食品科学

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QuEChERS前处理方法结合高效液相色谱-串联质谱测定蜂蜜和蜂王浆中14 种喹诺酮类药物残留

张中印,赵柳微,曹葳蕤,周金慧   

  1. 1.河南科技学院资源与环境学院,河南 新乡 453003;
    2.中国农业科学院蜜蜂研究所,农业部蜂产品质量监督检验测试中心,北京 100093
  • 出版日期:2016-08-25 发布日期:2016-08-30
  • 通讯作者: 周金慧
  • 基金资助:

    国家现代农业(蜂)产业技术体系建设专项(CARS-45-41)

Simultaneous Determination of Fluoroquinolone Residues in Honey and Royal Jelly by QuEChERS and High Performance Liquid Chromatography-Tandem Mass Spectrometry

ZHANG Zhongyin, ZHAO Liuwei, CAO Weirui, ZHOU Jinhui   

  1. 1. College of Resources and Environment, Henan Institute of Science and Technology, Xinxiang 453003, China;
    2. Institute of Apicultural Research, Bee Products Quality Supervision and Inspection Center, Ministry of Agriculture,
    Chinese Academy of Agricultural Sciences, Beijing 100093, China
  • Online:2016-08-25 Published:2016-08-30
  • Contact: ZHOU Jinhui

摘要:

建立一种快速、简便的测定蜂蜜和蜂王浆中14 种喹诺酮类药物残留的分析方法。样品经1%乙酸-乙腈提取,C18-EC和N-丙基乙二胺吸附剂分散净化后以高效液相色谱-串联质谱测定。结果表明,14 种喹诺酮类药物在3 个添加水平的回收率范围为80.4%~110.2%,相对标准偏差不大于16.3%,在0.1~100 ng/mL质量浓度范围内线性关系良好,相关系数大于0.99,蜂蜜的检出限和定量限分别为0.45~2.58 ng/g和 1.51~8.59 ng/g;蜂王浆的检出限和定量限分别为0.51~3.22 ng/g和1.69 ~10.75 ng/g。该方法操作简单、灵敏度高,适用于蜂蜜和蜂王浆14 种喹诺酮类药物残留的测定。

关键词: 蜂蜜, 蜂王浆, QuEChERS前处理, 高效液相色谱-串联质谱, 喹诺酮类药物

Abstract:

A multi-residue analytical method for the determination of 14 fluoroquinolone residues in honey and royal
jelly using QuEChERS extraction coupled with high performance liquid chromatography-tandem mass spectrometry
(HPLC-MS/MS) was developed. Samples were extracted with acetonitrile containing 1% acetic acid, cleaned up by
dispersive solid phase extraction with C18-EC and PSA as absorbent. Recoveries from samples spiked at three levels were
between 80.4% and 110.2% with relative standard deviations (RSDs) lower than 16.3%. The limits of detection (LODs) and
limits of quantification (LOQs) for honey were 0.45-2.58 ng/g and 1.51-8.59 ng/g, respectively. For royal jelly, the LODs
and LOQs were 0.51-3.22 ng/g and 1.69-10.75 ng/g, respectively. The established method could meet the requirement for
the determination of fluoroquinolone residues in honey and royal jelly samples.

Key words: honey, royal jelly, QuEChERS, HPLC-MS/MS, fluoroquinolone residues

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