动物源食品中氯霉素、甲砜霉素、氟苯尼考及氟苯尼考胺残留检测－超高效液相色谱-串联质谱法研究

Determination of Chloramphenicol，Thiamphenicol， Florfenicol and Florfenicol Amine Residues in Animal Derived Food by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

关键词:  动物源食品  氯霉素类药物  残留  超高效液相色谱-串联质谱

Key words:  animal derived food  Chloramphenicols  residue  UPLC-MS/MS

摘要:

建立了动物源食品中氯霉素、甲砜霉素、氟苯尼考及氟苯尼考胺残留检测的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。样品在碱性条件下用乙酸乙酯提取后，再用正己烷去除脂肪，浓缩后用BEH C18（50×2.1mm，1.7µm）色谱柱分离，以乙腈和水为流动相进行梯度洗脱，流速为0.3mL/min，多反应监测（MRM）模式检测。结果表明：四种药物在2～500μg/L的系列浓度范围内均呈良好线性关系，相关系数（r）均大于0.990。样品中氯霉素的检测限为0.1μg/kg，定量限为0.2μg/kg；甲砜霉素、氟苯尼考和氟苯尼考胺的检测限为0.5μg/kg，定量限为1μg/kg。本方法氯霉素在0.2μg/kg～1μg/kg的添加浓度范围内，甲砜霉素、氟苯尼考及氟苯尼考胺在1μg/kg～50μg/kg的添加浓度范围内平均回收率均为70%～120%，相对标准偏差（RSD）均小于20％。该方法具有简便快捷、灵敏度高、定性准确等特点。

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was established for the determination of Chloramphenicol, Thiamphenicol, Florfenicol and Florfenicol Amine residues in animal derived food. The samples were extracted by ethyl acetate in basic conditions. The fat was removed by hexane. The separation of 4 drugs was performed on Waters Acquity UPLC system with the column of BEH C18（50×2.1mm，1.7µm）and the gradient elution solvent of acetonitrile and water at a flow rate of 0.3mL/min.The calibration curves were good linear between the peak areas and the concentrations of 2～500μg/L，and the correlation coefficients(r) were more than 0.990. The limit of detection of Chloramphenicol was 0.1µg/kg, and the limit of quantification was 0.2μg/kg. The limits of detection of Thiamphenicol, Florfenicol and Florfenicol Amine were 0.5µg/kg , and the limits of quantification were 1μg/kg.The average recoveries of 4 drugs ranged 70%～120%. The RSD of method was less than 20%.