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首页> 外文期刊>The Journal of automatic chemistry >Simultaneous Determination of Malachite Green, Chloramphenicols, Sulfonamides, and Fluoroquinolones Residues in Fish by Liquid Chromatography-Mass Spectrometry
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Simultaneous Determination of Malachite Green, Chloramphenicols, Sulfonamides, and Fluoroquinolones Residues in Fish by Liquid Chromatography-Mass Spectrometry

机译：通过液相色谱 - 质谱法同时测定鱼类中鱼中鱼氨酸绿，氯霉素，氟喹唑和氟喹啉残基

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A fast-analytical method using simplified extraction has been developed for the simultaneous determination of 42 compounds from 4 different classes of veterinary drugs (amphenicols, triphenylmethane, fluoroquinolones, and sulfonamides) in fish by reverse phase liquid chromatography-tandem mass spectrometry. The selection of extraction reagents was optimized using different types of microfiltration membrane, mobile phase, and LC column. Samples were extracted using 0.4% hydrochloric acid in acetonitrile and ethyl acetate and then were cleaned up using solid-phase extraction Cleanert Alumina N columns (500?mg) and Oasis hydrophilic-lipophilic balance (HLB) cartridges. The chromatographic separation was performed on a XR-ODS C_(8) column using a mobile phase of (A) 0.1% formic acid and 2?mM ammonium acetate and (B) 0.1% formic acid acetonitrile at a flow rate of 0.25?mL·min~(?1). The results indicated 67.7–112.8% recovery of 42 compounds with an intra- and interday relative standard deviations less than 10%. The limits of quantification for analytes were in the range of 0.3–1.0? μ g?kg~(?1) for samples which were satisfactory to support future surveillance monitoring. The method applicability was checked by analyzing 30 fish samples collected from local markets. Two fish samples surpassed the established MRL of 100? μ g?kg~(?1) with values of 104? μ g?kg~(?1) and 112? μ g?kg~(?1).
机译：通过反相液相色谱 - 串联质谱法在鱼中同时测定使用简化萃取的快速分析方法，用于同时测定来自4种不同兽药（Amphenicols，三苯基甲烷，氟喹啉，氟喹啉）的42种化合物。利用不同类型的微滤膜，流动相和LC柱进行优化提取试剂的选择。在乙腈和乙酸乙酯中使用0.4％盐酸萃取样品，然后使用固相萃取洁净氧化铝N柱（500μmg）和绿洲亲水 - 亲脂性平衡（HLB）盒进行清洁。使用（a）0.1％甲酸的流动相和（b）0.1％甲酸乙腈，在0.25Ωml的流速下对XR-ODS C_（8）柱进行色谱分离。 ·min〜（？1）。结果表明，42种化合物回收率67.7-112.8％，具有少于10％的内部和白天相对标准偏差。分析物的定量极限在0.3-1.0的范围内？ μg？kg〜（α1）对于令人满意，以支持未来监视监测。通过分析来自局部市场收集的30个鱼样本来检查该方法的应用。两种鱼类样本超过了100岁的MRL？ μg？kg〜（？1）值104？ μg？kg〜（？1）和112？ μg≤kg〜（？1）。

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