Tailoring a MOF-on-MOF (ZIF-8-on-NH2-MIL-53(Al)) Hybrid Composite for Micro Solid Phase Extraction of Furosemide in artificial biological fluids prior to LC-q-TOF/MS detection

IF 6.5 Q1 CHEMISTRY, ANALYTICAL

Advances in Sample Preparation Pub Date : 2025-02-01 DOI:10.1016/j.sampre.2025.100157

Zinar Pinar Gumus , Mustafa Soylak

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Abstract

Furosemide, a powerful diuretic that increases urine excretion, is used to treat many diseases. However, due to its abuse in sport, it is considered a doping substance. As a result, it has been banned by the World Anti-Doping Agency (WADA) and included in the group of diuretics and masking agents. Given the clinical significance of furosemide and its dependable application in athletics, this research employed the "MOF-on-MOF" hybrid material composite to leverage the synergistic effects of various components for detecting this drug in biological samples. After characterization of the ZIF-8-on-NH₂-MIL-53(Al) composite by FT-IR, XRD, TGA, XPS, BET and SEM-EDX techniques, the µ-SPE procedure was optimized using liquid chromatography-time of flight mass spectrometry (LC-q-TOF/MS) based on the recovery values. The optimum conditions were determined as pH 6, adsorbent amount of 20 mg, and total adsorption-desorption time of 7 min. The recovery values of the solid-phase extraction method for simulated body fluids samples under optimum conditions were between 77.5 % and 93.4 %. The µ-SPE technique was effectively utilized on physiological samples using the ZIF-8-on-NH₂-MIL-53(Al) composite under optimal conditions. This study's findings will inform future research into the design of 'MOF-on-MOF' hybrids for various applications.

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定制MOF-on-MOF （ZIF-8-on-NH2-MIL-53(Al)）混合复合材料，用于LC-q-TOF/MS检测前人工生物液中速尿的微固相萃取

速尿是一种强大的利尿剂，可以增加尿液的排出，被用来治疗许多疾病。然而，由于其在体育运动中的滥用，它被认为是一种兴奋剂物质。因此，它已被世界反兴奋剂机构（WADA）禁用，并被列入利尿剂和掩蔽剂组。鉴于呋塞米的临床意义及其在体育运动中的可靠应用，本研究采用“MOF-on-MOF”混合材料复合材料，利用各组分的协同作用在生物样品中检测呋塞米。利用FT-IR、XRD、TGA、XPS、BET和SEM-EDX等技术对ZIF-8-on-NH2-MIL-53（Al）复合材料进行表征后，利用液相色谱-飞行时间质谱（LC-q-TOF/MS）对其回收率进行优化。最佳条件为pH 6、吸附剂用量20 mg、总吸附-解吸时间7 min。在最佳条件下，固相萃取法对模拟体液样品的回收率为77.5% ~ 93.4%。在最佳条件下，利用ZIF-8-on-NH2-MIL-53（Al）复合材料对生理样品进行了微固相萃取。这项研究的发现将为未来设计各种应用的“MOF-on-MOF”混合材料的研究提供信息。

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来源期刊

Advances in Sample Preparation

CiteScore

3.50

自引率

0.00%

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