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Determination of tetracycline residues in lake water by on-line coupling of molecularly imprinted solid-phase extraction with high performance liquid chromatography

机译:分子印迹固相萃取-高效液相色谱在线耦合法测定湖水中四环素残留

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A new method has been developed for the determination of tetracycline residues in water samples by on-line solid-phase extraction-HPLC analysis method. Tetracycline-imprinted microspheres, synthesized by reversible additiona€“fragmentation chain transfer precipitation polymerization, were applied for the extraction of the tetracyclines. Tetracycline residues were selectively extracted from 10.0 mL lake water using the molecularly imprinted solid-phase extraction (MISPE) method. After the sample clean-up, tetracyclines were back-flushed into a reversed-phase C18 analytical column and oxytetracycline, tetracycline and doxycycline were separated for quantification. The recoveries of three tetracyclines in the spiked lake water were between 83.2% and 111.0% with relative standard deviations (RSDs) 5.3%, demonstrating that the established MISPE-HPLC method has good accuracy and precision. Linearity in the range of 1a€“200 ??g La?’1 was obtained. The detection limits and quantification limits for the analytes were 0.08a€“1.02 ??g La?’1 and 0.41a€“3.56 ??g La?’1, respectively. The enhancement factors, which ranged from 376 to 528, indicated that the MISPE has the ability to enrich trace tetracycline residues. The results demonstrated that this method can be used in the determination of tetracyclines in environmental water samples with good sensitivity and efficiency.
机译:建立了在线固相萃取-HPLC分析法测定水样中四环素残留的新方法。通过可逆加成和“片段链转移沉淀聚合”法合成的四环素印迹微球被用于四环素的提取。使用分子印迹固相萃取(MISPE)方法从10.0 mL湖水中选择性地萃取四环素残留物。样品净化后,将四环素回冲到反相的C18分析柱中,并分离出土霉素,土霉素和强力霉素进行定量。加标的湖水中三种四环素的回收率在83.2%至111.0%之间,相对标准偏差(RSD)<5.3%,表明所建立的MISPE-HPLC方法具有良好的准确性和精密度。获得的线性范围为1a€200 g La?1。分析物的检出限和定量限分别为0.08a€“ 1.02 g?La?1”和0.41a€“ 3.56?g La?'1。增强因子介于376至528之间,表明MISPE具有富集痕量四环素残基的能力。结果表明,该方法可用于环境水样中四环素类的测定,具有良好的灵敏度和效率。

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