加速溶剂萃取/液相色谱-串联质谱法测定鹌鹑蛋和鸽蛋中氯霉素类药物残留

Determination of Chloramphenicols Residues in Quail Eggs and Pigeon Eggs by Accelerated Solvent Extraction/Liquid Chromatography-Tandem Mass Spectrometry

建立了加速溶剂萃取/液相色谱-串联质谱(ASE/LC-MS/MS)分离检测鹌鹑蛋和鸽蛋中3种氯霉素类药物及其代谢产物的分析方法。样品经加速溶剂萃取,正己烷去脂,采用Waters XBridge^TMC18色谱柱(250×4.6 mm,5μm)分离,流动相A为2 mmol/L NH 4Ac溶液,B为2 mmol/L NH 4Ac-乙腈,梯度洗脱。质谱采用多反应监测(MRM)模式进行检测,内标法定量。结果表明,3种氯霉素类药物及其代谢产物在各自线性范围内呈良好线性,相关系数均在0.9993以上,检测限为0.04~0.5μg/kg,定量限为0.1~1.5μg/kg。样品在定量限、0.5倍最大残留限量(MRL)、1倍MRL和2倍MRL加标水平下的平均回收率为90.26%~105.73%,相对标准偏差(RSD)均低于3.29%。该方法简单、快速、定性准确、灵敏度高,适合鹌鹑蛋和鸽蛋中3种氯霉素类药物及其代谢产物的检测。

Accelerated solvent extraction/liquid chromatography-tandem triple quadrupole mass spectrometry(ASE/LC-MS/MS)was established to detect chloramphenicols and its metabolites in quail eggs and pigeon eggs.The sample was extracted by ASE,degreased in n-hexane,and separated on a water XBridge^TM C18 column(250×46 mm,5μm)with gradient elution.The mobile phase A was 2 mmol/L NH 4Ac,and B was 2 mmol/L NH 4Ac-acetonitrile.The target compounds were detected under the multiple reaction monitoring(MRM)mode,and quantified by internal standard method.The results showed that the three drugs and their metabolites of chloramphenicol showed good linearity with correlation coefficient above 0.9993,the limits of detection were 0.04-0.5μg/kg,and the limits of quantitation(LOQs)were 0.1-1.5μg/kg.The average recoveries of the samples at the LOQ,0.5MRL,1MRL and 2MRL spiked levels ranged from 90.26%to 105.73%,and the relative standard deviations were all below 3.29%.The method is simple,fast,accurate and sensitive,which is suitable for the detection of three drugs and their metabolites of chloramphenicol in quail eggs and pigeon eggs.