色谱

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高效液相色谱-电喷雾电离三级四极杆质谱测定鸡肉中氯霉素、甲砜霉素和氟甲砜霉素的残留量

陈小霞1,岳振峰2,吉彩霓2, 梁世中1   

  1. 1. College of Food Engineering and Biotechnology, South China University of Technology, Guangzhou 510640, China; 2. Inspection Center of Import and Export Food, Shenzhen Entry-Exit Inspection and Quarantine Bureau of PRC, Shenzhen 518067, China
  • 收稿日期:2004-02-05 修回日期:1900-01-01 出版日期:2005-01-30 发布日期:1989-03-25
  • 通讯作者: 岳振峰
  • 基金资助:

Analysis of Chloramphenicol, Thiamphenicol and Florfenicol in Chickens by High Performance Liquid Chromatography with Electrospray Ionization Mass Spectrometry

CHEN Xiaoxia1, YUE Zhenfeng2, JI Caini2, LIANG Shizhong1   

  1. 1. College of Food Engineering and Biotechnology, South China University of Technology, Guangzhou 510640, China; 2. Inspection Center of Import and Export Food, Shenzhen Entry-Exit Inspection and Quarantine Bureau of PRC, Shenzhen 518067, China
  • Received:2004-02-05 Revised:1900-01-01 Online:2005-01-30 Published:1989-03-25

摘要: 建立了鸡肉中3种氯霉素类抗生素残留的高效液相色谱-电喷雾电离三级四极杆质谱(HPLC-ESI-MS-MS)测定法。该方法采用多反应监测(MRM)负离子模式,可一次对鸡肉中的氯霉素、甲砜霉素和氟甲砜霉素进行定性和定量。该方法仅需1 g样品,并省去固相萃取步骤,具有操作简便、有机试剂消耗量少、测定周期短等优点。方法的检出限为0.010 μg/kg,测定低限为0.100 μg/kg,线性范围为0.050~1.00 μg/L,加标回收率为69.0%~92.8%,相对标准偏差为6.3%~12.9%。

关键词: 残留, 氟甲砜霉素, 高效液相色谱-电喷雾电离质谱, 鸡肉 , 甲砜霉素, 氯霉素

Abstract: The method for the analysis of three chloramphenicols including chloramphenicol, thiamphenicol and florfenicol in chickens was developed by high performance liquid chromatography combined with electrospray ionization mass spectrometry (HPLC-ESI-MS-MS). The mass spectrometer was operated in the negative ion mode using multiple reaction monitoring for qualitative and quantitative analysis of these compounds at the same time. Only 1 g of sample was needed, and no solid phase extraction (SPE) procedure was adopted. The advantages of the method are simple operation, less organic chemicals consumed, and shorter operation time. The limits of detection (LOD) were 0.010μg/kg, and the limits of quantitation (LOQ) were 0.100 μg/kg. The linear plots were obtained between 0.050 and 1.00 μg/L. Overall recoveries were between 69.0%and 92.8%with relative standard deviations between 6.3%and 12.9%.

Key words: chicken , chloramphenicol, florfenicol, residue, thiamphenicol, high performance liquid chromatography-electrospray ionization mass spectrometry