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

Determination of Antibiotics Residues in Fresh Meat by Ultra Performance Liquid Chromagraphy-tandem Mass Spectrometry

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 m L/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/m L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 ＆#215;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 .