高效液相色谱—串联质谱法测定鸡粪中癸氧喹酯的残留量

Determination of decoquinate in chicken excreta by high performance liquid chromatography-tandem mass spectrometry

采用高效液相色谱—串联质谱法测定鸡粪中癸氧喹酯的残留量.样品经乙腈提取、HLB固相萃取小柱净化,采用ESI+电离模式和多反应监测模式(MRM),以内标法进行定量.结果表明:该法的线性范围为1-200 ng.mL-1,r2大于0.99;选取5、10、100μg.kg-1 3个含量进行空白鸡粪添加癸氧喹酯的回收率试验,回收率为84.4%-100.1%,批内、批间RSD均小于15%,方法检出限为2.5μg.kg-1,定量限为5.0μg.kg-1.可见,高效液相色谱—串联质谱法简单快速、灵敏度高、选择性强,适用于鸡粪中癸氧喹酯药物残留量的确证检测.

A high performance liquid chromatography-tandem mass spectrometry（LC-MS/MS） method was developed for the determination of decoquinate residue in chicken excreta.The sample was extracted with acetonitrile,and purified with HLB solid phase extraction（SPE） cartridge.The analyte was identified by positive electrospray ionization mode and multiple reactions monitoring mode（MRM）.The results showed as following： The calibration curve showed good linearity within the concentrations of 1-200 ng·mL-1 with the correlation coefficient r20.99.At the spiked levers of 5,10 and 100 μg·kg-1,the recoveries of decoquinate were 84.4%-100.1%.The relative standard deviations（RSD） of intra-batch and inter-batch were both less than 15%.The limit of detection of decoquinate was 2.5 μg·kg-1 and the limit of quantification was 5.0 μg·kg-1.The method was simple,sensitive and accurate in the determination of decoquinate residue.