色谱

色谱 ›› 2016, Vol. 34 ›› Issue (11): 1063-1069.DOI: 10.3724/SP.J.1123.2016.07024

• 研究论文 • 上一篇    下一篇

分子印迹固相萃取-超高效液相色谱-串联质谱法测定鸡肉中9种氟喹诺酮药物残留

杨艳菲1,2, 曹旭敏2,3, 李雪莲4, 宋建德2, 孙晓亮2,3, 王淑婷2,3, 王晓茵2,3, 李琳1, 赵思俊2,3   

  1. 1. 安徽农业大学动物科技学院, 安徽 合肥 230000;
    2. 中国动物卫生与流行病学中心, 山东 青岛 266032;
    3. 农业部畜禽产品质量安全风险评估实验室(青岛), 山东 青岛 266032;
    4. 青岛易邦生物工程有限公司, 山东 青岛 266032
  • 收稿日期:2016-07-24 出版日期:2016-11-08 发布日期:2016-11-03
  • 通讯作者: 李琳, 赵思俊
  • 基金资助:

    国家畜禽质量安全风险评估项目（GJFP201600706）；中国动物卫生与流行病学中心创新基金项目（2014IF-0003FF）.

Determination of nine fluoroquinolone residues in chicken by ultra performance liquid chromatography-tandem mass spectrometry coupled with molecularly imprinted solid phase extraction

YANG Yanfei1,2, CAO Xumin2,3, LI Xuelian4, SONG Jiande2, SUN Xiaoliang2,3, WANG Shuting2,3, WANG Xiaoyin2,3, LI Lin1, ZHAO Sijun2,3   

  1. 1. College of Animal Science and Technology, Anhui Agriculture University, Hefei 230000, China;
    2. China Animal Health and Epidemiology Center, Qingdao 266032, China;
    3. Livestock and Poultry Products Quality and Safety Risk Assessment Laboratory, Ministry of Agriculture(Qingdao), Qingdao 266032, China;
    4. Qingdao Yebio Biological Engineering Co., Ltd., Qingdao 266032, China
  • Received:2016-07-24 Online:2016-11-08 Published:2016-11-03
  • Supported by:

    National Livestock Quality and Safety Risk Assessment Project (No. GJFP201600706); Innovation Fund of China Animal Health and Epidemiology Center (No. 2014IF-0003FF).

PDF

123

被引次数

6

摘要：

建立了分子印迹固相萃取（MISPE）-超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定鸡肉中9种氟喹诺酮药物残留的分析方法。样品经均质处理后，采用磷酸盐缓冲液提取，提取液经MISPE柱净化后，采用BEH C18柱分离，以乙腈-0.1%（v/v）甲酸水溶液为流动相，梯度洗脱，采用电喷雾正离子多反应监测模式，外标法定量。考察了MISPE柱对9种氟喹诺酮药物的吸附特异性；9种药物在0.25~100 μg/L范围内线性关系良好，相关系数（r）>0.9965；检出限和定量限分别为0.08 μg/kg和0.25 μg/kg；在0.25、2.5、5.0 μg/kg添加水平下，9种药物的回收率为65.8%~112.2%，批内、批间RSD分别为0.6%~13.5%和0.5%~14.9%；MISPE的最大柱容量为464.7~932.4 μg/L。该方法灵敏度好、操作简单、快速。

关键词: 超高效液相色谱-串联质谱, 分子印迹固相萃取, 氟喹诺酮, 鸡肉

Abstract:

An ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method coupled with molecularly imprinted solid phase extraction (MISPE) for the determination of nine fluoroquinolone residues in chicken was developed. The samples were extracted with phosphate buffer solution, and cleaned up with MISPE columns. Then the drugs were analyzed on a BEH C18 column by gradient elution with acetonitrile and 0.1% (v/v) formic acid solution as mobile phase. The samples were analyzed in electrospray positive ion mode and multiple reaction monitoring (MRM) mode. The analytes were quantified by external standard method. The specific adsorption of MISPE for the nine fluoroquinolones in chicken samples was investigated. The linear ranges were 0.25-100 μg/L with correlation coefficients (r) greater than 0.9965. The limits of detection (LODs, S/N=3) and the limits of quantification (LOQs, S/N=10) were 0.08 μg/kg and 0.25 μg/kg, respectively. At the spiked levels of 0.25, 2.5, 5.0 μg/kg, the recoveries were 65.8%-112.2% with the intra-RSDs of 0.6%-13.5% and inter-RSDs of 0.5%-14.9%, respectively. The maximum capacities of the MISPE column were 464.7-932.4 μg/L. The method is sensitive, simple and rapid for the simultaneous determination of the nine fluoroquinolone residues.

Key words: chicken, fluoroquinolones, molecularly imprinted solid phase extraction (MISPE), ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)

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