Food Safety Department, Teagasc Food Research Centre, Ashtown, Dublin, Ireland.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2013;30(6):958-69. doi: 10.1080/19440049.2013.794306. Epub 2013 Jun 3.
In this paper, methods were developed to measure coccidiostats in bovine milk, duck muscle and non-avian species. The methods were validated to the maximum levels and MRLs laid down in European Union legislation. A simple sample preparation procedure was developed for the isolation of coccidiostat residues from bovine, ovine, equine, porcine and duck muscle tissue, based on solvent extraction with acetonitrile and concentration. An alternative method had to be developed for milk samples based on the QuEChERS sample preparation approach because of the high water content in this matrix. Milk samples were adjusted to basic pH with sodium hydroxide and extracted by using a slurry of acetonitrile, MgSO4 and NaCl. Purified sample extracts were subsequently analysed by using UHPLC-MS/MS in a 13.2-min chromatographic run. It was found that the use of rapid polarity switching enabled both negatively and positively charged ions to be analysed from a single injection. By using this approach, solvent usage was reduced significantly and sample throughput improved. The method was validated for the analysis of 20 coccidiostats (arprinocid, clopidol, decoquinate, diclazuril, diaveridine, ethopabate, halofuginone, laidlomycin, lasalocid, maduramicin, monensin, narasin, nequinate, nicarbazin, robenidine, salinomycin, semduramicin, toltrazuril, toltrazuril sulphoxide and toltrazuril sulphone) in muscle and milk. The method is quantitative for toltrazurils, but it cannot be used for confirmation because only the precursor ion is monitored. Accuracy values for muscle ranged from 80% to 125%, while CCα ranged from 2.2 µg kg(-1) for clopidol to 122 µg kg(-1) for toltrazuril sulphoxide. Bovine milk accuracy ranged from 84% to 120% for all analytes except maduramicin, semduramicin and salinomycin, for which the values were higher. CCα values achieved ranged from 1.1 µg kg(-1) for arprinocid, nequinate and lasalocid to 27 µg kg(-1) for toltrazuril.
本文开发了用于检测牛奶、鸭肉和非禽类物种中抗球虫药的方法。该方法经验证符合欧盟法规规定的最高残留限量和最大残留限量。本文开发了一种简单的样品前处理方法，用于从牛、羊、马、猪和鸭肉组织中分离抗球虫药残留，该方法基于用乙腈和浓缩溶剂提取。由于该基质水分含量高，因此必须为牛奶样品开发替代方法，基于 QuEChERS 样品制备方法。将牛奶样品用氢氧化钠调至碱性 pH 值，然后用乙腈、硫酸镁和氯化钠的浆液提取。随后，使用超高效液相色谱-串联质谱法（UHPLC-MS/MS）在 13.2 分钟的色谱运行中分析净化后的样品提取物。结果发现，使用快速极性切换能够从单个进样中同时分析带负电荷和带正电荷的离子。通过使用这种方法，大大减少了溶剂的使用，提高了样品的通量。该方法经验证可用于分析肌肉和牛奶中的 20 种抗球虫药（阿苯达唑、氯羟吡啶、地克珠利、二氯二甲吡啶、二甲氧嘧啶、乙氧酰胺苯甲酯、哈尔菌素、拉沙里菌素、马杜霉素、莫能菌素、那拉菌素、尼卡巴嗪、喹乙醇、硝羟喹啉、罗硝唑、盐霉素、萨林霉素、托曲珠利、托曲珠利亚砜和托曲珠利砜）。该方法对托曲珠利是定量的，但不能用于确证，因为只监测前体离子。肌肉的准确度值在 80%至 125%之间，而 CCα 值在氯羟吡啶的 2.2μg/kg 至托曲珠利亚砜的 122μg/kg 之间变化。除了马杜霉素、萨林霉素和盐霉素外，牛奶中所有分析物的准确度值均在 84%至 120%之间，而这三种物质的准确度值较高。CCα 值的范围从阿苯达唑、尼卡巴嗪和拉沙里菌素的 1.1μg/kg 到托曲珠利的 27μg/kg。
