compounds are ionised either positively or negatively. Calculated recoveries range between 77.1% and 118.2%. Maximum levels are in the range of 1-20 μg/kg. The developed method was validated in line with the requirements of Commission Decision 2002/657/EC (2002). It is applicable for control of coccidiostat residues in milk as indicated in Regulation 124/2009/EC (2009).
建立了一种反相液相色谱-串联质谱法，通过固相萃取（SPE）进行简单的溶剂萃取和净化，用于牛奶中抗球虫药的测定。还测试了用于样品制备的基质固相分散法、有机溶剂提取和不同小柱的 SPE。测定的化合物包括拉沙菌素、那拉菌素、盐霉素、马杜霉素、赛杜霉素、马杜霉素、罗贝林、癸氧喹酯、二硝托胺、尼卡巴嗪和地克珠利。该方法的主要步骤是向牛奶样品中加入乙腈，离心，通过 SPE 去除基质，蒸发浓缩，然后进行 LC-MS-MS 测定。在 15 分钟的分段色谱运行过程中，化合物要么正离子化，要么负离子化。计算的回收率在 77.1%至 118.2%之间。最高水平在 1-20μg/kg 范围内。所建立的方法符合欧盟委员会 2002/657/EC 号决议（2002 年）的要求。根据 2009 年欧盟委员会第 124/2009/EC 号法规（2009 年），该方法适用于牛奶中抗球虫药残留的控制。
Zotero 插件