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

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：0.1 mL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,检出限为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%.

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：0.1mL 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 0.1~100μg/L and low detection limits of 0.027~0.078μg/L.The method was applied to determine sulfonamides in milk with recoveries of 88.3%~113.6%.