Department of Chemistry, Institute of Physical and Theoretical Chemistry, Eberhard Karls Universität Tübingen, Tübingen, Germany.
Anal Bioanal Chem. 2024 Nov;416(28):6387-6403. doi: 10.1007/s00216-024-05525-0. Epub 2024 Sep 18.
The efficient extraction of various analytes from a wide spectrum of matrices with organic solvents is still a great challenge in analytical chemistry. Especially polar and charged compounds are hard to extract in combination with neutral analytes of intermediate to low polarity. The QuEChERS method is often chosen and has been adapted not only to the analysis of food samples, but also to environmental matrices (soil, wastewater) or biota. In this study, we overcome major drawbacks of QuEChERS such as low recoveries of charged analytes and impairment of downstream analysis by high salt loads. The new extraction method, applicable to liquid and solid samples, is called SWIEET (sugar water isopropanol ethyl nitrile extraction technique). Phase separation of the otherwise miscible extraction solvents water and acetonitrile is achieved by sugaring-out instead of salting-out. Extraction efficiencies were greatly improved by adding isopropanol to the acetonitrile phase. The concentrations of the additives glucose and isopropanol, as well as temperature, were optimized by a design of experiment. Further improvement was achieved through electro- or double-extractions. For all sample types tested (surface water, wastewater treatment plant effluent, tomato, soil, and oats), recoveries and precision were higher with SWIEET than with the established QuEChERS method. From wastewater treatment plant effluent, 75% recovery on average were achieved with our SWIEET method compared to 37% with QuEChERS for a model analyte mixture with polarities of logD = - 5.7 - 3.5. Higher recoveries and lower standard deviations compared to QuEChERS were achieved especially for polar and charged analytes such as metformin. Handling proved to be easy, since there was no additional solid phase and no tedious weighing of salts.
从广泛的基质中用有机溶剂高效提取各种分析物仍然是分析化学中的一个巨大挑战。特别是带电荷和极性化合物与中等到低极性的中性分析物结合时很难提取。QuEChERS 方法经常被选择,并不仅适用于食品样品的分析,还适用于环境基质(土壤、废水)或生物群。在本研究中,我们克服了 QuEChERS 的主要缺点,例如带电荷分析物的回收率低以及高盐负荷对下游分析的影响。这种新的提取方法适用于液体和固体样品,称为 SWIEET(糖水异丙醇乙腈提取技术)。通过加糖而不是加盐来实现原本可混溶的提取溶剂水和乙腈的相分离。通过向乙腈相中添加异丙醇,大大提高了萃取效率。通过实验设计优化了添加剂葡萄糖和异丙醇的浓度以及温度。通过电萃取或双萃取进一步提高了效率。对于所有测试的样品类型(地表水、污水处理厂出水、番茄、土壤和燕麦),SWIEET 的回收率和精密度都高于已建立的 QuEChERS 方法。与 QuEChERS 相比,我们的 SWIEET 方法从污水处理厂出水中获得的模型分析物混合物的极性为 logD=-5.7-3.5 的平均回收率为 75%,而 QuEChERS 方法的回收率为 37%。与 QuEChERS 相比,SWIEET 尤其对极性和带电荷的分析物(如二甲双胍)的回收率更高,标准偏差更低。处理证明很容易,因为没有额外的固相,也没有繁琐的盐称重。