高效液相色谱-串联质谱法测定鸡肉组织中癸氧喹酯残留  

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

作　　者：陈瑞清[1,2] 俞道进[1] 陈锋[2] 黄一帆[1] 

机构地区：[1]福建农林大学动物科学学院,福建福州350002 [2]福建省农产品质量安全检验检测中心,福建福州350003

出　　处：《色谱》2010年第10期997-1000,共4页Chinese Journal of Chromatography

基　　金：福建省科技重点项目(No.2008Y0002)

摘　　要：建立了测定鸡肉组织中癸氧喹酯(DEC)残留的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经乙腈提取,正己烷脱脂,固相萃取(SPE)小柱净化;采用0.1%甲酸乙腈溶液-0.1%甲酸水溶液(78∶22,v/v)为流动相,电喷雾正离子电离(ESI+)模式,多反应监测(MRM)检测模式,以内标法进行定量。结果表明:DEC在1～200μg/L范围内呈良好的线性关系,相关系数(r2)大于0.99;1、10、100μg/kg3个添加水平的回收率为78.2%～107.4%,日内、日间相对标准偏差(RSD)均小于15%,方法检出限为0.25μg/kg,定量限为0.5μg/kg。该方法简便、灵敏、精确,可用于鸡肉组织中DEC药物残留的确证检测。A high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method was developed for the determination of decoquinate （DEC） residue in chicken meat. The sample was extracted with acetonitrile,cleaned-up with hexane,and purified with solid phase extraction （SPE） cartridge. The mobile phase was acetonitrile （containing 0.1% formic acid） and water （containing 0.1% formic acid）. The analyte was identified by positive electrospray ionization （ESI＋） mode and multiple reaction monitoring （MRM） mode. The results showed as follows：The calibration curve showed good linearity within the concentrations of 1-200 μg/L with the correlation coefficient （r2）0.99. At the spiked levels of 1,10 and 100 μg/kg,the recoveries of DEC were 78.2%-107.4%. The relative standard deviations （RSDs） of intra-and inter-days were both less than 15%. The limit of detection of DEC was 0.25 μg/kg and the limit of quantification was 0.5 μg/kg. The method is simple,sensitive and accurate in the determination of DEC residue,which can meet the requirements of the domestic and international legislations.

关 键 词：高效液相色谱-串联质谱 癸氧喹酯 残留 鸡肉 

分 类 号：O658[理学—分析化学]