将基质固相分散、离子液体均相液-液微萃取和高效液相色谱法相结合,建立一种用于肌肉组织中依诺沙星、培氟沙星、诺氟沙星和恩诺沙星4种氟喹诺酮类药物的分析方法.首先以硅胶为分散剂,以200 μL1-己基-3-甲基咪唑四氟硼酸盐([C6mim]BF4)离子液体为萃取剂,pH 1.0水溶液为洗脱剂,采用基质固相分散法处理样品,目标分析物被转移至洗脱液中后,再以六氟磷酸铵为离子对试剂,采用均相液-液微萃取法分离、富集目标分析物于离子液体相中,最后通过高效液相色谱-二极管阵列检测器对目标物进行定量分析.结果表明,各化合物在线性范围内具有较好的线性关系(r＞0.997 4),检出限为2.9～8.6μg/kg,加标回收率在87.9％～105.3％之间,其相对标准偏差为2.2％～8.6％.本法操作简单,不使用有机溶剂,可广泛应用于动物肌肉组织中氟喹诺酮类抗生素的萃取与检测.%A new method based on matrix solid phase dispersion,ionic liquid-based homogeneous liquid-liquid microextraction and high performance liquid chromatography was developed for the determination of fluroquinolones (FQs),including enoxacin (ENO),pefloxacin (PEF),norfloxacin (NOR) and enrofloxacin (ENR) in muscle samples.Muscle samples were directly treated by matrix solid phase dispersion using silica gel as dispersant,200 μL of 1-hexyl-3-methylimidazolium hexafluorophosphate ([C6mim]BF4) was used as extraction solvent,and aqueous solution of pH 1.0 was used as elution solvent.After the target analytes were transferred into eluate,ammonium hexafluorophosphate was added.The eluate obtained was treated by ionic liquid-based homogeneous liquid-liquid microextraction and the analytes were enriched into the ionic liquid phase.High performance liquid chromatography with diode array detection was applied to separate and determine the target analytes.The experimental results showed that the calibration curve exhibited a good linear relationship (r ＞ 0.997 4).The limits of detection (LODs) of the method were in the range of 2.9 to 8.6 μg/kg.The recoveries were between 87.9％ and 105.3％ with relative standard deviations (RSDs) of 2.2％-8.6％.The proposed method has the advantages of simple operation and no need for organic solvent and can be extensively applied for determination of fluroquinolones in animal tissue samples.
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