比较使用基于 MOFs(MIL-53(Al) 和 ZIF-8)的 D-µ-SPE 与 HPLC-UV 联用从人体血浆中提取睾酮的方法

IF 1.2 4区 化学 Q4 BIOCHEMICAL RESEARCH METHODS Chromatographia Pub Date : 2024-04-22 DOI:10.1007/s10337-024-04329-9
Somaye Akbari, Azra Takhvar, Effat Souri, Reza Ahmadkhaniha, Ali Morsali, Mohammad Reza Khoshayand, Mohsen Amini, Alireza Taheri
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引用次数: 0

摘要

利用金属有机框架(MOFs),即 MIL-53(Al)和 ZIF-8,开发了一种新技术,通过分散微固相萃取(D-µ-SPE 或 DMSPE)从人体血浆中提取睾酮。通过傅立叶变换红外光谱(FT-IR)、粉末 X 射线衍射(PXRD)和扫描电子显微镜(SEM)对合成的 MOFs 进行了表征。采用响应面法(RSM)对影响萃取的参数进行了优化。最佳萃取条件被确定为:接触时间为 15 分钟,MIL-53(Al) 用量为 1 毫克,NaCl 浓度为 0.23% (w/v)。对于 ZIF-8,接触时间为 22 分钟,吸附剂用量为 5.4 毫克,盐浓度为 0.34%(w/v)。为了找到合适的动力学和等温线模型,进行了批量吸收研究。结果表明,虽然两种情况都有利于睾酮的吸收,但 MIL-53 (Al) 的吸收能力高于 ZIF-8。最后,对所提出的方法进行了分析验证,以测定血浆样品中的睾酮。该方法的分析性能良好,每种吸附剂的动态范围均为 0.05-1 µg/mL。该方法对睾酮和MIL-53(Al)的精密度(以相对标准偏差(RSD)表示)和准确度(以误差百分比表示)分别为3.40%和2.79%,对睾酮和ZIF-8的精密度和准确度分别为4.24%和4.22%。使用 MIL-53(Al) 和 ZIF-8 方法从血浆样品中分别有效提取了 97% 和 96% 的睾酮。
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Comparison of Testosterone Extraction from Human Plasma Using MOFs (MIL-53(Al) and ZIF-8)-Based D-µ-SPE Coupled to HPLC–UV

A novel technique utilizing metal–organic frameworks (MOFs), namely MIL-53(Al) and ZIF-8, has been developed for the extraction of testosterone from human plasma through dispersive micro-solid phase extraction (D-µ-SPE or DMSPE). The synthesized MOFs were subjected to characterization via Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (PXRD), and scanning electron microscopy (SEM). The parameters affecting the extraction were optimized by response surface methodology (RSM). The optimal extraction conditions were determined to be 15 min for contact time, 1 mg for MIL-53(Al) amount, and 0.23% (w/v) for NaCl concentration. For ZIF-8, a contact time of 22 min, a sorbent amount of 5.4 mg, and a salt concentration of 0.34% (w/v) were obtained. Batch absorption studies were conducted to find appropriate kinetic and isotherm models. The results indicated that while testosterone absorption was favorable in both cases, MIL-53 (Al) had a higher absorption capacity than ZIF-8. Finally, the proposed method was subjected to analytical validation for determination of testosterone in plasma samples. Good analytical performance was achieved, including a dynamic range of 0.05–1 µg/mL using each of the sorbents. The precision (expressed as the relative standard deviation (RSD)) and accuracy (expressed as the percentage error) of the method for testosterone and MIL-53(Al) were found to be 3.40% and 2.79%, respectively, while for testosterone and ZIF-8, they were 4.24% and 4.22%, respectively. The method effectively extracted 97% and 96% of testosterone from spiked plasma samples using MIL-53(Al) and ZIF-8, respectively.

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来源期刊
Chromatographia
Chromatographia 化学-分析化学
CiteScore
3.40
自引率
5.90%
发文量
103
审稿时长
2.2 months
期刊介绍: Separation sciences, in all their various forms such as chromatography, field-flow fractionation, and electrophoresis, provide some of the most powerful techniques in analytical chemistry and are applied within a number of important application areas, including archaeology, biotechnology, clinical, environmental, food, medical, petroleum, pharmaceutical, polymer and biopolymer research. Beyond serving analytical purposes, separation techniques are also used for preparative and process-scale applications. The scope and power of separation sciences is significantly extended by combination with spectroscopic detection methods (e.g., laser-based approaches, nuclear-magnetic resonance, Raman, chemiluminescence) and particularly, mass spectrometry, to create hyphenated techniques. In addition to exciting new developments in chromatography, such as ultra high-pressure systems, multidimensional separations, and high-temperature approaches, there have also been great advances in hybrid methods combining chromatography and electro-based separations, especially on the micro- and nanoscale. Integrated biological procedures (e.g., enzymatic, immunological, receptor-based assays) can also be part of the overall analytical process.
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