Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, 97105-900 Santa Maria, RS, Brazil.
Laboratory of Pesticide Residue Analysis (LARP), Chemistry Department, Federal University of Santa Maria, 97105-900 Santa Maria, RS, Brazil.
Food Chem. 2018 Apr 25;246:404-413. doi: 10.1016/j.foodchem.2017.11.049. Epub 2017 Nov 14.
In this study a simple and fast multi-class method for the determination of veterinary drugs in bovine liver, kidney and muscle was developed. The method employed acetonitrile for extraction followed by clean-up with EMR-Lipid® sorbent and trichloracetic acid. Tests indicated that the use of TCA was most effective when added in the final step of the clean-up procedure instead of during extraction. Different sorbents were tested and optimized using central composite design and the analytes determined by ultra-high-performance liquid chromatographic-tandem mass spectrometry (UHPLC-MS/MS). The method was validated according the European Commission Decision 2002/657 presenting satisfactory results for 69 veterinary drugs in bovine liver and 68 compounds in bovine muscle and kidney. The method was applied in real samples and in proficiency tests and proved to be adequate for routine analysis. Residues of abamectin, doramectin, eprinomectin and ivermectin were found in samples of bovine muscle and only ivermectin in bovine liver.
本研究建立了一种简单、快速的多类方法,用于测定牛肝、肾和肌肉中的兽药。该方法采用乙腈提取,然后用 EMR-Lipid®吸附剂和三氯乙酸进行净化。试验表明,在净化步骤的最后一步而不是在提取过程中添加 TCA 时效果最佳。使用中心组合设计对不同的吸附剂进行了测试和优化,并通过超高效液相色谱-串联质谱法(UHPLC-MS/MS)测定了分析物。该方法按照欧盟委员会第 2002/657 号决定进行了验证,在牛肝中 69 种兽药和牛肌肉和肾脏中 68 种化合物的测定结果令人满意。该方法已应用于实际样品和能力验证中,结果表明该方法适用于常规分析。在牛肌肉样本中发现了阿维菌素、多拉菌素、依普菌素和伊维菌素的残留,而在牛肝中仅发现了伊维菌素的残留。