Pietruk Konrad, Olejnik Małgorzata, Posyniak Andrzej
a Department of Pharmacology and Toxicology , National Veterinary Research Institute , Pulawy , Poland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018 Aug;35(8):1508-1518. doi: 10.1080/19440049.2018.1461256. Epub 2018 Jun 6.
A confirmatory multi-residue method was developed for the determination in milk of 19 coccidiostats (amprolium, arprinocid, clazuril, clopidol, decoquinate, diclazuril, ethopabate, halofuginone, lasalocid, maduramicin, monensin, narasin, nicarbazin, nequinate, robenidine, salinomycin, semduramicin, toltrazuril sulfone and toltrazuril sulfoxide). Sample preparation utilising extraction with organic solvent and clean up by SPE and freezing was found reliable and time-efficient. Optimised chromatography and MS conditions with positive and negative ESI achieved sufficient sensitivity and selectivity. Validation experiments has proven method usefulness for routine analysis of coccidiostats in milk samples. An on-farm study conducted on dairy cows fed with experimentally contaminated feed with salinomycin and lasalocid showed negligible transfer to milk. No residues of lasalocid were found in collected samples. Salinomycin was found only in 5 of 168 samples analysed, while the concentrations of salinomycin in those samples (0.119-0.179 µg kg) was significantly below the limit of salinomycin in milk set by European Union legislation. Such low concentrations of both coccidiostats cannot be explained by conjugation during dairy cows' metabolism, as shown by experiments with enzymatic hydrolysis.
开发了一种确证性多残留方法，用于测定牛奶中的19种抗球虫药（氨丙啉、阿普林诺西德、氯羟吡啶、氯吡醇、癸氧喹酯、地克珠利、乙氧酰胺苯甲酯、常山酮、拉沙洛西钠、马杜霉素、莫能菌素、那拉菌素、尼卡巴嗪、奈喹酯、氯苯胍、盐霉素、赛杜霉素、托曲珠利砜和托曲珠利亚砜）。利用有机溶剂萃取、固相萃取净化和冷冻进行样品制备，结果可靠且高效省时。采用正、负离子电喷雾电离的优化色谱和质谱条件，实现了足够的灵敏度和选择性。验证实验证明该方法可用于牛奶样品中抗球虫药的常规分析。对饲喂经盐霉素和拉沙洛西钠实验性污染饲料的奶牛进行的农场研究表明，药物向牛奶中的转移可忽略不计。在采集的样品中未发现拉沙洛西钠残留。在168份分析样品中，仅5份检测到盐霉素，且这些样品中盐霉素的浓度（0.119 - 0.179 µg/kg）显著低于欧盟法规规定的牛奶中盐霉素的限量。酶解实验表明，奶牛代谢过程中的结合作用无法解释这两种抗球虫药如此低的浓度。
