【摘要】 本实验对蜂王浆中链霉素残留的提取净化及液相色谱检测方法进行研究。蜂王浆样品用含有蛋白沉淀剂的磷酸提取液(pH2.0)溶解,超声波辅助提取蜂王浆中的链霉素残留。样液经离心后,分别用阳离子交换柱和反相固相萃取柱净化。采用柱后衍生-高效液相色谱梯度洗脱与荧光检测分析蜂王浆中的链霉素残留。以Atlantis HILIC Silica(2.1mm×150mm,3.0μm)为色谱柱,以酸性水溶液和乙腈为流动相,链霉素在25min内实现较好的分离,方法快速准确,灵敏度高,是一种较好的定性和定量方法。所研究的提取净化方法及色谱分离条件能有效排除蜂王浆中的杂质干扰,添加回收率在71.7%～77.4%之间,方法检出限为10μg/kg。更多还原

【Abstract】 In this study,the royal jelly samples were dissolved in phosphorus solution(pH 2) containing protein precipitator to extract streptomycin residue by means of ultrasonic.The sample extract was cleaned up by cation exchange column and reverse-phase column,while the streptomycin was eluted off via SPE cartridge with methanol and evaporate to dryness on nitrogen dry evaporator,and the residues were dissolved in mobile phase and then passed through 0.45 μm filter for determination by a liquid chromatography FLD detection with post-column derivatization.A Atlantis HILIC Silica(2.1 mm×150 mm,3.0 μm) was as chromatographic separation column,and the mixed solution of acidic aqueous solution and acetonitrile was as mobile phase under gradient elution.The total analysis time is less than 25 min.The spiked recoveries are 71.7% to 77.4%.The limit of detection of the method is 10 μg/kg.更多还原