Turnipseed Sherri B, Andersen Wendy C, Karbiwnyk Christine M, Madson Mark R, Miller Keith E
Animal Drugs Research Center, Food and Drug Administration, Denver Federal Center, Denver, CO 80225, USA.
Rapid Commun Mass Spectrom. 2008 May;22(10):1467-80. doi: 10.1002/rcm.3532.
This paper describes the development and optimization of a multi-residue veterinary drug screening method for whole milk. The drug residues of regulatory interest in milk include beta-lactams, sulfonamides, tetracyclines, fluoroquinolones, and macrolides. Milk samples were extracted with acetonitrile and the samples were then subjected to a clean-up procedure using a bonded solid-phase extraction cartridge and a molecular weight cut-off filter. Liquid chromatography/tandem mass spectrometry (LC/MS/MS) triple quadrupole electrospray methods were developed to monitor for the drugs in milk. Since established tolerance levels are set for most of these drugs in milk, the initial screening procedure was semi-quantitative, where samples were compared to the response of a positive control. The positive control, consisting of an extract from a portion of milk fortified with the drugs at half their allowed levels, was used to set the laboratory's minimum response criteria for unknown samples. Confirmatory analyses, with additional ion transitions for each residue, were performed on the same extracts.
本文描述了一种全脂牛奶中多残留兽药筛查方法的开发与优化。牛奶中受监管关注的药物残留包括β-内酰胺类、磺胺类、四环素类、氟喹诺酮类和大环内酯类。牛奶样品用乙腈提取,然后使用键合固相萃取柱和分子量截留滤器进行净化处理。开发了液相色谱/串联质谱(LC/MS/MS)三重四极杆电喷雾方法来监测牛奶中的药物。由于为牛奶中的大多数这些药物设定了既定的耐受水平,初始筛查程序是半定量的,即将样品与阳性对照的响应进行比较。阳性对照由添加了允许水平一半药物的部分牛奶提取物组成,用于设定实验室对未知样品的最低响应标准。对相同的提取物进行确证分析,对每个残留进行额外的离子跃迁分析。