Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, Dr Moliner 50, 46100, Burjassot, Valencia, Spain.
Department of Analytical Chemistry, Faculty of Chemistry, University of Valencia, Dr Moliner 50, 46100, Burjassot, Valencia, Spain.
Talanta. 2020 Mar 1;209:120566. doi: 10.1016/j.talanta.2019.120566. Epub 2019 Nov 15.
In this work, a simple device for extraction glutathione (GSH) in biological fluids using a hybrid monolithic material within a polypropylene syringe is developed. For this purpose, glycidyl methacrylate-based monolith was firstly prepared within this housing material, and the polymer was modified with different ligands (ammonia, cysteamine and cystamine). The resulting materials (containing amine or thiol groups, respectively) were then functionalized with gold nanoparticles (AuNPs). The hybrid material that gave the largest AuNPs coverage was selected as solid-phase (SPE) sorbent and several variables affecting the extraction recovery of this compound were investigated. Under optimal conditions, GSH was quantitatively retained at pH 6.0, and then it was desorbed with aqueous dithiothreitol solution and determined, after derivatization with o-phthaldialdehyde, via reversed-phase LC with fluorometric detection. The limit of detection was ca. 1.5 ng mL, and the reproducibility between extraction units was below 8% (expressed as relative standard deviation), which demonstrates the robustness of the method. The developed material was also applied for the extraction of GSH in saliva and urine samples yielding recoveries ranging from 86 to 105%.
在这项工作中，开发了一种简单的装置，用于在聚丙烯注射器内的混合整体材料中提取生物流体中的谷胱甘肽 (GSH)。为此，首先在这种外壳材料内制备基于甲基丙烯酰氧乙基的整体材料，然后用不同的配体（氨、半胱氨酸和胱胺）对聚合物进行修饰。然后，将所得材料（分别含有胺或巯基）用金纳米粒子（AuNPs）进行功能化。选择对 AuNPs 覆盖率最大的混合材料作为固相（SPE）吸附剂，并研究了影响该化合物萃取回收率的几个变量。在最佳条件下，GSH 在 pH 6.0 下被定量保留，然后用含二硫苏糖醇的水溶液解吸，并在反相 LC 中用荧光检测进行衍生化后测定。检测限约为 1.5ng/mL，萃取单元之间的重现性低于 8%（表示为相对标准偏差），这证明了该方法的稳健性。所开发的材料还应用于唾液和尿液样品中 GSH 的提取，回收率范围为 86%至 105%。
