色谱

色谱 ›› 2015, Vol. 33 ›› Issue (11): 1169-1174.DOI: 10.3724/SP.J.1123.2015.08010

• 研究论文 • 上一篇    下一篇

分散固相萃取净化-超高效液相色谱-串联质谱法测定鸡蛋和鸡肉中金刚烷胺和金刚乙胺残留

林涛1,2, 樊建麟1, 刘兴勇1, 陈兴连1, 李彦刚1, 刘宏程1,2   

  1. 1. 云南省农业科学院质量标准与检测技术研究所, 云南 昆明 650223;
    2. 农业部农产品质量安全风险评估实验室(昆明), 云南 昆明 650223
  • 收稿日期:2015-08-09 出版日期:2015-11-08 发布日期:2012-05-30
  • 通讯作者: 刘宏程
  • 基金资助:

    云南省社会发展科技计划项目(2013RA012);云南省应用基础研究计划青年项目(2013FD064);云南省科技创新平台建设计划项目(2014DA001).

Determination of amantadine and rimantadine residues in egg and chicken samples by dispersive solid phase extraction purification-ultra high performance liquid chromatography-tandem mass spectrometry

LIN Tao1,2, FAN Jianlin1, LIU Xingyong1, CHEN Xinglian1, LI Yangang1, LIU Hongcheng1,2   

  1. 1. Institute of Quality Standards & Testing Technique, Yunnan Academy of Agricultural Science, Kunming 650223, China;
    2. Laboratory of Quality & Safety Risk Assessment for Agro-Products (Kunming), Ministry of Agriculture, Kunming 650223, China
  • Received:2015-08-09 Online:2015-11-08 Published:2012-05-30

PDF

117

被引次数

6

摘要：

建立了鸡蛋和鸡肉中金刚烷胺和金刚乙胺残留量的分散固相萃取-超高效液相色谱-串联质谱测定方法。鸡蛋和鸡肉样品经氨水-乙腈(2 : 98, v/v)提取后,提取液经氮气吹干至1 mL后,利用C18和NH2填料进行分散固相萃取净化,过滤膜后分析。采用ZORBAX C18色谱柱分离,用1 mmol/L乙酸铵水溶液(含0.1%(v/v)甲酸)-甲醇作为流动相进行梯度洗脱,正离子多反应监测模式。结果表明,金刚烷胺和金刚乙胺在0.15~10.0 μ g/L范围内具有较好的线性关系,鸡蛋和鸡肉中的检出限均为0.05 μ g/kg,定量限均为0.20 μ g/kg。当2种药物在鸡蛋和鸡肉中的加标水平为0.2、1.0和2.0 μ g/kg时,平均回收率范围为89%~108%,相对标准偏差范围为5.0%~8.6%。该方法能够满足鸡蛋和鸡肉中金刚烷胺和金刚乙胺残留量分析的要求。

关键词: 超高效液相色谱, 串联质谱, 分散固相萃取, 鸡蛋, 鸡肉, 金刚烷胺, 金刚乙胺

Abstract:

A method was developed for the determination of residual amantadine and rimantadine in eggs and chickens by dispersive solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry. Egg and chicken samples were extracted with ammonia water-acetonitrile (2 : 98, v/v). The extraction solution was dried to 1 mL under nitrogen, and then purified by dispersive solid phase extraction method with C18 and NH2 sorbents. After purification, the extraction solution was filtered through a filter. The target compounds were analyzed by ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) on a ZORBAX C18 column using a mixture of 1 mmol/L ammonium acetate solution (containing 0.1% (v/v) formic acid) and methanol as mobile phases with gradient elution. The mass spectrometer was operated under multiple reaction monitoring (MRM) mode in positive mode. The good linearities were obtained for amantadine and rimantadine at a concentration range of 0.15-10.0 μ g/L. The limits of detection for amantadine and rimantadine were all 0.05 μ g/kg, and the limits of quantification were 0.20 μ g/kg. The recoveries of amantadine and rimantadine in eggs and chickens at three spiked levels (0.2, 1.0 and 2.0 μ g/kg) were in the range of 89%-108% with the relative standard deviations of 5.0%-8.6%. The results demonstrated that the method is suitable for the determination of amantadine and rimantadine in eggs and chickens.

Key words: amantadine, chickens, dispersive solid phase extraction, eggs, rimantadine, tandem mass spectrometry (MS/MS), ultra high performance liquid chromatography (UHPLC)

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