蜂王浆中八种磺胺类药物残留测定方法研究

Determination of Eight Sulfonamides Residue in Royal Jelly by Using High Performance Liquid Chromatography with Fluorescence Detector

建立蜂王浆中八种磺胺类药物残留的固相萃取-高效液相色谱荧光分析方法。蜂王浆样品中的磺胺类药物残留用含沉淀剂的乙酸乙酯提取,提取液旋转浓缩近干后,用磷酸缓冲溶液溶解,再经OasisHLB固相萃取柱净化,洗脱液经氮气吹干后,用盐酸和乙酸钠溶解,样液经荧光胺衍生后,用高效液相色谱分析,采用外标法定量。该方法的检测限为10～50μg/kg,回收率在62.3%～74.8%之间,能满足目前蜂王浆中磺胺类药物残留测定要求。

A method for determination of eight sulfonamides residue in royal jelly by using solid-phase extraction high performance liquid chromatography with fluorescence detector was established. Sulfonamides residue was extracted with ethyl acetate containing protein precipitator. The sample extract was evaporated under reduced pressure and dissolved with phosphate buffer solution, and then purified by using an Oasis HLB column, while the sulfonamides residue was eluted offvia solid-phase extraction （SPE） cartridge with methanol and evaporated to dryness on nitrogen dry evaporator, and the residues were dissolved in and sodium acetate solution. Sulfonamides residue was derivatized by using fluorescamine. The sulfonamides derivates were detected by a liquid chromatography with fluorescence detector. The recoveries are 62.3% to 74.8%, and the limit of detection of the metshod is 10 to 50μg/kg. The developed method is suitable to monitor sulfonamides residue in royal jelly samples.