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Biocompatible magnetite nanoparticles coated with ionic liquid-based surfactant as a hydrophilic sorbent for dispersive solid phase microextraction of cephalosporins prior to their quantitation by HPTLC
Journal of Chromatography B ( IF 3 ) Pub Date : 2022-06-13 , DOI: 10.1016/j.jchromb.2022.123339
Sherien A Farrag 1 , Azza H Rageh 2 , Hassan F Askal 2 , Gamal A Saleh 3
Affiliation  

Extraction of highly hydrophilic compounds from biological fluids including urine or plasma samples is a dilemma due to high hydrophilicity of the matrix itself. The main aim of the current work is to explore the competence of ionic liquid (IL)-based surfactant-coated mineral oxide nanoparticles (NPs) in dispersive solid-phase microextraction (d-SPME) of highly hydrophilic analytes taking cefoperazone (CPZ) as a model analyte for the study. The IL-based surfactant coated Fe3O4 NPs is utilized as an innovative adsorbent for the separation and pre-concentration of CPZ after intramuscular injection (I.M) in rabbits. The utilized magnetite NPs were synthesized via simple and reliable co-precipitation procedure, which doesn’t require any air-free environment and depends on a single iron (III) salt. Characterization of the as-synthesized NPs was achieved by X-ray powder diffraction (XRD), Fourier transform infrared (FT-IR) and energy dispersive X-ray (EDX). Surface area measurements show that Fe3O4 NPs have large surface area of 75 m2 g−1. The developed approach utilizes the unique properties of the IL-based surfactant including multiple polar interaction types provided by the polar head in addition to merits of Fe3O4 nanoparticles, which include large adsorptive capacity and magnetic properties, to improve separation, save time, and achieve satisfactory recovery. Comprehensive study was developed for the factors, that affect the adsorption capacity such as pH, NPs amount, IL-based surfactant concentration, ionic strength, adsorption time, and desorption conditions. Moreover, the adsorption data was fitted to Langmuir and second-order kinetic models as reflected by the reasonable determination coefficients of 0.9319 and 0.9726, respectively. Under the optimized conditions, the developed approach achieves good correlation coefficient of 0.9975, and 0.9981 over linearity range of 0.7–12.0 and 4.0–50.0 µg mL−1 for both CPZ standard solutions and spiked rabbit plasma, respectively. It also provides good sensitivity expressed by the low values of limit of detection (LOD) of 0.2 and 1.2 µg mL−1 and limit of quantitation (LOQ) of 0.7 and 4.0 µg mL−1 for both the standard solutions and spiked plasma, respectively. The developed approach was also applied successfully for monitoring CPZ in rabbit plasma samples with satisfactory recovery % (83–110). In addition, a detailed pharmacokinetic study is performed where pharmacokinetic parameters of CPZ in rabbit plasma samples were calculated.



中文翻译:

生物相容性磁铁矿纳米粒子涂有离子液体表面活性剂作为亲水性吸附剂,用于头孢菌素的分散固相微萃取,然后通过 HPTLC 对其进行定量

由于基质本身的高亲水性,从包括尿液或血浆样品在内的生物体液中提取高亲水性化合物是一个难题。目前工作的主要目的是探索基于离子液体(IL)的表面活性剂包覆的矿物氧化物纳米粒子(NPs)在以头孢哌酮(CPZ)作为高亲水性分析物的分散固相微萃取(d-SPME)中的能力。研究的模型分析物。基于IL的表面活性剂包覆Fe 3 O 4NPs 被用作一种创新的吸附剂,用于兔子肌肉注射 (IM) 后 CPZ 的分离和预浓缩。所利用的磁铁矿纳米粒子是通过简单可靠的共沉淀过程合成的,不需要任何无空气环境,并且依赖于单一的铁 (III) 盐。通过 X 射线粉末衍射 (XRD)、傅里叶变换红外 (FT-IR) 和能量色散 X 射线 (EDX) 对合成的纳米颗粒进行表征。表面积测量表明,Fe 3 O 4 NPs 具有 75 m 2 g -1的大表面积. 所开发的方法利用了基于 IL 的表面活性剂的独特性质,包括由极性头提供的多种极性相互作用类型以及 Fe 3 O 4的优点纳米粒子,包括大的吸附能力和磁性,以改善分离,节省时间,并获得令人满意的回收率。对影响吸附容量的因素进行了综合研究,如 pH 值、NPs 量、基于 IL 的表面活性剂浓度、离子强度、吸附时间和解吸条件。此外,吸附数据符合 Langmuir 和二级动力学模型,分别由 0.9319 和 0.9726 的合理确定系数所反映。在优化条件下,开发的方法在 0.7–12.0 和 4.0–50.0 µg mL -1的线性范围内实现了 0.9975 和 0.9981 的良好相关系数分别用于 CPZ 标准溶液和加标兔血浆。它还提供了良好的灵敏度,通过标准溶液和加标血浆的低检测限 (LOD) 0.2 和 1.2 µg mL -1和定量限 (LOQ) 分别为 0.7 和 4.0 µg mL -1表示. 所开发的方法也成功地应用于监测兔血浆样品中的 CPZ,并具有令人满意的回收率 (83-110)。此外,还进行了详细的药代动力学研究,计算了兔血浆样品中 CPZ 的药代动力学参数。

更新日期:2022-06-13
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