Köke Niklas, Zahn Daniel, Knepper Thomas P, Frömel Tobias
Hochschule Fresenius, University of Applied Sciences, Limburger Straße 2, 65510, Idstein, Germany.
Anal Bioanal Chem. 2018 Mar;410(9):2403-2411. doi: 10.1007/s00216-018-0921-1. Epub 2018 Feb 12.
Analysis of polar organic chemicals in the aquatic environment is exacerbated by the lack of suitable and widely applicable enrichment methods. In this work, we assessed the suitability of a novel combination of well-known solid-phase extraction (SPE) materials in one cartridge as well as an evaporation method and for the enrichment of 26 polar model substances (predominantly log D < 0) covering a broad range of physico-chemical properties in three different aqueous matrices. The multi-layer solid-phase extraction (mlSPE) and evaporation method were investigated for the recovery and matrix effects of the model substances and analyzed with hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). In total, 65% of the model substances were amenable (> 10% recovery) to the mlSPE method with a mean recovery of 76% while 73% of the model substances were enriched with the evaporation method achieving a mean recovery of 78%. Target and non-target screening comparison of both methods with a frequently used reversed-phase SPE method utilizing "hydrophilic and lipophilic balanced" (HLB) material was performed. Target analysis showed that the mlSPE and evaporation method have pronounced advantages over the HLB method since the HLB material retained only 30% of the model substances. Non-target screening of a ground water sample with the investigated enrichment methods showed that the median retention time of all detected features on a HILIC system decreased in the order mlSPE (3641 features, median t 9.7 min), evaporation (1391, 9.3 min), HLB (4414, 7.2 min), indicating a higher potential of the described methods to enrich polar analytes from water compared with HLB-SPE. Graphical abstract Schematic of the method evaluation (recovery and matrix effects) and method comparison (target and non-target analysis) of the two investigated enrichment methods for very polar chemicals in aqueousmatrices.
缺乏合适且广泛适用的富集方法加剧了对水环境中极性有机化合物的分析难度。在本研究中，我们评估了一种新型组合方法的适用性，即将多种知名的固相萃取（SPE）材料置于一个萃取柱中，再结合蒸发法，用于富集26种极性模型物质（主要log D < 0），这些物质涵盖了三种不同水性基质中广泛的物理化学性质。研究了多层固相萃取（mlSPE）和蒸发法对模型物质的回收率和基质效应，并采用亲水作用液相色谱 - 串联质谱（HILIC - MS/MS）进行分析。总体而言，65%的模型物质适用于mlSPE方法（回收率>10%），平均回收率为76%，而73%的模型物质可通过蒸发法富集，平均回收率为78%。将这两种方法与常用的使用“亲水亲脂平衡”（HLB）材料的反相SPE方法进行了目标和非目标筛选比较。目标分析表明，mlSPE和蒸发法相对于HLB方法具有显著优势，因为HLB材料仅保留了30%的模型物质。用所研究的富集方法对一个地下水样品进行非目标筛选表明，在HILIC系统上所有检测到的特征的中位保留时间按以下顺序降低：mlSPE（3641个特征，中位t 9.7分钟）、蒸发法（1391个，9.3分钟）、HLB（4414个，7.2分钟），这表明与HLB - SPE相比，所述方法从水中富集极性分析物的潜力更高。图摘要 水性基质中两种研究的极极性化学品富集方法的方法评估（回收率和基质效应）及方法比较（目标和非目标分析）示意图
