Popova Inna E, Morra Matthew J, Parikh Sanjai J
a 1 Department of Soil and Water Systems , University of Idaho , Moscow , ID , USA.
b 2 Department of Land, Air, and Water Resources , University of California-Davis , Davis , CA , USA.
J Environ Sci Health B. 2019;54(1):35-40. doi: 10.1080/03601234.2018.1530547. Epub 2018 Nov 8.
Veterinary antibiotics used in agriculture can be introduced into the environment through land application of animal manure, accumulating in soils and groundwaters and posing a significant risk to human health and animal well-being. As the analysis of tetracyclines in soil is challenging due to their strong interaction with soil minerals and organic carbon, the objective of this study was to develop a reliable and reproducible method for quantitative analysis of chlortetracycline and oxytetracycline, and their respective metabolites in soils. A method based on pressurized liquid extraction (PLE) with in-cell clean-up was developed for the extraction of chlortetracycline and oxytetracycline and four likely metabolites from a set of four soils. Optimized conditions included a cell size of 22 mL, soil loading of 5 g, pH of 8.0, methanol:water ratio of 3:1, 50 °C, and two cycles. Soil extracts were analysed by high-performance liquid chromatography (HPLC) coupled with ion trap mass spectrometry (MS). Recoveries of seven tetracyclines from soil ranged from 41% to 110%. The limits of detection for tetracyclines were 0.08-0.3 µg g soil, and intra- and inter-day variation ranged from 0.12-0.34%. The proposed PLE method is suitable for quantification of tetracyclines in agricultural soils at typical concentrations expected in contaminated environments.
农业中使用的兽用抗生素可通过施用动物粪便进入环境，在土壤和地下水中蓄积，对人类健康和动物福祉构成重大风险。由于四环素与土壤矿物质和有机碳的强烈相互作用，对土壤中的四环素进行分析具有挑战性，因此本研究的目的是开发一种可靠且可重复的方法，用于定量分析土壤中的金霉素、土霉素及其各自的代谢物。开发了一种基于加压液体萃取（PLE）并在萃取池中进行净化的方法，用于从四种土壤中萃取金霉素、土霉素和四种可能的代谢物。优化条件包括萃取池大小为22 mL、土壤装样量为5 g、pH值为8.0、甲醇与水的比例为3:1、温度为50°C以及进行两个循环。土壤提取物通过高效液相色谱（HPLC）与离子阱质谱（MS）联用进行分析。七种四环素在土壤中的回收率为41%至110%。四环素的检测限为0.08 - 0.3 μg/g土壤，日内和日间变化范围为0.12% - 0.34%。所提出的PLE方法适用于对受污染环境中预期的典型浓度的农业土壤中的四环素进行定量分析。
