分散固相萃取-高效液相色谱-串联质谱快速测定鸡肉中盐霉素残留

建立了分散固相萃取-超高效色谱-电喷雾串联质谱快速测定鸡肉中盐霉素残留的方法。样品经乙腈提取后,采用QuEChERS方法净化,氮吹转换溶剂后,采用Acquity BEH C18柱进行分离,0.3%甲酸水溶液-甲醇体系为流动相,梯度洗脱,电喷雾质谱正离子多反应监测模式测定,外标法定量。结果表明,在优化的条件下对样品进行分析检测,盐霉素的检出限为0.03μg·kg-1,添加水平为5.5~31.4μg·kg-1时,加标回收率为78.2-97.8%,RSD<2.0%(n=6),在0.630~25.2μg·L-1质量浓度范围内呈良好线性,相关系数R2>0.9989。该方法前处理步骤简单,具有较高灵敏度,可用于大批量样品的快速筛查检测。

Rapid Determination of Salinomycin Residues in Chicken by Dispersive Solid Phase Extraction-High Performance Liquid Chromatography Tandem Mass Spectrometry

A method for rapid determination of salinomycin in chicken was developed by ultra high performance liquid chromatography-electrospray ionization tandem mass spectrometry with dispersive solid-phase extraction. The compounds were extracted from chicken tissue with acetonitrile and then cleaned up by dispersive solid phase extraction, after solvent exchanged, the salinomycin was analyzed by LC-MS/MS on an Acquity BEH C18 column with methanol-0.3%FA-H2O solution as mobile phase by gradient elution under positive ion multiple reaction monitoring（MRM）mode. It showed, under optimized conditions the limit of detection for salinomycin was 0.03μg·kg-1, the recoveries between 5.5~31.4μg·kg-1spiked levels ranged from 78.2-97.8%, with RSDs less than 2.0%（n=6）. The calibration curves was linear in the ranges of 0.630~25.2 μg·L-1, with a correlation coefficient more than 0.9989. Owe to its simple pretreatment, high sensitivity, this method could be used for rapid screening for detection of large quantities of samples.