Widstrand Christine, Larsson Fredrik, Fiori Maurizio, Civitareale Cinzia, Mirante Sabrina, Brambilla Gianfranco
MIP Technologies AB, Research Park Ideon, SE-223 70 Lund, Sweden.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 May 5;804(1):85-91. doi: 10.1016/j.jchromb.2003.12.034.
Methods based on molecular recognition mechanisms for the clean-up of veterinary drugs and their residues, such as immuno-, receptor- and acceptor-affinity and molecularly imprinted polymers (MIPs), have been described as selective tools to improve the selectivity and the reliability of analytical results. In this work, we tested the extraction recovery performances of a MISPE column, designed for multi-residual clean-up of beta-agonists. For this purpose, 18 different samples of calf urine were spiked at 0.25, 0.50 and 1.00 ppb with pooled standard solutions of clenbuterol (Clen), tulobuterol (Tolu), isoxsuprine (Isox), brombuterol (Brom), mapenterol (Mape) and ractopamine (Racto) and analysed on two independent analytical sessions, on a LC-MS/MS ion trap detector. Averaged recoveries, constant for each molecule considered, were 64.6% for Racto, 63.0% for Salm, 59.9% for Form, 54.7% for Brom, 52.0% for Clen, 41.8% for Mape, 38.6% for Tolu and 34.5% for Isox, respectively. Reproducibility studies gave a CV < 11% at the 0.25 ppb level. The decision limit for the identification of the target drugs ranged from 0.01 ppb for mapenterol to 0.19 ppb for salmeterol, when considering one precursor, and two product ions as identification points. Such findings indicate that the choice of the appropriate molecule as template in the MIP preparation is the critical factor to guarantee a reliable analytical multi-residue approach for beta-agonists, despite the structural differences among molecules exploiting almost the same pharmacological effect.
基于分子识别机制的用于清理兽药及其残留的方法，如免疫、受体和受体亲和以及分子印迹聚合物（MIPs），已被描述为提高分析结果选择性和可靠性的选择性工具。在这项工作中，我们测试了一种用于β-激动剂多残留清理的MISPE柱的萃取回收性能。为此，将18个不同的小牛尿液样品分别加入浓度为0.25、0.50和1.00 ppb的克伦特罗（Clen）、妥布特罗（Tolu）、异克舒令（Isox）、溴布特罗（Brom）、马喷特罗（Mape）和莱克多巴胺（Racto）混合标准溶液，并在两个独立的分析时段，使用液相色谱-串联质谱离子阱检测器进行分析。对于所考虑的每个分子，平均回收率分别为：莱克多巴胺64.6%、沙丁胺醇63.0%、福莫特罗59.9%、溴布特罗54.7%、克伦特罗52.0%、马喷特罗41.8%、妥布特罗38.6%、异克舒令34.5%。重现性研究表明，在0.25 ppb水平下变异系数（CV）<11%。当将一个前体离子和两个产物离子作为识别点时，目标药物鉴定的决策限范围为马喷特罗0.01 ppb至沙丁胺醇0.19 ppb。这些发现表明，尽管利用几乎相同药理作用的分子之间存在结构差异，但在MIP制备中选择合适的分子作为模板是保证β-激动剂可靠分析多残留方法的关键因素。
