Departamento de Química Analítica, Instituto Universitario de Investigación en Química Fina y Nanoquímica IUNAN, Universidad de Córdoba, Campus de Rabanales, Edificio Marie Curie (anexo), E-14071, Córdoba, Spain; Department of Analytical Chemistry, University of Valencia, 46100, Burjassot, Valencia, Spain.
Department of Analytical Chemistry, University of Valencia, 46100, Burjassot, Valencia, Spain.
Anal Chim Acta. 2021 Jun 15;1164:338512. doi: 10.1016/j.aca.2021.338512. Epub 2021 Apr 19.
The development of analytical methods that allow the simultaneous determination of a wide range of analytes with different properties is one of the focuses of attention in Analytical Chemistry. This work describes a proof-of-concept of the synergistic extraction of a planar paper-based sorptive phase modified with a polyamide such as nylon. This as-prepared sorptive phase enables the extraction of six penicillin-derived antibiotics of different polarity from human saliva samples in the same analysis, since the analytes either interact with the paper or with the nylon. The synthesis of the sorptive phase is simple as it only requires dipping the paper into an organic solution of the polymer (i.e., nylon in formic acid). Then, the modified paper-based sorptive phase is introduced in an Eppendorf tube to perform the extraction of the analytes, and subsequent desorption and measurement by liquid chromatography-tandem mass spectrometry. Under the optimized extraction conditions, the method enables the determination of the analytes in saliva samples with limits of detection from 2.4 to 3.7 ng mL. Relative standard deviation (RSD) below 10% for all the target analytes and relative recoveries between 84 and 123% were achieved by using matrix-matched calibration. The results confirm the versatility and the synergistic extraction of the polyamide-coated paper-based sorptive phase, and its potential to be applied in bioanalysis. Moreover, the easy synthesis of the sorptive phase and the low cost of its preparation, as well as the high sample throughput analysis, are some of the main features of the proposed method.
开发能够同时测定具有不同性质的多种分析物的分析方法是分析化学关注的焦点之一。本工作描述了协同提取经聚酰胺(如尼龙)修饰的平面纸基固相萃取剂的概念验证。这种制备的固相萃取剂能够从人唾液样品中同时提取六种不同极性的青霉素衍生抗生素,因为分析物与纸或尼龙相互作用。由于固相萃取剂的合成非常简单,只需将纸浸入聚合物(例如,在甲酸中的尼龙)的有机溶液中即可。然后,将改性的纸基固相萃取剂引入到 Eppendorf 管中以提取分析物,然后通过液相色谱-串联质谱法进行洗脱和测量。在优化的提取条件下,该方法能够以 2.4 至 3.7ng/mL 的检测限测定唾液样品中的分析物。通过使用基质匹配校准,所有目标分析物的相对标准偏差(RSD)均低于 10%,相对回收率在 84%至 123%之间。结果证实了涂有聚酰胺的纸基固相萃取剂的多功能性和协同提取能力,以及其在生物分析中的应用潜力。此外,该方法易于合成固相萃取剂且制备成本低,以及具有高样品通量分析等特点。