王玲玲, 吴志伟. 基于新型固相萃取 - 高效液相色谱法灵敏测定牛奶中的药物残留[J]. 信阳师范学院学报(自然科学版), 2015, 28(4): 559-562. DOI: 10.3969/j.issn.1003-0972.2015.04.023
引用本文: 王玲玲, 吴志伟. 基于新型固相萃取 - 高效液相色谱法灵敏测定牛奶中的药物残留[J]. 信阳师范学院学报(自然科学版), 2015, 28(4): 559-562. DOI: 10.3969/j.issn.1003-0972.2015.04.023
Wang Lingling , Wu Zhiwei . Determination of Drug Residue in Milk with Novel Solid Extraction-High Performance Chromatography[J]. Journal of Xinyang Normal University (Natural Science Edition), 2015, 28(4): 559-562. DOI: 10.3969/j.issn.1003-0972.2015.04.023
Citation: Wang Lingling , Wu Zhiwei . Determination of Drug Residue in Milk with Novel Solid Extraction-High Performance Chromatography[J]. Journal of Xinyang Normal University (Natural Science Edition), 2015, 28(4): 559-562. DOI: 10.3969/j.issn.1003-0972.2015.04.023

基于新型固相萃取 - 高效液相色谱法灵敏测定牛奶中的药物残留

Determination of Drug Residue in Milk with Novel Solid Extraction-High Performance Chromatography

  • 摘要: 利用水热法制备了还原氧化石墨烯 - 硅胶复合物, 将其用于固相萃取柱制备, 并与高效液相色谱相结合, 建立了牛奶中磺胺类药物测定的新方法 . 对萃取条件进行了优化, 优化条件为: 0.1mL的甲醇 - 乙酸( V ∶V ' =1∶1. 5 ) 混合液为洗脱剂, 75mL的样品溶液 . 在优化条件下, 目标物的线性范围为 0.1~100μg/L , 出限为 0.027~0.078μg /L( RSN =3 ) . 新方法用于牛奶样品分析, 加标回收率为 88.3%~113.6%.

     

    Abstract: Reduced graphene oxide-silica gel composites were prepared by hydrothermal method and used as adsorbents of solid phase extraction column. A new method was developed for sensitive determination of sulfonamides in milk by solid-phase extraction coupled with high-performance liquid phase chromatography. The extraction conditions were optimized as follows: 0.1 mL methanol-acetic acid solution(V∶V′=1∶1.5)was selected as eluent and the volume of sample were 75 mL. The developed method showed a wide linear range of 0.1~100 μg/L and low detection limits of 0.027~0.078 μg/L. The method was applied to determine sulfonamides in milk with recoveries of 88.3%~113.6%

     

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