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Extraction of tetracycline antimicrobials from river water and sediment: a comparative study of three solid phase extraction methods

机译:从河水和沉积物中提取四环素抗菌剂:三种固相提取方法的比较研究

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Tetracyclines are ubiquitous pollutants in the aquatic environment so it is necessary to determine their levels in river water and sediment. Many extraction techniques have been suggested in previous studies. However there is lack of comparisons among them. This work compared three extraction methods Ultrasonic Assisted Tandem Solid Phase Extraction (UA-TSPE), Ultrasonic Assisted Dispersive Solid Phase Extraction (UA-DSPE) and Ultrasonic Assisted Matrix Solid Phase Dispersion (UA-MSPD) in conjunction with a complexing agent to complex metal cations, for the extraction of tetracycline antibacterials from fortified ultra-pure water, river water and sediment samples under acid conditions. Samples were analyzed on a RP-HPLC coupled to UV detection. The linear dynamic range for calibration curves of all techniques were 0.01 to 1 μgml-1 (water) and 0.01 to 1 μgg-1 (sediment) with R2 values ranging from 0.995 to 0.999. The overall recovery was in the range 92.13 to 99.62%. UA-DSPE yielded the best recoveries (at p > 0.05), range 97.23 to 99.62%. UA-TSPE was second at 94.99 to 97.75%, while UA-MSPD was third at 92.13 to 97.84% recovery. Limit of detection (LOD) (at signal to noise ratio = 3) and Limit of quantification (LOQ) (at signal to noise ratio = 10) for spiked river water and sediment were in the range 11.53 to 22.75 ngml-1 and 30.12 to 56.22 ngml-1, respectively.
机译:四环素是水生环境中普遍存在的污染物,因此有必要确定其在河水和沉积物中的含量。在先前的研究中已经提出了许多提取技术。但是,它们之间缺乏比较。这项工作比较了三种萃取方法:超声辅助串联固相萃取(UA-TSPE),超声辅助分散固相萃取(UA-DSPE)和超声辅助基质固相分散(UA-MSPD)以及与络合剂缔合的复杂金属阳离子,用于在酸性条件下从强化的超纯水,河水和沉积物样品中提取四环素抗菌素。样品在结合紫外检测的RP-HPLC上进行分析。所有技术的校准曲线的线性动态范围为0.01至1μgml-1(水)和0.01至1μgg-1(沉积物),R2值范围为0.995至0.999。总体回收率在92.13至99.62%的范围内。 UA-DSPE的回收率最高(p> 0.05),范围为97.23至99.62%。 UA-TSPE以94.99至97.75%位居第二,而UA-MSPD以92.13至97.84%的恢复位居第三。掺入的河水和沉积物的检出限(LOD)(信噪比= 3)和定量限(LOQ)(信噪比= 10)介于11.53至22.75 ngml-1和30.12至分别为56.22 ngml-1。

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