磁性氧化石墨烯固相萃取-高效液相色谱质谱法测定水中的氟喹诺酮残留

Determination of fluoroquinolone residue in water samples by magnetic graphene oxide solid phase extraction and high performance liquid chromatography-mass spectrometry

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-Fe_3O_4),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-Fe_3O_4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-Fe_3O_4） 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-Fe_3O_4 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.