School of Materials and Chemical Engineering, Ningbo University of Technology, Ningbo 315211, China; Fenghua Institute, Ningbo University of Technology, Ningbo 315500, China.
J Chromatogr A. 2018 Dec 21;1581-1582:16-24. doi: 10.1016/j.chroma.2018.11.006. Epub 2018 Nov 3.
In this work, a novel polyethyleneimine-modified hybrid silica material was developed and utilized as a solid support for hydrophilic solid-phase extraction (HILIC SPE) of thyreostats in animal tissue samples. The effects of critical parameters of extraction, including acetonitrile content, pH, sample loading volume, elution volume, sample loading flow rate and elution flow rate were completely optimized. It was found that the polyethyleneimine-modified hybrid silica sorbent displayed a high adsorption capacity of 15.8 mg/g, and the breakthrough volume was up to 40 mL. The proposed HILIC SPE method provided low detection limits of 0.5-2.2 μg/kg, and excellent recoveries of 93.4-103.1% with relative standard deviations of 3.6-9.6% (n = 3). Importantly, compared with the traditional clean-up methods for determination of thyreostats in complex matrices, the developed HILIC SPE method eliminated drying and redissolving steps. In the further, the proposed HILIC SPE method is expected to be widely applied for the clean-up of small polar and hydrophilic compounds in complex matrices.
在这项工作中，开发了一种新型的聚乙烯亚胺改性杂化硅胶材料，并将其用作动物组织样品中甲状腺抑制剂的亲水固相萃取（HILIC SPE）的固体支撑物。完全优化了萃取的关键参数，包括乙腈含量、pH 值、样品加载体积、洗脱体积、样品加载流速和洗脱流速。结果发现，聚乙烯亚胺改性杂化硅胶吸附剂具有高达 15.8mg/g 的高吸附容量，并且突破体积高达 40mL。所提出的 HILIC SPE 方法提供了低至 0.5-2.2μg/kg 的检测限，以及 93.4-103.1%的优异回收率，相对标准偏差为 3.6-9.6%（n=3）。重要的是，与用于复杂基质中甲状腺抑制剂测定的传统净化方法相比，所开发的 HILIC SPE 方法消除了干燥和重新溶解步骤。在进一步，所提出的 HILIC SPE 方法有望广泛应用于复杂基质中小极性和亲水化合物的净化。
