液相色谱-串联质谱法检测蜂蛹粉中链霉素及双氢链霉素的残留量

Detemination of streptomycin and dyhydrostreptomycin in bee pupa powder by liquid chromatography-tandem mass spectrometry

中文关键词:  蜂蛹粉  固相萃取  链霉素  双氢链霉素  液相色谱-串联质谱法

英文关键词:bee pupa powder  solid phase extraction  streptomycin  dyhydrostreptomycin  liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立全自动固相萃取-液相色谱-串联质谱法测定蜂蛹粉中链霉素及双氢链霉素含量的分析方法。方法 样品经磷酸缓冲溶液提取, 高氯酸沉淀蛋白后, 采用waters HLB固相萃取小柱净化, 以Protemix WCX色谱柱进行色谱分离, 多反应监测模式测定, 外标法定量。结果 结果表明2种化合物在10~200 μg/kg的浓度范围内线性关系良好, 检出限为5 μg/kg, 定量限为10 μg/kg。空白蜂蛹粉样品的3水平加标回收率为80.6%~93.5%, 相对标准偏差为4.7%~8.8%。结论 该方法适用于蜂蛹粉中链霉素和双氢链霉素残留的检测。

英文摘要:

      Objective To establish a method for the determination of streptomycin and dihydrostreptomycin in bee pupa powder by automatic solid phase extraction liquid chromatography-tandem mass spectrometry. Methods The samples were extracted by phosphoric acid buffer solution, the protein was precipitated by perchloric acid, and purified by the small column of waters HLB solid phase extraction. The chromatographic separation was carried out by Protemix WCX chromatographic column, and the multi-reaction monitoring mode was used for determination. The external standard method was used for quantitative analysis. Results The results showed that the 2 compounds had a good linear relationship in the range of 10?200 μg/kg, the limit of detection was 5 μg/kg, and the limit of quantitative was 10 μg/kg. The recoveries of blank bee pupa powder at 3 spiked levels were 80.6%?93.5%, with the relative standard deviations of 4.7%?8.8%. Conclusion This method is suitable for the determination of streptomycin and dihydrostreptomycin residues in bee pupa powder.