【摘要】 建立动物源性食品中二硝甲酚残留量的分析方法。样品以丙酮-正己烷(1:2,V/V)为提取溶剂,经高速匀浆方法提取,提取液经Oasis HLB固相萃取柱净化,除去样品中大部分的脂肪和无机盐等干扰基质,有效地降低了样品中的复杂基质所带来的背景干扰。以乙腈-水(梯度洗脱)为流动相经BEH C18柱(50mm×2.1mm,1.7μm)进行分离后以MS/MS多反应监测扫描模式下检测。方法的相关系数r>0.999,最低检出限为0.005mg/kg。在3种添加水平(0.005、0.010、0.020mg/kg)条件下,其平均回收率为82.6%～108%,相对标准偏差小于10%(n=6)。该方法是一种快速、准确、灵敏度高的检测动物源性食品中二硝甲酚残留量的检测方法。更多还原

【Abstract】 A solid-phase extraction and ultrahigh performance liquid chromatography-tandem mass spectrometry method has been developed for the determination of DNOC residue in animal-origin foods.Samples were extracted with acetone-hexane(1: 2,V/V) after high-speed homogenization.The crude extract was purified on Oasis HLB solid phase extraction column to remove fat and inorganic salts,which could effectively reduce the background interference generated by complex matrix in samples.The DNOC residue was separated on BEH C18(50 mm × 2.1 mm,1.7μm) column using acetonitrile-water as the mobile phase by gradient elution and detected using a tandem mass analyzer in the multi-reaction monitoring(MRM) mode.The developed method exhibited an excellent linear relationship(r>0.999) and a detection limit of 0.005 mg/kg.At the spiked levels of 0.005,0.01 mg/kg and 0.02 mg/kg,the average recovery rates for DNOC were in the range of 82.6%-108% with a relative standard deviation(RSD) of less than 10%(n = 6).This method proved rapid,accurate and highly sensitive and can therefore be used for the determination of DNOC residue in animal-origin foods.更多还原