Pietruk Konrad, Olejnik Małgorzata, Jedziniak Piotr, Szprengier-Juszkiewicz Teresa
National Veterinary Research Institute, Department of Pharmacology and Toxicology, Al. Partyzantow 57, 24-100 Pulawy, Poland.
National Veterinary Research Institute, Department of Pharmacology and Toxicology, Al. Partyzantow 57, 24-100 Pulawy, Poland.
J Pharm Biomed Anal. 2015 Aug 10;112:50-9. doi: 10.1016/j.jpba.2015.03.019. Epub 2015 Apr 22.
A multi-residue method has been developed and validated for the simultaneous determination of authorized (decoquinate, diclazuril, halofuginone, lasalocid, maduramicin, monensin, narasin, nicarbazin, robenidine, salinomycin and semduramicin) and non-authorized (amprolium, clopidol, ethopabate and toltrazuril) coccidiostats in animal feed. Feed samples were extracted with basic followed by acidified solution in methanol and, after centrifugation, were injected directly into LC-MS/MS system. Detection was performed in selected reaction monitoring mode with both positive and negative electrospray ionization. The time efficient validation experiment has verified the robustness of a method in different types of feed and on two separate LC-MS/MS instruments. The comparison of different quantification methods demonstrated that, against expectations, the standard addition did not prove better in comparison with matrix-matched calibration curve. Although the sample preparation was very easy, the observed matrix effects were not significant for the most part but they could explain the problems with the quantification of some coccidiostats.
已开发并验证了一种多残留方法，用于同时测定动物饲料中已批准的（癸氧喹酯、地克珠利、常山酮、拉沙洛西钠、马杜霉素、莫能菌素、那拉菌素、尼卡巴嗪、氯苯胍、盐霉素和赛杜霉素）和未批准的（氨丙啉、氯羟吡啶、乙氧酰胺苯甲酯和托曲珠利）抗球虫药。饲料样品先用碱性溶液提取，然后用酸化的甲醇溶液提取，离心后直接注入液相色谱-串联质谱系统。采用正、负离子电喷雾电离，在选择反应监测模式下进行检测。高效的验证实验验证了该方法在不同类型饲料和两台不同液相色谱-串联质谱仪器上的稳健性。不同定量方法的比较表明，与预期相反，标准加入法与基质匹配校准曲线相比并没有更好的效果。虽然样品制备非常简单，但观察到的基质效应在很大程度上并不显著，但它们可以解释一些抗球虫药定量中的问题。
