色谱

色谱 ›› 2015, Vol. 33 ›› Issue (6): 590-596.DOI: 10.3724/SP.J.1123.2015.02062

• 研究论文 • 上一篇    下一篇

疏水整体柱在线固相萃取与高效液相色谱-串联质谱联用测定牛肝中5种阿维菌素类药物残留

李欣1, 张瑶琴1, 艾连峰2, 王学生1, 王曼曼1, 徐厚君1, 郝玉兰1   

  1. 1. 华北理工大学公共卫生学院, 河北 唐山 063000;
    2. 河北出入境检验检疫局, 河北 石家庄 050000
  • 收稿日期:2015-03-20 出版日期:2015-06-08 发布日期:2015-05-26
  • 通讯作者: 王学生
  • 基金资助:

    国家自然科学基金项目(21305028);河北省自然科学基金项目(B2013209238);河北省高等学校科学研究计划项目(Q2012155);国家质检总局项目(2013IK154,2014IK092).

Determination of five avermectins in bovine liver by on-line solid-phase extraction with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry

LI Xin1, ZHANG Yaoqin1, AI Lianfeng2, WANG Xuesheng1, WANG Manman1, XU Houjun1, HAO Yulan1   

  1. 1. School of Public Health, North China University of Science and Technology, Tangshan 063000, China;
    2. Hebei Entry-Exit Inspection and Quarantine Bureau, Shijiazhuang 050000, China
  • Received:2015-03-20 Online:2015-06-08 Published:2015-05-26

PDF

177

被引次数

5

摘要：

建立了牛肝中5种阿维菌素类药物残留的疏水整体柱在线固相萃取结合高效液相色谱-串联质谱测定的方法。以疏水的聚(甲基丙烯酸丁酯-乙二醇二甲基丙烯酸酯)整体柱(10 mm×2.1 mm)作为固相萃取介质,考察了上样流动相和洗脱流速对阿维菌素类药物的萃取效果,优化了梯度洗脱流动相的种类及质谱条件。方法在1~100 μg/L范围内线性关系良好(r>0.995),定量限为5 μg/kg。在5、10、50、100 μg/kg添加水平的回收率为77.4%~98.4%,日内和日间相对标准偏差分别为4.46%~8.03%和4.79%~8.68%,并且该柱反复使用400次后未发现萃取效率降低。结果表明,该整体柱对牛肝中5种阿维菌素类药物能够有效萃取,并且可以重复使用。该方法简单,自动化程度高,可应用于常规阿维菌素类药物残留分析。

关键词: 阿维菌素类药物, 高效液相色谱-串联质谱, 牛肝, 疏水整体柱, 在线固相萃取

Abstract:

A method based on on-line solid-phase extraction (SPE) with hydrophobic monolithic column coupled with high performance liquid chromatography-tandem mass spectrometry was developed for the simultaneous determination of five avermectins in bovine liver. A poly(butyl methacrylate-co-ethylene dimethacrylate) monolithic column was used as the sorbent. The parameters influenced on on-line SPE and separation process such as the loading mobile phase, the eluting flow rate and the solvent for the separation were investigated in detail. Blank samples, spiked samples, matrix effect and recovery experiments were investigated to evaluate the extraction efficiency and potential interfering compounds originating from the matrix. Under the optimized conditions, the method showed a linear range of 1-100 μg/L and the quantification limit of 5 μg/kg for each analyte. The presented method gave recoveries of 77.4%-98.4%. The relative standard deviations of intra-day and inter-day were 4.46%-8.03% and 4.79%-8.68%, respectively. Moreover, no significant changes were found in the extraction performance after more than 400 usages on one monolithic column, and even on the monoliths with various batches. The feasibility of the developed poly(butyl methacrylate-co-ethylene dimethacrylate) monolithic column based on the on-line SPE method for the determination of avermectins was further demonstrated by the analysis of real samples.

Key words: avermectins, bovine liver, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), hydrophobic monolithic column, on-line solid-phase extraction

中图分类号: