Online solid phase extraction LC–MS/MS method for the analysis of succinate dehydrogenase inhibitor fungicides and its applicability to surface water samples
Online solid phase extraction LC–MS/MS method for the analysis of succinate dehydrogenase inhibitor fungicides and its applicability to surface water samples
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DOI：
10.1007/s00216-014-8073-4
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发表时间：
2014-08
影响因子：
4.3
通讯作者：
A. Gulkowska;I. J. Buerge;T. Poiger
中科院分区：
文献类型：
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作者：
A. Gulkowska;I. J. Buerge;T. Poiger
开发并验证了一种基于在线固相萃取与 LC-MS/MS 联用的灵敏且选择性的分析方法，用于测定地表水和废水中最近引入的几种杀菌剂的痕量。目标分析物列表包括八种琥珀酸脱氢酶抑制剂（联苯吡菌胺、啶酰菌胺、氟吡菌酰胺、氟吡菌胺、fluxapyroxad、isopyrazam、penflufen 和吡噻菌胺），以及另外两种具有不同作用方式的杀菌剂：fenpyrazamine 和 Fluopicolide。各种基质的检测限和定量限分别在 0.1 至 2 和 0.5 至 10 ng/L 范围内。在地表水 (≤15%) 和废水 (≤25%) 中观察到中等信号抑制，并通过所选内标得到了很好的补偿。日内和日间精度通常分别<10% 和<20%。该方法的适用性在一项针对瑞士格拉特河中杀菌剂发生情况的研究中得到了证明，该河流域面积为 419 平方公里，其中大部分为农业用地。在所研究的化合物中，在与流量成比例的每周复合样品中仅检测到啶酰菌胺和氟吡考利特，通常浓度分别低至 15 ng/L 和 5 ng/L。虽然只有 30% 的样品检测到 LOD 高于 0.5 ng/L，但在 2012 年 3 月至 10 月分析的所有样品中均检测到啶酰菌胺。图解摘要 2012 年瑞士格拉特河按流量比例每周复合水样中杀菌剂啶酰菌胺和氟吡菌胺的浓度
A sensitive and selective analytical method, based on online solid phase extraction coupled to LC–MS/MS, was developed and validated to determine traces of several recently introduced fungicides in surface water and wastewater. The list of target analytes included eight succinate dehydrogenase inhibitors (bixafen, boscalid, fluopyram, flutolanil, fluxapyroxad, isopyrazam, penflufen, and penthiopyrad), and two other fungicides with different modes of action, fenpyrazamine and fluopicolide. Detection and quantification limits in various matrices were in the range of 0.1 to 2 and 0.5 to 10 ng/L, respectively. Moderate signal suppression was observed in surface water (≤15 %) and wastewater (≤25 %) and was well compensated by the selected internal standard. The intra- and inter-day precisions were generally <10 and <20 %, respectively. The applicability of the method was demonstrated in a study on the occurrence of fungicides in the river Glatt, Switzerland, that drains a catchment area of 419 km2with a substantial proportion of agricultural land. Of the studied compounds, only boscalid and fluopicolide were detected in flow-proportional weekly composite samples, generally at low concentrations up to 15 and 5 ng/L, respectively. While fluopicolide was detected in only 30 % of the samples above the LOD of 0.5 ng/L, boscalid was detected in all samples analyzed between March and October 2012.Graphical AbstractConcentration of the fungicides boscalid and fluopicolide in flow-proportional weekly-composite watersamples from River Glatt, Switzerland in 2012