色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 724-728.DOI: 10.3724/SP.J.1123.2013.01023

• 研究论文 • 上一篇    下一篇

超高效液相色谱-串联质谱法测定鸡肉中的利巴韦林和金刚烷胺

云环, 崔凤云, 严华, 刘鑫, 何悦, 张朝晖   

  1. 北京出入境检验检疫局技术中心, 北京 100026
  • 收稿日期:2013-01-10 修回日期:2013-03-11 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 云环
  • 基金资助:

    国家质检总局科研项目(2013IK146).

Determination of ribavirin and amantadine in chicken by ultra performance liquid chromatography-tandem mass spectrometry

YUN Huan, CUI Fengyun, YAN Hua, LIU Xin, HE Yue, ZHANG Zhaohui   

  1. Technology Center of Beijing Entry-Exit Inspection and Quarantine Bureau, Beijing 100026, China
  • Received:2013-01-10 Revised:2013-03-11 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

PDF

298

被引次数

67

摘要：

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定鸡肉中利巴韦林和金刚烷胺的分析方法。样品用1%(体积分数)三氯乙酸溶液-乙腈(1:1, v/v)溶液提取,经Supelco LC-SCX固相萃取柱净化后用Acquity UPLC BEH Hillic柱(150 mm×2.1 mm, 1.7 μm)分离,以甲醇和0.1%(体积分数)甲酸作为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测(MRM)模式进行检测。结果表明,利巴韦林和金刚烷胺在10.0~100.0 μg/L范围内线性关系良好(r2≥0.99)。方法的定量限(信噪比为10)为4.0 μg/kg,在4.0、8.0、20.0 μg/kg添加水平的回收率为78%~102.5%,相对标准偏差(n=6)在2.2%~7.6%之间。该方法快速、灵敏、准确,适合于鸡肉中利巴韦林和金刚烷胺的同时、快速、高灵敏度的分析检测。

关键词: 超高效液相色谱-串联质谱, 鸡肉, 金刚烷胺, 利巴韦林

Abstract:

A method for the determination of ribavirin and amantadine in chicken has been developed by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). After extracted by 1% (volume percentage) trichloroacetic acid solution-acetonitrile (1:1, v/v) and purified by a Supelco LC-SCX cartridge, the samples were loaded onto an Acquity UPLC BEH Hillic column (150 mm×2.1 mm, 1.7 μm)and separated with gradient elution. The electrospray was operated in the positive mode and the samples were monitored by the multiple reaction monitoring (MRM) mode. The limits of quantification (LOQs, S/N=10) of ribavirin and amantadine were 4.0 μg/kg. The calibration curves showed good linearity in the range of 10.0-100.0 μg/L, and the correlation coefficients (r2) were not lower than 0.99. When the spiked levels were 4.0, 8.0 and 20.0 μg/kg, the recoveries of ribavirin and amantadine in chicken ranged from 78% to 102.5%, with the relative standard deviations (RSDs) of 2.2%-7.6%. The results indicate that the method is simple, rapid, sensitive and suitable for the qualitative and quantitative analyses of ribavirin and amantadine in chicken samples.

Key words: amantadine, chicken, ribavirin, ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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