超高效液相色谱法测定饲料中地昔尼尔  

The determination of dicyclanil in feed by ultra performance liquid chromatographic

作　　者：方忠意[1] 刘素梅[1] 

机构地区：[1]农业部畜禽产品质量安全检验测试中心(郑州)

出　　处：《中国饲料》2010年第6期38-40,共3页China Feed

摘　　要：本研究建立了超高效液相色谱测定饲料中地昔尼尔的方法。饲料样品经过乙腈提取,取5mL上清液氮气吹干,用20%甲醇溶液(含0.2%甲酸)溶解,经过Waters Oasis MCX固相萃取小柱净化,然后用Waters Acquity UPLC HSS T3色谱柱(2.1mm×100mmi.d.,1.8μm)分离,以甲醇和水为流动相进行洗脱,外标法定量。结果表明,地昔尼尔质量浓度在0.05～100μg/mL内线性良好,相关系数大于0.9999;在10～200mg/kg的添加水平,平均加标回收率为78.0%～86.3%;相对标准偏差为4.2%～6.1%;方法的检出限低至0.05mg/kg,定量下限低至0.1mg/kg。该方法简单、快速、灵敏,可满足饲料中地昔尼尔的快速筛选检测的要求。An ultra performance liquid chromatographic method was developed for determination of dicyclanil in feeds.The sample was extracted by acetonitrile.The extract was evaporated to dryness under nitrogen,and redissolved by 20 %methanol solution （add 0.2 % formic acid） and cleaned up on a Waters Oasis MCX solid phase extraction column.The separation of compounds was carried on a HSS T3 column （2.1 mm×100 mm i.d.,1.8 μm） eluted with methanol and water.The method was quantified by external standard method.The experimental conditions were optimized.Under the optimal conditions,the calibration curve showed a good linear over the concentration of dicyclanil in the range of 0.05 ～ 100 mg/L with a correlation coefficient of more than 0.9999.The limit of detection（LOD） and the quantitative limits （LOQ） of dicyclanil were 0.05 mg/kg and 0.1 mg/kg respectively.The average recoveries from spiked feeds samples at three concentration levels of 10,50 mg/kg and 200 mg/kg ranged from 78.0 % to 86.3 % with relative standard deviations of 4.2 % ～ 6.1 %.The method showed a good repeatability and high sensitivity,and was suitable for the fast determination of dicyclanil in feeds.

关 键 词：地昔尼尔 超高效液相色谱 饲料 

分 类 号：S816.17[农业科学—饲料科学]