张建伟;彭丽;张盼盼;吴宁鹏;孟蕾;赵晨浩;吴志明;程相朝;
ZHANG Jian-wei;PENG Li;ZHANG Pan-pan;WU Ning-peng;MENG Lei;ZHAO Chen-hao;WU Zhi-ming;CHENG Xiang-chao;School of Food and Bioengineering, Henan University of Science and Technology;Henan Institute of Veterinary Drug and Feed Control;College of Veterinary Medicine,Henan Agricultural University;

• 1:河南科技大学食品与生物工程学院
• 2:河南省兽药饲料监察所
• 3:河南农业大学动物医学院

摘要(Abstract)：

本试验旨在建立一种液相色谱-串联质谱法(LC-MS/MS)快速测定牛奶和羊奶中β-内酰胺类、大环内酯类、磺胺类、喹诺酮类、林可胺类、四环素类、性激素类、抗虫类共8大类43种药物(47种残留标志物)的残留。样品经1%氨化乙腈提取，90%乙腈(含0.5%乙酸)重复提取，低温冷冻净化除脂，使用ACQUITY UPLC BEH C18柱(100 mm×2.1 mm, 1.7μm)色谱柱分离，以10 mmol/L甲酸铵溶液(含0.1%甲酸)和甲醇为流动相进行梯度洗脱，采用电喷雾电离(ESI)和多反应监测(MRM)模式进行检测，基质外标法进行定量。结果显示，47种残留标志物在相应线性范围内线性关系均良好，相关系数均大于0.99,方法的定量限为0.5～5μg/kg;在0.5～200μg/kg添加浓度范围内，平均回收率为61.4%～115.7%,相对标准偏差(RSD)为1.2%～11.4%。结果表明，本试验建立的方法灵敏度高、准确性好、适用性强，适用于牛奶和羊奶中43种药物的残留检测。
This study aimed to establish a liquid chromatography-tandem mass spectrometry(LC-MS/MS) method for the rapid determination of 43 drug residues(47 residue markers) in cow and sheep milk in 8 categories, including β-lactams, macrolides, sulfonamides, quinolones, lincosamides, tetracyclines, sex hormones and anthelmintics. The sample was extracted with 1% ammoniated acetonitrile and repeated with 90% acetonitrile(containing 0.5% acetic acid),cleaned up by cryopreservation, and separated on an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7 μm) with a gradient elution of 10 mmol/L ammonium formate solution(containing 0.1% formic acid) and methanol as mobile phases. Detection was performed by electrospray ionization(ESI) and multiple reaction monitoring(MRM) mode, and quantification by matrix external standard method.The linearity of the 47 residue markers corresponded to the linear ranges with the correlation coefficients greater than 0.99. The limits of quantification of the method were 0.5-5 μg/kg. The average recoveries were 61.4%-115.7% with the relative standard deviations of 1.2%-11.4% in the spiked concentration range of 0.5-200 μg/kg.Thus, the new established method enabled sensitive, accurate and efficient detection of 43 drug residues in cow and sheep milk.

关键词(KeyWords)： 牛奶;羊奶;兽药残留;液相色谱-串联质谱法;测定
cow milk;sheep milk;veterinary drug residue;liquid chromatography-tandem mass spectrometry;determination

Abstract:

Keywords:

基金项目(Foundation):

作者(Authors): 张建伟;彭丽;张盼盼;吴宁鹏;孟蕾;赵晨浩;吴志明;程相朝;
ZHANG Jian-wei;PENG Li;ZHANG Pan-pan;WU Ning-peng;MENG Lei;ZHAO Chen-hao;WU Zhi-ming;CHENG Xiang-chao;School of Food and Bioengineering, Henan University of Science and Technology;Henan Institute of Veterinary Drug and Feed Control;College of Veterinary Medicine,Henan Agricultural University;

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