Determination of Fluoroquinolone Antibiotic in Milk with Graphene HF-SPME-HPLC
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摘要: 建立了一种石墨烯中空纤维固相微萃取-高效液相色谱联用测定牛奶中6种氟喹诺酮类药物的方法。以中空纤维为模板,石墨烯为增强体,采用溶胶-凝胶法制备了石墨烯中空纤维。以最大峰面积为标准考察了影响萃取效率的因素。结果表明,最佳实验条件为解析液为乙腈(含5%甲酸)1.0 mL,样品体积10.0 mL,NaCl 2.0 g,萃取体系pH=7,萃取温度为50℃。在最佳实验条件下,富集倍数为14.2~30.8,6种氟喹诺酮药物线性良好,方法检出限为0.38~0.70 μg/L,相对标准偏差为2.4%~8.5%,牛奶中加标回收率为75.2%~95.4%。在品牌牛奶2和市售鲜奶中分别检出2.1 μg/L诺氟沙星和4.8 μg/L沙氟沙星。该样品处理方法基质效应小、灵敏度高、简便、准确,可用于牛奶中残留氟喹诺酮类药物的检测。Abstract: A method for determination of 6 fluoroquinolones in milk by graphene hollow solid phase microextraction coupled with high performance liquid chromatography(HPLC)was established. Graphene hollow fiber was prepared by sol-gel method using hollow fiber as template and graphene as reinforcement. Taking the maximum chromatographic peak area as an indicator,the factors affecting extraction efficiency were investigated. Results showed that,the best experimental conditions with acetonitrile(1.0 mL,5% formic acid)as disorption solution,sample solution volume 10 mL,pH7,NaCl 2.0 g,extraction temperature 50℃. Enrichment factor ranged from 14.2 to 30.8. The linear range of 6 fluoroquinolone drugs was 0.38~0.70 μg/L,the relative standard deviation was between 2.4% and 8.5%,and the recovery rate was 75.20%~95.4%. 2.1 μg/L norfloxacin and 4.8 μg/L ofloxacin were detected in brand milk 2 and market fresh milk respectively. This method with low matrix effect is sensitive,simple,accurate,and can be successfully applied to the detection of residual fluoroquinolones in milk.
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