色谱

色谱 ›› 2011, Vol. 29 ›› Issue (02): 120-125.DOI: 10.3724/SP.J.1123.2011.00120

• 研究论文 • 上一篇    下一篇

分散固相萃取-超高效液相色谱-串联质谱法测定鸡肝中磺胺类、喹诺酮类和苯并咪唑类药物及其代谢物的残留量

李锋格1,2*, 苏敏1, 李晓岩1, 张洪霞2, 姚伟琴1, 窦辉1, 张万权1   

  1. 1. 新疆出入境检验检疫局技术中心, 新疆 乌鲁木齐 830063; 2. 新疆农业大学食品科学学院, 新疆 乌鲁木齐 830063
  • 收稿日期:2010-10-20 修回日期:2010-12-07 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 李锋格,硕士,高级工程师,主要研究方向为食品、农产品、动物源性食品中药物残留检测.
  • 基金资助:

    国家质量监督检验检疫总局科研项目(No. 2007IK174)

Determination of sulfonamides, quinolones, benzimidazoles and the metabolites of benzimidazoles in chicken livers by dispersive solid-phase extraction and ultra performance liquid chromatography-tandem mass spectrometry

LI Fengge1,2*, SU Min1, LI Xiaoyan1, ZHANG Hongxia2, YAO Weiqin1, DOU Hui1, ZHANG Wanquan1   

  1. 1. Technical Center of Xinjiang Entry-Exit Inspection and Quarantine Bureau, Urumqi 830063, China; 2. Food Science Institute, Xinjiang Agricultural University, Urumqi 830063, China
  • Received:2010-10-20 Revised:2010-12-07 Online:2011-02-28 Published:2007-03-25

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摘要： 建立了一种分散固相萃取-超高效液相色谱-串联质谱(QuEChERS-UPLC-MS/MS)测定鸡肝中12种磺胺类、19种喹诺酮类和8种苯并咪唑类药物及其代谢物残留的分析方法。样品用1%乙酸-乙腈溶液提取,NH2吸附剂净化,正己烷脱脂。用Kromasil Eternity C18色谱柱(100 mm×2.1 mm, 2.5 μm)分离,以0.1%甲酸水溶液和甲醇为流动相进行梯度洗脱,电喷雾正离子(ESI+)模式电离,多反应监测模式检测,内标法定量。39种药物在5～100 μg/kg的空白添加浓度范围内线性良好(r2＞0.98);在10～50 μg/kg的添加水平范围内,平均回收率为72%～121%,相对标准偏差(RSD)为1.5%～23.4%; 39种药物的检出限(LOD)为5 μg/kg,定量限(LOQ)为10 μg/kg。该方法简便、快速、灵敏、准确,适合鸡肝中磺胺类、喹诺酮类和苯并咪唑类药物残留的确证和定量测定。

关键词: 苯并咪唑, 超高效液相色谱-串联质谱法, 分散固相萃取, 磺胺, 鸡肝, 喹诺酮

Abstract: A method for the determination of 12 sulfonamides, 19 quinolones and 8 benzimidazoles and the metabolites of benzimidazoles in chicken livers by quick, easy, cheap, effective, rugged and safe (QuEChERS) extraction and ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) has been developed. The samples were extracted with 1% acetic acid-acetonitrile solution, cleaned up with amine (NH2) sorbent and defatted with n-hexane. The identification and quantification were achieved by using electrospray ionization in positive ion mode (ESI+) with multiple reaction monitoring (MRM). The matrix-matched internal standard calibration curves were used for quantitative determination. The linear range was from 5 to 100 μg/kg. The average recoveries and relative standard deviations were 72%~121% and 1.5%~23.4% respectively in the spiked range of 10~50 μg/kg. The limits of detection were 5 μg/kg and the limits of quantification were 10 μg/kg for the 39 drugs. The method is simple, rapid, sensitive and accurate. It is suitable for the quantitative determination and confirmation of 12 sulfonamides, 19 quinolones, 8 benzimidazoles and the metabolites of benzimidazoles.

Key words: amine(NH2) sorbent, benzimidazoles, chicken livers, multiresidue, QuEChERS, quinolones, sulifonamides, ultra performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）

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