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Separation of Seven Residues of Fluoroquinolones from Fish Samples using Solid Phase Microextraction and Electrophoresis and their detection by Electrochemiluminescence method

机译:使用固相微萃取和电泳与鱼样品的荧光喹啉的七个残留物分离及其通过电化学荧光法检测

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A new method for the simultaneous determination of 7 fluoroquinolones (FQs) in fish was establishedbased on purifing and enriching by solid phase microextraction, separating by capillary electrophoresis(CE) and detecting by column end electrochemiluminescence. The effects of pH value, extraction time,extraction temperature, ionic strength and eluate type on the extraction efficiency of 7 FQs wereinvestigated. The effects of buffer additives and separation voltage on the separation efficiency of 7FQs were investigated. The best purification and enrichment parameters of 10.0 ml extraction solutionmade from 2.0 g fish sample are: pH value of extraction system is 7, extraction time is 40 min,extraction temperature is 50 °C, addition of NaCl is 2.0 g, and eluate is 2.0 ml methanol (containing5% formic acid). The separation solution of CE is 0.02 mol/L phosphate buffer solution (pH=6,containing 18% cyclodextrin), and the separation voltage is 20 kV. All the 7 FQs have good linearrelationship. Their detection limits were 0.4-0.8 μg/L. The recovery of fish samples was 89.2%-110.4%.4 FQs were detected in two fish samples. This method has the advantages of small matrix effect, highsensitivity, simplicity and accuracy. It can be used for the detection of FQs in other fish or meat..
机译:通过固相微萃取,通过固相微萃取,通过固相微萃取,通过固相微萃取,通过毛细管电泳(Ce)分离并通过柱末端电荧光检测来确定鱼中7种氟喹啉酮(FQs)的新方法。 pH值,提取时间,提取温度,离子强度和洗脱液对7个FQs的提取效率的影响。研究了缓冲剂添加剂和分离电压对7FQs分离效率的影响。从2.0g鱼样品的最佳纯化和富集参数为10.0mL萃取溶液,是:提取系统的pH值为7,提取时间为40分钟,提取温度为50℃,加入NaCl为2.0g,洗脱液为2.0 ml甲醇(含5%甲酸)。 Ce的分离溶液是0.02mol / L磷酸盐缓冲溶液(pH = 6,含有18%环糊精),分离电压为20kV。所有7个FQS都有良好的线性条形。它们的检测限为0.4-0.8μg/升。在两种鱼样品中检测到鱼类样品的回收率为89.2%-110.4%。该方法具有小的矩阵效果,耐高感,简单和精度的优点。它可用于检测其他鱼或肉类的FQ。

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