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Vacuum-assisted evaporative concentration combined with LC-HRMS/MS for ultra-trace-level screening of organic micropollutants in environmental water samples

机译:真空辅助蒸发浓缩与LC-HRMS / MS结合用于超痕量筛选环境水样品中的有机微量污染物

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摘要

Vacuum-assisted evaporative concentration (VEC) was successfully applied and validated for the enrichment of 590 organic substances from river water and wastewater. Different volumes of water samples (6 mL wastewater influent, 15 mL wastewater effluent, and 60 mL river water) were evaporated to 0.3 mL and finally adjusted to 0.4 mL. 0.1 mL of the concentrate were injected into a polar reversed-phase C18 liquid chromatography column coupled with electrospray ionization to high-resolution tandem mass spectrometry. Analyte recoveries were determined for VEC and compared against a mixed-bed multilayer solid-phase extraction (SPE). Both approaches performed equally well (≥ 70% recovery) for a vast number of analytes (n = 327), whereas certain substances were especially amenable to enrichment by either SPE (e.g., 4-chlorobenzophenone, logDow,pH7 4) or VEC (e.g., TRIS, logDow,pH7 − 4.6). Overall, VEC was more suitable for the enrichment of polar analytes, albeit considerable signal suppression (up to 74% in river water) was observed for the VEC-enriched sample matrix. Nevertheless, VEC allowed for accurate and precise quantification down to the sub-nanogram per liter level and required no more than 60 mL of the sample, as demonstrated by its application to several environmental water matrices. By contrast, SPE is typically constrained by high sample volumes ranging from 100 mL (wastewater influent) to 1000 mL (river water). The developed VEC workflow not only requires low labor cost and minimum supervision but is also a rapid, convenient, and environmentally safe alternative to SPE and highly suitable for target and non-target analysis. Electronic supplementary materialThe online version of this article (10.1007/s00216-019-01696-3) contains supplementary material, which is available to authorized users.
机译:成功地使用了真空辅助蒸发浓缩(VEC)并对其进行了验证,以从河水和废水中富集590种有机物质。将不同体积的水样本(6 mL废水进水,15 mL废水出水和60 mL河水)蒸发至0.3 mL,最后调节至0.4 mL。将0.1 mL浓缩液注入极性反相C18液相色谱柱中,并与电喷雾电离耦合至高分辨率串联质谱。确定了VEC的分析物回收率,并将其与混合床多层固相萃取(SPE)进行了比较。两种方法对大量分析物(n = 327)的性能均相同(≥70%回收率),而某些物质尤其适合通过SPE(例如4-氯二苯甲酮,logDow,pH7 4)或VEC(例如,TRIS,logDow,pH7 -4.6)。总体而言,VEC更适合于极性分析物的富集,尽管对富含VEC的样品基质观察到了相当大的信号抑制(在河水中高达74%)。尽管如此,VEC仍可以精确,精确地定量至每升亚纳克级以下的水平,并且所需要的样品量不超过60 mL,这已将其应用于多种环境水基质中。相比之下,SPE通常受限于从100毫升(废水流入)到1000毫升(河流水)的大量样品。发达的VEC工作流程不仅需要较低的劳动力成本和最少的监督,而且是SPE的快速,便捷和环境安全的替代方案,非常适合目标和非目标分析。电子补充材料本文的在线版本(10.1007 / s00216-019-01696-3)包含补充材料,授权用户可以使用。

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