超高效液相色谱－串联三重四级杆质谱检测生鲜肉中四环素类抗生素残留

摘要

建立了超高效液相色谱－串联三重四级杆质谱（ UPLC－MS／MS）检测生鲜肉中四环素类抗生素残留的分析方法。方法采用C18色谱柱（50 mm ×2．1 mm，1．7μm）分离，柱温30℃，样品室温度10℃。流动相由A相（乙腈）和B相（0．1％甲酸溶液）组成，流速为0．4 mL／min，采用梯度洗脱。在ESI正离子模式下，采用多反应离子监测模式进行测定，可以在5 min内完成检测。四种四环素类抗生素土霉素、金霉素、四环素和强力霉素均在10～200μg／mL范围内有良好的线性关系，相关系数大于0．995。样品最低检出限为50μg／kg，回收率在80％～89％之间，相对标准偏差为2．5％～6．3％。该方法准确度高，灵敏度好，适用于生鲜肉中四环素类抗生素的检测。%An ultra performance liquid chromatography -electrospray ionization tandem mass spectrometry ( UPLC-ESI-MS/MS) method for the determination of Antibiotics Residues in fresh meat was developed .Methods C18 chromatographic column (50mm ×2.1mm, 1.7 μm), the solvent system was composed of mobile phase A (Acetonitrile), and mobile phase B (water with 0.1%methanoic acid ).The flow rate was 0.4 mL/min and gradient elution, and the temperature is held constant at 30℃within a thermostated column .Multiple reaction monitoring ( MRM) in ESI positive mode was used for quantitation .The Antibiotics Residues was successfully detected within 5 min.Antibiotics Residues have good linear relationship in the range of 0.5μg /L -8μg /L with the correlation coefficient larger than 0.995.The detection limit was 50 μg /kg, and the recovery is between 80%-89% with the relative standard deviation between 2.5%~6.3%.An accurate and sensitivity method was developed in this study .The established method has been successfully applied to the determination of antibiotics residues in fresh meat .