液相色谱串联质谱法快速测定猪尿中10种镇静剂类药物残留量  

Rapid Determination of Tranquillizers Residues in Swine Urine by Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李存[1] 皇甫伟国[2] 杨挺[2] 吴银良[2] 

机构地区：[1]河北工程大学农学院动物医学系,邯郸056038 [2]农业部农产品质量安全监督检验测试中心(宁波),宁波315040

出　　处：《分析化学》2010年第7期1015-1018,共4页Chinese Journal of Analytical Chemistry

基　　金：宁波市科技重大攻关项目(No.2007C10036);宁波市农科院院长基金(No.09-12)资助

摘　　要：建立了快速测定猪尿中10种镇静剂类药物(噻拉嗪、阿扎哌隆、氟哌啶、氟哌啶醇、艾司唑仑、硝西泮、地西泮、奥沙西泮、氯丙嗪和奋乃静)残留量的液相色谱串联质谱方法。猪尿样品离心后过C18固相萃取小柱,用甲醇-乙酸乙酯(1:4,V/V)混合溶剂洗脱,氮气吹干后用0.1%甲酸溶液溶解进行仪器分析。采用EclipseXDB-C18色谱柱分离,以乙腈和0.1%甲酸溶液为流动相进行梯度洗脱,电喷雾正电子(ESI+)模式电离,多反应监测(MRM)模式检测,基质校准进行定量分析。10种镇静剂类药物在5～200μg/L范围内呈良好的线性,线性相关系数均大于0.99。方法检出限为0.11～0.52μg/L;定量限为0.20～0.91μg/L。添加浓度为1.0,2.0和10.0μg/L时,平均回收率在74.6%～115%之间,批内和批间相对标准偏差均小于15%。A method was developed for the determination residual tranquillizers （xylazine,azaperone,droperidol,haloperidol,estazolam,chlorpromazine,perphenazine,nitrazepam,oxazepam,and diazepam） in swine urine by liquid chromatography-tandem mass spectrometry.Samples were directly purified through C18 cartridge after centrifugation.Then the eluate was dried under nitrogen and residues were dissolved in 0.1% formic acid solution.The samples were analyzed by LC-MS/MS on an Eclipse XDB-C18 column with a mixture of acetonitrile and 0.1% formic acid solution as the mobile phase.The samples were quantified with the matrix standard calibration curve method.Good linearities were obtained for the ten tranquillizers at the concentration of 5-200 μg/L with the linear relative coefficient more than 0.99.The recoveries for the ten tranquillizers in swine urine were 74.6%-115.0% at the fortified levels of 1.0-10.0 μg/L with the limit of detection of 0.11-0.52 μg/L and the limit of quantitation of 0.20-0.91 μg/L.The relative standard deviations were less than 15.0%.

关 键 词：镇静剂类药物 液相色谱串联质谱法 猪尿 残留 

分 类 号：S859.8[农业科学—临床兽医学]