School of Chemistry, College of Science, University of Tehran, P.O. Box 14155-6455, Tehran, Iran.
Nanomaterial, Separation and Trace Analysis Research Lab, K.N, Toosi University of Technology, P.O. Box 16315-1618, Tehran, 15418-49611, Iran.
Mikrochim Acta. 2024 Sep 7;191(10):581. doi: 10.1007/s00604-024-06650-4.
To meet the needs of developing efficient extractive materials alongside the evolution of miniaturized sorbent-based sample preparation techniques, a mesoporous structure of g-CN doped with sulfur as a heteroatom was achieved utilizing a bubble template approach while avoiding the severe conditions of other methods. In an effort to increase the number of adsorption sites, the resultant exfoliated structure was then modified with thymol-coumarin NADES as a natural sorbent modifier, followed by introduction into a nylon 6 polymer via an electrospinning process. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, field-emission scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and Brunauer-Emmett-Teller (BET) surface area analysis validated S-doped g-CN and composite production. The prepared electrospun fiber nanocomposite, entailing satisfactory processability, was then successfully utilized as a sorbent in on-chip thin film micro-solid-phase extraction of non-steroidal anti-inflammatory drugs (NSAIDs) from saliva samples prior to liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. Utilizing a chip device, a thin film μ-SPE coupled with LC-MS/MS analysis yielded promising outcomes with reduced sample solution and organic solvents while extending lifetime of a thin film sorbent. The DES-modified S-doped g-CN amount in electrospun was optimized, along with adsorption and desorption variables. Under optimal conditions, selected NSAIDs were found to have a linear range of 0.05-100.0 ng mL with an R ≥ 0.997. The detection limits were ranged between 0.02 and 0.2 ng mL. The intra-day and inter-day precisions obtained were less than 6.0%. Relative recoveries were between 93.3 and 111.4%.
为了满足高效萃取材料的发展需求，同时结合基于小型化吸附剂的样品制备技术的发展，利用气泡模板法实现了掺杂硫杂原子的介孔 g-CN 结构，同时避免了其他方法的苛刻条件。为了增加吸附位点的数量，然后用天然吸附剂修饰剂香豆素-薄荷醇 NADES 对所得剥离结构进行修饰，再通过静电纺丝工艺引入尼龙 6 聚合物中。X 射线衍射 (XRD)、傅里叶变换红外 (FT-IR) 光谱、场发射扫描电子显微镜 (SEM)、能谱 (EDS) 和 Brunauer-Emmett-Teller (BET) 表面积分析验证了 S 掺杂 g-CN 和复合材料的制备。制备的具有良好加工性能的静电纺纤维纳米复合材料，然后成功地用作芯片上薄膜微固相萃取的吸附剂，用于从唾液样品中提取非甾体抗炎药 (NSAIDs)，再进行液相色谱-串联质谱 (LC-MS/MS) 分析。利用芯片装置，薄膜 μ-SPE 与 LC-MS/MS 分析相结合，在减少样品溶液和有机溶剂用量的同时，延长了薄膜吸附剂的寿命，得到了有前景的结果。对静电纺丝中掺杂 S 的 g-CN 的 DES 修饰量以及吸附和解吸变量进行了优化。在最佳条件下，发现选定的 NSAIDs 在 0.05-100.0ngmL 范围内具有线性范围，R≥0.997。检测限在 0.02 和 0.2ngmL 之间。日内和日间精密度均小于 6.0%。相对回收率在 93.3%至 111.4%之间。
