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Highly sensitive multi-residue analysis of veterinary drugs including coccidiostats and anthelmintics in pond water using UHPLC-MS/MS: application to freshwater ponds in Flanders, Belgium.
Environmental Science: Processes & Impacts ( IF 4.3 ) Pub Date : 2020-09-18 , DOI: 10.1039/d0em00215a T Goessens 1 , S D Baere , N D Troyer , A Deknock , P Goethals , L Lens , F Pasmans , S Croubels
Environmental Science: Processes & Impacts ( IF 4.3 ) Pub Date : 2020-09-18 , DOI: 10.1039/d0em00215a T Goessens 1 , S D Baere , N D Troyer , A Deknock , P Goethals , L Lens , F Pasmans , S Croubels
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Veterinary drugs, such as coccidiostats and anthelmintics are routinely administered in extensive animal husbandry, finding their way into the aquatic environment through urine and/or feces of treated animals kept outdoors or by the application of contaminated liquid manure on agricultural fields and subsequent mechanisms of surface run-off, leaching and drift. Several of these compounds are known to exert acute and chronic toxicity effects on aquatic organisms, and can lead to changes in biodiversity and ecosystem functioning. The overall objective of this research was to develop, validate and apply a highly sensitive, multi-residue SPE-UHPLC-MS/MS method for the determination of 12 coccidiostats, registered as a feed supplement or veterinary medicine in Europe and three regularly used anthelmintics, in pond water, often functioning as amphibian habitat. Sample extraction was optimized using a fractional factorial resolution design. Pond water filtration efficiency (i.e. 80–118%, ≤25% RSD) and matrix effects (i.e. 72–119%, ≤39% RSD) were evaluated using water from respectively 3 and 20 different ponds in Flanders. By incorporating internal standards, overall results improved and adequate precision values (i.e. ≤15%) were obtained according to the EMA guidelines. Acceptable within-run and between-run apparent recoveries, satisfactory precision as well as good linearity were demonstrated according to the CD 2002/657/EC, SANTE/12682/2019 and VICH 49 guidelines, except for robenidine for which the between-day precision was between 21.0 and 34.5%. Sample storage stability studies indicated that storage at 4 °C and analysis performed within 96 hours after sampling was sufficient to avoid loss by degradation for all compounds, excluding robenidine. Values for the limit of detection (LOD) and quantification (LOQ) were in nanograms per liter, which was essential for the environmental application of this novel method. The method was successfully applied on grab water samples from the water surface of 18 different ponds across Flanders, Belgium, detecting amprolium and levamisole at concentrations below the LOQ of 2.5 ng L−1 and at 250.0 ng L−1 or below the LOQ of 250.0 ng L−1, respectively. In conclusion, our newly developed method may provide insights about the contamination status of amphibian breeding ponds.
中文翻译：
使用UHPLC-MS / MS对池塘水中的兽药（包括抗球虫药和驱虫药）进行高灵敏度的多残留分析：应用于比利时富兰德斯的淡水池塘。
兽药，例如抗球虫药和驱虫药通常在广泛的畜牧业中施用，通过在室外饲养的被处理动物的尿液和/或粪便或通过在农业领域施用受污染的液体肥料以及随后的地表机理而进入水生环境径流，淋滤和漂移。这些化合物中的几种已知对水生生物具有急性和慢性毒性作用，并可能导致生物多样性和生态系统功能的变化。这项研究的总体目标是开发，验证和应用高灵敏度，多残留的SPE-UHPLC-MS / MS方法测定12种抗球虫药，在欧洲注册为饲料补充剂或兽药，以及三种常规使用的驱虫药在池塘水中 常作为两栖动物栖息地。使用分数阶分解设计优化了样品提取。池塘水过滤效率（即80-118％，≤25％RSD）和基质效应（即使用水从在佛兰德分别为3和20个不同的池塘楼72-119％，≤39％RSD）进行了评价。通过合并内部标准，可以改善总体结果并获得足够的精度值（即≤15％）是根据EMA指南获得的。根据CD 2002/657 / EC，SANTE / 12682/2019和VICH 49准则，证明了可接受的批内和批间表观回收率，令人满意的精密度和良好的线性，但罗贝替丁的日间精密度除外在21.0和34.5％之间。样品的储存稳定性研究表明，在4°C下储存并在取样后96小时内进行分析足以避免除罗苯替丁以外的所有化合物降解引起的损失。检测限（LOD）和定量（LOQ）的值以纳克/升为单位，这对于这种新方法的环境应用至关重要。该方法已成功应用于比利时佛兰德市18个不同池塘水面的抓取水样中-1和250.0毫微克大号-1或以下的250.0的LOQ纳克大号-1，分别。总之，我们新开发的方法可以提供有关两栖繁殖池污染状况的见解。
更新日期：2020-09-24
中文翻译：
使用UHPLC-MS / MS对池塘水中的兽药（包括抗球虫药和驱虫药）进行高灵敏度的多残留分析：应用于比利时富兰德斯的淡水池塘。
兽药，例如抗球虫药和驱虫药通常在广泛的畜牧业中施用，通过在室外饲养的被处理动物的尿液和/或粪便或通过在农业领域施用受污染的液体肥料以及随后的地表机理而进入水生环境径流，淋滤和漂移。这些化合物中的几种已知对水生生物具有急性和慢性毒性作用，并可能导致生物多样性和生态系统功能的变化。这项研究的总体目标是开发，验证和应用高灵敏度，多残留的SPE-UHPLC-MS / MS方法测定12种抗球虫药，在欧洲注册为饲料补充剂或兽药，以及三种常规使用的驱虫药在池塘水中 常作为两栖动物栖息地。使用分数阶分解设计优化了样品提取。池塘水过滤效率（即80-118％，≤25％RSD）和基质效应（即使用水从在佛兰德分别为3和20个不同的池塘楼72-119％，≤39％RSD）进行了评价。通过合并内部标准，可以改善总体结果并获得足够的精度值（即≤15％）是根据EMA指南获得的。根据CD 2002/657 / EC，SANTE / 12682/2019和VICH 49准则，证明了可接受的批内和批间表观回收率，令人满意的精密度和良好的线性，但罗贝替丁的日间精密度除外在21.0和34.5％之间。样品的储存稳定性研究表明，在4°C下储存并在取样后96小时内进行分析足以避免除罗苯替丁以外的所有化合物降解引起的损失。检测限（LOD）和定量（LOQ）的值以纳克/升为单位，这对于这种新方法的环境应用至关重要。该方法已成功应用于比利时佛兰德市18个不同池塘水面的抓取水样中-1和250.0毫微克大号-1或以下的250.0的LOQ纳克大号-1，分别。总之，我们新开发的方法可以提供有关两栖繁殖池污染状况的见解。
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