| 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 |
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| 引用本文： | 李存,皇甫伟国,杨挺,吴银良.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[J].分析化学,2010,38(7). |
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| 作者姓名： | 李存 皇甫伟国 杨挺 吴银良 |
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| 作者单位： | 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 |
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| 基金项目： | 宁波市科技重大攻关项目，宁波市农科院院长基金 |
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| 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Eclipse XDB-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5～200 μg/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0.11～0.52 μg/L; 定量限为0.20～0.91 μg/L.添加浓度为1.0, 2.0和10.0 μg/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%.
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| 关 键 词： | 镇静剂类药物 液相色谱串联质谱法 猪尿 残留 |
Rapid Determination of Tranquillizers Residues in Swine Urine by Liquid Chromatography-Tandem Mass Spectrometry |
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| LI Cun,HUANGFU Wei-Guo,YANG Ting,WU Yin-Liang.Rapid Determination of Tranquillizers Residues in Swine Urine by Liquid Chromatography-Tandem Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2010,38(7). |
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| Authors: | LI Cun HUANGFU Wei-Guo YANG Ting WU Yin-Liang |
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| Institution: | LI Cun1,HUANGFU Wei-Guo2,YANG Ting2,WU Yin-Liang2 1(College of Agriculture,Hebei University of Engineering,Handan 056038) 2(The Supervision,Inspection & Testing Center of Agricultural Products Quality & Security,Ministry of Agriculture,Ningbo 315040) |
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| Abstract: | 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 aceton... |
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| Keywords: | Tranquillizers Liquid chromatography with tandem mass spectrometry Swine urine Residue |
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