基于分子印迹聚合物微球的在线固相萃取-液相色谱联用技术测定牛奶中酰胺醇类药物残留

On-line Solid-Phase Extraction Using Molecularly Imprinted Polymer Microspheres in Combination with HPLC for the Determination of Amphenicols Residues in Milk

以氟苯尼考为模板分子,甲基丙烯酸为功能单体,二甲基丙烯酸乙二醇酯为交联剂,偶氮二异丁腈为引发剂,用乳液-悬浮聚合法制备分子印迹聚合物微球。将制备的微球用于固相萃取,建立酰胺醇类抗生素的在线固相萃取-高效液相色谱检测方法,优化在线萃取条件及影响因素。在最佳条件下,分离检测了牛奶中的酰胺醇类药物,实现了有效地净化,其加标回收率为80.6%～96.7%,检出限为6.8～27.8 g/kg。

Molecularly imprinted microspheres（MIMs） were synthesized using florfenicol as template molecule,methacrylic acid as functional monomer,ethylene glycoldimethacrylate as crosslinking agent,2,2-azobisisobutyronitrile as initiator by emulsion-suspension polymerization.An analytical method was established for the determination of amphenicols residue milk using on-line solid-phase extraction with the microspheres coupled with high performance liquid chromatography.Some extraction and detection conditions were investigated.Under the optimal conditions,the best separation and cleanup were obtained.The average recoveries for spiked milk were in the range of 80.6%–96.7% and the detection limits for thiamphenicol,florfenicol and chloramphenicol were 6.8,10.9 μg/kg and 27.8 μg/kg,respectively.