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A new approach for the extraction of tetracyclines from soil matrices: application of the microwave-extraction technique
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2018-01-19 , DOI: 10.1007/s00216-017-0815-7
Paulina Łukaszewicz , Anna Białk-Bielińska , Joanna Dołżonek , Jolanta Kumirska , Magda Caban , Piotr Stepnowski

The widespread use of tetracyclines (TCs) in animal husbandry is associated with their constant penetration into the environment and the threat they might pose to living organisms. While the literature data on the analysis of these substances in such matrices as food, tissues, or wastewater are quite extensive, there are still only a few methods presented for the determination of these compounds in soil samples. Moreover, among the literature methods for the extraction of TCs from soil samples, microwave-assisted solvent extraction (MAE) was used only once and in combination with liquid chromatography with spectrophotometric detection (LC-UV). However, according to the EU Commission Decision 2002/657/EC, the use of LC-UV for the determination of compounds, including pharmaceuticals, in environmental samples is not sufficient. Therefore, the development and application of a sensitive and selective method using the MAE-SPE-LC-MS/MS(MRM) technique for the isolation and identification of a mixture of oxytetracycline (OTC), tetracycline (TC), and chlortetracycline (CTC) in soils is presented in our study. The credibility of this method has been confirmed with good parameters of validation. The optimal extraction conditions of three TCs using MAE techniques were to conduct double extraction for 10 min each, at 60 °C, using a mixture of ACN:McIlvaine buffer:0.1 M EDTA (2:1:1, v/v/v) and an additional cleaning of the extracts by SPE. The effectiveness of the extraction of these compounds was assessed based on two different ways (absolute recovery from 46 to 65.1% and relative recovery from 101.1 to 109.5%). Finally, the validated MAE-SPE-LC-MS/MS(MRM) method was used for the analysis of six samples from agricultural areas of northern Poland. OTC and TC, at concentrations of 11.7 and 14.5 μg kg−1 were determined in two different samples. An assessment of risk quotients was also performed. The presented method was proven to be a useful tool in the analysis of residues of selected TCs in the soil ecosystem. Obtained data on the presence of these drugs in Polish soils is the first report for this country.



中文翻译:

从土壤基质中提取四环素的新方法:微波萃取技术的应用

四环素在畜牧业中的广泛应用与其不断渗透到环境中以及它们可能对活生物体构成的威胁有关。尽管有关在食物,组织或废水等基质中分析这些物质的文献数据非常丰富,但仍仅提供了几种测定土壤样品中这些化合物的方法。此外,在从土壤样品中提取TC的文献方法中,微波辅助溶剂提取(MAE)仅使用一次,并与带分光光度检测的液相色谱法(LC-UV)结合使用。但是,根据欧盟委员会第2002/657 / EC号决定,仅使用LC-UV测定环境样品中的化合物(包括药物)是不够的。所以,MAE-SPE-LC-MS / MS(MRM)技术开发灵敏,选择性的方法,用于分离和鉴定土霉素,四环素和金霉素的混合物在我们的研究中介绍了土壤。该方法的可信度已通过验证的良好参数得到证实。使用MAE技术的三个TC的最佳提取条件是在60°C下使用ACN:McIlvaine缓冲液:0.1 M EDTA(2:1:1,该方法的可信度已经通过验证的良好参数得到了证实。使用MAE技术的三个TC的最佳提取条件是在60°C下使用ACN:McIlvaine缓冲液:0.1 M EDTA(2:1:1,该方法的可信度已经通过验证的良好参数得到了证实。使用MAE技术的三个TC的最佳提取条件是在60°C下使用ACN:McIlvaine缓冲液:0.1 M EDTA(2:1:1,v / v / v)并通过SPE额外清洁提取物。基于两种不同的方法评估了这些化合物的提取效果(绝对回收率从46%降低至65.1%,相对回收率从101.1%降低至109.5%)。最后,将经过验证的MAE-SPE-LC-MS / MS(MRM)方法用于分析波兰北部农业地区的六种样品。在两个不同的样品中测定了11.7和14.5μgkg -1浓度的OTC和TC 。还对风险商进行了评估。事实证明,所提出的方法是分析土壤生态系统中所选TC残留的有用工具。获得的有关波兰土壤中这些药物存在的数据是该国的第一份报告。

更新日期:2018-01-19
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