建立了磁性氧化石墨烯固相萃取-高效液相色谱质谱法测定环境水样中8种氟喹诺酮类抗生素的分析方法。采用一步合成法制备了磁性氧化石墨烯复合材料（GO-Fe₃O₄），并用FTIR及SEM对其进行表征。磁性固相萃取的最优条件为：以含有6%氨水的甲醇为洗脱剂，GO-Fe₃O₄的质量为8.0 mg，萃取时间为20 min。在最优条件下，8种氟喹诺酮类抗生素的检出限为0.4~1.2 ng/L。用该方法对实际水样进行分析，加标回收率为80.7%~96.5%，相对标准偏差为3.4%~8.9%。该实验方法操作简单快捷、检出限低、重现性良好，可以满足环境水样中的痕量氟喹诺酮类抗生素的分析。

An analytical method combining magnetic graphene oxide solid phase extraction,high performance liquid chromatography and mass spectrometry is developed for the determination of eight fluoroquinolone antibiotics in water samples.Graphene oxide-based magnetic nanoparticles (GO-Fe₃O₄) are synthesized by one-step method and is characterized by FTIR and SEM.The optimal conditions for magnetic solid phase extraction are that 6% ammonia in methanol (v/v) is used as elution solution,the adding amount of GO-Fe₃O₄ is 8.0 mg and the extraction time is 20 min.Under these conditions,the detection limits for eight fluoroquinolone antibiotics range from 0.4 to 1.2 ng·L^-1.This method is applied to the analysis of the environmental water samples,with recoveries between 80.7% and 96.5% and the relative standard deviations (RSDs) in the range of 3.4%-8.9%.This method is simple and fast in operation,exhibits low detection limit and good reproducibility,and can be used to determine the trace residue of fluoroquinolone antibiotics in water samples.

李欣悦(1993-),女,硕士,研究方向为环境监测分析技术,1508164698@qq.com