HPLC-MS/MS法测定饲料中甲硝唑和二甲硝咪唑含量  

Determination of Metronidazole and Dimetridazole in Feed by High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：郭礼强[1] 张金玲[1] 李凯[1] 丁葵英[1] 吴翠玲[2] GUO Li - qiang ZHANG Jing - lin LI Kai DING Kui - ying WU Cui - ling(Weifang Entry -Exit Inspection and Quarantine Bureau, Weifang, Shandong 261041, China Agilent technologies Co. , Ltd in China, Beijing 100102, China)

机构地区：[1]潍坊出入境检验检疫局,山东潍坊261041 [2]安捷伦科技(中国)有限公司,北京100102

出　　处：《中国兽药杂志》2017年第1期52-56,共5页Chinese Journal of Veterinary Drug

基　　金：潍坊市2015年科学技术发展计划(2015ZJ1101);山东出入境检验检疫局科研基金项目(SK201349)

摘　　要：建立了高效液相色谱-串联质谱法(HPLC-MS/MS)快速测定饲料中甲硝唑和二甲硝咪唑的含量。饲料样品用乙酸乙酯提取后,经PCX固相萃取柱净化处理,过0.22μm滤膜,以乙腈和含0.1%的甲酸水溶液为流动相,经Eclipse Plus C18色谱柱(3.0 mm×100 mm,1.8μm)分离,多级反应监测(MRM)正离子模式下扫描分析。结果表明,甲硝唑和二甲硝咪唑在0.2~50μg/L范围呈良好线性,线性相关系数均大于0.997,检出限均为0.2μg/kg,定量下限均为0.5μg/kg。样品在定量下限1倍、2倍、10倍3个加标水平下的平均回收率为95.3%~103.2%,相对标准偏差(RSD)为4.67%~8.46%。该方法灵敏、简便、准确,可用于饲料中甲硝唑和二甲硝咪唑的检测分析。A method for the determination of metronidazole and dimetridazole in feed by high performance liquid chromatography -tandem mass spectrometry （HPLC -MS/MS） is presented. The sample were purified with solid phase extraction column of PCX after extraction by ethyl acetate. After filtered with a 0.22μm membrane, the sample was separated on a eclipse plus C18 column（3.0 mm × 100 mm, 1.8 μm）using gradient elution with mobile phases of acetonitrile and aqueous solution containing 0. 1% formic acid, and detected on positive eleetrospray ionization with a multiple reaction monitoring （MRM） as survey scan. The results showed that the calibration curves were linear in the range of 0.2 - 50 μg/L for metronidazole and dimetridazole with correlation coefficient （r） more than 0.997. The LODs for metronidazole and dimetridazole was 0.2 μg/kg and the LOQs was 0.5 μg/kg. The average recoveries （n = 6 ） in feed samples at three spiked levels （1 tismes, 2 times, 10 times） ranged from 95.3% to 103.2% with relative standard deviations （RSDs） of 4.67 - 8.46%. The method was sensitive, convenient and accurate, and could satisfy the demand of detection and analysis of metronidazole and dimetridazole in feed.

关 键 词：饲料 含量分析 甲硝唑 二甲硝咪唑 液相色谱-串联质谱 

分 类 号：S859.83[农业科学—临床兽医学]