Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, P.O. Box 53714-161, Tabriz, Iran.
Molecular Science and Engineering Research Group (MSERG), Azarbaijan Shahid Madani University, P.O. Box 53714-161, Tabriz, Iran.
Anal Methods. 2024 Aug 22;16(33):5710-5722. doi: 10.1039/d4ay00784k.
In the current study, nickel oxide nanoparticles (NiO NPs) modified with dimethylglyoxime (DMG) were deposited onto the cellulose surface (Ni(DMG)-NiO-Cell) and used as an efficient adsorbent for thin film microextraction (TFME) of tramadol (TRA). The extracted TRA was determined using a high-performance liquid chromatography-ultraviolet detector (HPLC-UV). NiO NPs were synthesized by co-precipitation method on the surface of the cellulose substrate; afterward, its surface was modified by DMG to increase the extraction capability of the thin film toward TRA. The synthesized NiO-Cell and Ni(DMG)-NiO-Cell thin films were characterized using various techniques. The effect of modification of the NiO thin film with DMG reagent on the extraction efficiency was investigated. The crucial parameters influencing the extraction efficiency, including extraction time, desorption time, desorption solvent, pH and salt content, were investigated a one-at-a-time approach. The figures of merit for the developed method were evaluated in urine, plasma, and deionized water under the optimized extraction and desorption condition. The limits of detection and limits of quantification were in the range of 0.1 to 1 ng mL and 0.3 to 3 ng mL, respectively, for the studied samples. The linear dynamic ranges of the developed TFME-HPLC-UV method were 0.3-1000, 1-2500, and 3-5000 ng mL for the deionized water, urine, and plasma samples, respectively. The reproducibility and repeatability of the developed method was assayed in terms of intra-day, inter-day, and inter-thin film precisions by conducting six-replicate experiments at the concentration level of 0.1 and 1 μg mL, which were in the range of 5.9% to 8.3%. The sufficiency and applicability of the developed TFME-HPLC-UV method was investigated by determining TRA in urine and plasma samples, and the resulting relative recoveries (RR%) were 85.9% and 91.7%, respectively.
在本研究中，用二甲基乙二肟（DMG）修饰的氧化镍纳米粒子（NiO NPs）被沉积在纤维素表面上（Ni(DMG)-NiO-Cell），并用作曲马多（TRA）的薄膜微萃取（TFME）的有效吸附剂。提取的 TRA 使用高效液相色谱-紫外检测器（HPLC-UV）进行测定。通过共沉淀法在纤维素基质表面合成 NiO NPs；之后，用 DMG 对其表面进行修饰，以提高薄膜对 TRA 的萃取能力。合成的 NiO-Cell 和 Ni(DMG)-NiO-Cell 薄膜使用各种技术进行了表征。研究了 DMG 试剂修饰 NiO 薄膜对萃取效率的影响。通过逐一改变的方法研究了影响萃取效率的关键参数，包括萃取时间、解吸时间、解吸溶剂、pH 值和盐含量。在优化的萃取和解吸条件下，在尿液、血浆和去离子水中评估了所开发方法的优点。对于所研究的样品，检测限和定量限分别在 0.1 至 1ng/mL 和 0.3 至 3ng/mL 的范围内。开发的 TFME-HPLC-UV 方法的线性动态范围为去离子水、尿液和血浆样品的 0.3-1000、1-2500 和 3-5000ng/mL。通过在 0.1 和 1μg/mL 浓度水平上进行六次重复实验，以日内、日间和薄膜间精密度来测定开发方法的重现性和重复性，其范围在 5.9%至 8.3%之间。通过测定尿液和血浆样品中的 TRA，研究了开发的 TFME-HPLC-UV 方法的充分性和适用性，得到的相对回收率（RR%）分别为 85.9%和 91.7%。
