色谱Issue(6)：590-596,7.DOI:10.3724/SP.J.1123.2015.02062
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
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
摘要
Abstract
A method based on on-line solid-phase extraction( SPE)with hydrophobic mono-lithic 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 sor-bent. 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 investiga-ted 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 determi-nation of avermectins was further demonstrated by the analysis of real samples.关键词
疏水整体柱/在线固相萃取/高效液相色谱-串联质谱/阿维菌素类药物/牛肝Key words
hydrophobic monolithic column/on-line solid-phase extraction/high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)/avermectins/bovine liver分类
化学化工引用本文复制引用
李欣,张瑶琴,艾连峰,王学生,王曼曼,徐厚君,郝玉兰..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[J].色谱,2015,(6):590-596,7.基金项目
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）． （）
