液相色谱-质谱/质谱法快速测定牛奶中的氯舒隆残留量

Rapid Analysis of Clorsulon Residue in Milk with High Performance Liquid Chromatography-Tandem Mass Spectrometry

建立快速测定牛奶中氯舒隆残留量的液相色谱-质谱/质谱(LC-MS/MS)检测方法。样品用乙腈提取,Quechers方法净化后,采用LC-MS/MS电喷雾负离子(ESI-)电离,多反应监测(MRM)模式检测,外标法定量。方法定量限为5μg/kg。在添加水平为5～100μg/kg的范围内,氯舒隆的回收率为92.8%～99.3%;相对标准偏差(RSD)不高于4.7%。

An effective method was developed to determine clorsulon in milk with high performance liquid chromatographytandem mass spectrometry （LC-MS/MS）. Samples were extracted with acetonitrile.The concentrated extracts were cleaned up though Quechers method. Identification was achieved in electrospray ionizationin negative mode （ESI-） using multiple reaction monitoring（MRM）. The limit of quantification for clorsulon is 5 μg/kg.The recoveries of clorsulon are 92.8% to 99.3% at spiked levels of 5 to 100 μg/kg.The （RSD） of this relative standard deviation method is less than 8.6%.