【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。更多还原

【Abstract】 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. 22 μm 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 electrospray 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.更多还原