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基于静电纺丝的新型吸附剂用于电辅助固相微萃取六种非甾体抗炎药,然后用人血浆样品的 HPLC-UV 定量分析。

A novel sorbent based on electrospun for electrically-assisted solid phase microextraction of six non-steroid anti-inflammatory drugs, followed by quantitation with HPLC-UV in human plasma samples.

机构信息

Department of Analytical Chemistry and Pollutants, Faculty of Chemistry and Petroleum Sciences, Shahid Beheshti University, Tehran, Iran.

出版信息

Anal Chim Acta. 2024 Jan 25;1287:341839. doi: 10.1016/j.aca.2023.341839. Epub 2023 Sep 26.

Abstract

BACKGROUND

Although NSAIDs possess notable therapeutic and pharmaceutical qualities, it's essential to acknowledge that excessive doses can result in toxicity within the human body. Moreover, the importance lies in identifying and measuring their trace amounts. Due to their existence within intricate matrices, the creation of novel electrospun nanofibers as sorbents for electrically-assisted solidphase microextraction (EA-SPME) becomes vital. This innovation caters to the requirement for the effective pre-treatment of NSAID samples, providing a strategic approach to managing the complexities associated with trace quantities found in various matrices.

RESULTS

First, polyvinylalcohol/casein/tannic acid/polyaniline/titanium dioxide nanoparticles (PVA/CAS/TA/PANI/TiO NPs) electrospun nanofibers were prepared for EA-SPME on pewter rode and then, trace amounts of six NSAIDs (Acetaminophen, Caffeine, Naproxen, Celecoxib, Ibuprofen and mefenamic acid) were adsorbed chemically on these nanofibers. In the next step, the desorption of six NSAIDs was electrochemically done from prepared electrospun nanofibers on a pewter rod which was as working electrode at three electrodes system. Finally, these drugs were quantified from different human plasma samples with HPLC-UV. The synthesis of electrospun nanofibers was confirmed through a series of analytical techniques including field emission-scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy with elemental mapping analysis (EDX-Mapping), X-ray diffraction (XRD), and Fourier transform-infrared (FT-IR). The optimal percentage of additive compounds to PVA/CAS for electrospinning, as well as the factors influencing adsorption and desorption processes, were determined through both of Design Expert software and MATLAB programming language.

SIGNIFICANCE

Under optimum conditions, the wide linear range was 27-8000 ng mL with R≥ 0.9897, low detection limits were ranged from 8 to 27.3 ng mL based on S/N = 3 and significant enrichment factors were acquired. The intra-day and inter-day RSDs% were obtained within the 4.51% - 5.68% and 4.28%-5.45%, respectively. Finally, The effectiveness of the EA-SPME-HPLC-UV method was assessed for determining NSAIDs in plasma samples, demonstrating good recoveries ranging from 90.2% to 105.2%.

摘要

背景

尽管非甾体抗炎药(NSAIDs)具有显著的治疗和药物特性,但必须认识到,过量使用会导致人体毒性。此外,重要的是要识别和测量它们的痕量。由于它们存在于复杂的基质中,因此作为电辅助固相微萃取(EA-SPME)的吸附剂,新型的聚偏二氟乙烯/酪蛋白/单宁酸/聚苯胺/二氧化钛纳米纤维的制备变得至关重要。这一创新满足了有效预处理 NSAID 样品的要求,为管理各种基质中痕量物质的复杂性提供了一种策略方法。

结果

首先,在 pewter rode 上制备了聚(乙烯醇)/酪蛋白/单宁酸/聚苯胺/二氧化钛纳米粒子(PVA/CAS/TA/PANI/TiO NPs)电纺纳米纤维,然后通过化学吸附在这些纳米纤维上吸附痕量的六种 NSAIDs(对乙酰氨基酚、咖啡因、萘普生、塞来昔布、布洛芬和甲芬那酸)。下一步,在三电极系统中,将 pewter rode 上制备的电纺纳米纤维上的六种 NSAIDs 通过电化学解吸。最后,用高效液相色谱-紫外(HPLC-UV)法从不同的人血浆样品中定量这些药物。通过一系列分析技术,包括场发射扫描电子显微镜(FE-SEM)、能量色散 X 射线光谱与元素映射分析(EDX-Mapping)、X 射线衍射(XRD)和傅里叶变换红外(FT-IR),证实了电纺纳米纤维的合成。通过 Design Expert 软件和 MATLAB 编程语言,确定了电纺时添加化合物与 PVA/CAS 的最佳比例以及影响吸附和解吸过程的因素。

意义

在最佳条件下,宽线性范围为 27-8000ng mL,R≥0.9897,检测限范围为 8-27.3ng mL,基于 S/N=3,获得了显著的富集因子。日内和日间 RSD%分别为 4.51%-5.68%和 4.28%-5.45%。最后,通过测定血浆样品中的 NSAIDs,评估了 EA-SPME-HPLC-UV 方法的有效性,证明回收率良好,范围为 90.2%-105.2%。

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