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采用离子对液相色谱-串联质谱法分析优化氨基糖苷类抗生素,并将其应用于废水样品。

Aminoglycosides analysis optimization using ion pairing liquid chromatography coupled to tandem mass spectrometry and application on wastewater samples.

机构信息

Univ Lyon, CNRS, Université Claude Bernard Lyon 1, Institut des Sciences Analytiques, UMR 5280, 5 Rue de la Doua, F-69100 Villeurbanne, France.

Environmental Microbial Genomics, Laboratoire Ampère, UMR 5005, CNRS, Ecole Centrale de Lyon, Université de Lyon, 69134 Ecully.

出版信息

J Chromatogr A. 2021 Aug 16;1651:462133. doi: 10.1016/j.chroma.2021.462133. Epub 2021 Apr 2.

Abstract

Aminoglycosides are mostly used as veterinary antibiotics. In France, their consumption accounts for about 10% of all prescribed animal medicine. Due to their high polarity nature (log Kow < -3), they require chromatographic separation by hydrophilic interaction liquid chromatography or ion-pairing chromatography. This study presents the development of an ion pairing liquid chromatography with alkanesulfonates coupled to tandem mass spectrometry for the analysis of 10 aminoglycosides (spectinomycin, streptomycin, dihydrostreptomycin, kanamycin, apramycin, gentamicin, neomycin and sisomicin) in wastewater samples. The novelty of this method lies in the addition of the ion paring salt directly and only into the sample vial and not in the mobile phase, lowering the amount of salt added and consequently reducing signal inhibition. The optimized method was validated and showed satisfactory resolution, performances suitable with the analysis of aminoglycosides in wastewater samples, with limits of quantifications less than 10 ng/mL for most of the compounds, low matrix effects, high accuracy (85%-115% recoveries) and reproducibility (2%-12%RSD). It was then applied successfully to raw and treated wastewater samples.

摘要

氨基糖苷类抗生素主要用作兽用抗生素。在法国,它们的使用量约占所有规定的动物用药的 10%。由于其高极性性质(log Kow < -3),它们需要通过亲水相互作用液相色谱法或离子对色谱法进行色谱分离。本研究提出了一种烷磺酸盐与串联质谱联用的离子对液相色谱法,用于分析废水样品中的 10 种氨基糖苷类抗生素(大观霉素、链霉素、双氢链霉素、卡那霉素、安普霉素、庆大霉素、新霉素和西索米星)。该方法的新颖之处在于直接且仅将离子对盐添加到样品小瓶中,而不是在流动相中,从而减少了添加的盐量,进而降低了信号抑制。优化后的方法经过验证,显示出令人满意的分辨率,适用于废水样品中氨基糖苷类抗生素的分析,大多数化合物的定量限小于 10ng/mL,基质效应低,准确度高(85%-115%回收率)和重现性好(2%-12%RSD)。然后成功地将其应用于原水和处理后的废水样品中。

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