液相色谱-质谱质谱法快速测定牛奶中的氯舒隆残留量.pdfVIP

638 2008, Vol. 29, No. 12 食品科学 ※分析检测 1 2 3 郭俊峰 ，马 昕 ，尚 楠 (1.河南出入境检验检疫局技术中心，河南郑州 450003 ；2. 宁夏出入境检验检疫局技术中心，宁夏银川 750000 ； 3. 中国农业大学食品科学与营养工程学院，北京 100083) 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5 μg/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% 。 牛奶；氯舒隆；Quechers ；液相色谱- 质谱/ 质谱 Rapid Analysis of Clorsulon Residue in Milk with High Performance Liquid Chromatography-Tandem Mass Spectrometry 1 2 3 GUO Jun-feng ，MA Xin ，SHANG Nan (1. Technical Center of Henan Entry-Exit Inspection and Quarantine Bureau, Zhengzhou 450003, China ； 2. Technical Center of Ningxia Entry-Exit Inspection and Quarantine Bureau, Yinchuan 750000, China； 3.College of Food Science and Nutritional Engineering, China Agricultural University, Beijing 100083, China) Abstract ：An effective method was developed to determine clorsulon in milk with high performance liquid chromatography- tandem 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%. Key words ：milk ；clorsulon ；Quechers ；high performance liquid chromatography-tandem mass spectrometry(LC-