RESUMO
Composite nanofibers, namely, polyvinyl alcohol (PVA), citric acid (CA), ß-cyclodextrin (ß-CD), and copper oxide nanoparticles (PVA/CA/ß-cyclodextrin/CuO NPs), were developed as a novel, green, and efficient adsorbent in the pipette tip-micro-solid-phase extraction method (PT-µSPE), for the simultaneous extraction of three antidepressants drugs namely imipramine (IMP), citalopram (CIT), and clozapine (CLZ) in biological fluids before quantification by gas chromatography (GC-FID). Based on the obtained results from field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction (XRD), the successful synthesis of composite nanofibers was approved. Due to the presence of ß-cyclodextrins and CuO NPs rich of functional groups on their surface, the nanofibers have high extraction efficiency. Under the optimal conditions, the linear range for imipramine, citalopram, and clozapine was 0.1 to 1000.0 ng mL-1 with a determination coefficient ≥ 0.99. The limits of detection (LODs) were in the range 0.03 to 0.15 ng mL-1. The relative standard deviation was 4.8 to 8.7% (within-day, n = 4) and 5.1 to 9.2% (between-day, n = 3) for 3 consecutive days. In addition, excellent clean-up was achieved which is a great advantage over other sample preparation methods. Finally, the ability of the developed method to extract the target analytes from the biological samples was evaluated.
Assuntos
Clozapina , Nanofibras , beta-Ciclodextrinas , Álcool de Polivinil , Nanofibras/química , Citalopram , Espectroscopia de Infravermelho com Transformada de Fourier , Imipramina , Cromatografia Gasosa , beta-Ciclodextrinas/química , AntidepressivosRESUMO
Today, the wide use of triazole fungicides due to environmental damage and its side effects has raised global concern. Hence, in this research, poly-vinyl alcohol/polyacrylic-acid/CoFe-PBA@GO electrospun nanofiber was synthesized and applied as effective, degradable, and novel adsorbent at pipette-tip microextraction (PT-µSPE) method for the rapid and concurrent extraction of five of triazole fungicides in fruit and vegetable samples prior to quantitative analysis by high-performance liquid chromatography-ultraviolet. The incorporation of CoFe-PBA@GO with superporous structure and abundant functional groups in a polymer medium improves the extraction efficiency of nanofibers due to hydrogen bonding and π-π interactions formed between analytes and synthesized nano-adsorbent. Various important elements that affect the extraction yield of the target analytes were optimized utilizing a time-variable approach. Under the optimum conditions, dynamic range was attained in the range of 0.3-900.0 ng/mL with correlation coefficients ≥ 0.999. The identification limit of the PT-µSPE-HPLC-UV method ranged from 0.1 to 0.3 ng/mL.
Assuntos
Fungicidas Industriais , Nanofibras , Cromatografia Líquida de Alta Pressão , Nanofibras/química , Triazóis/análise , Fungicidas Industriais/análise , Polímeros/análise , Extração em Fase Sólida/métodos , Limite de DetecçãoRESUMO
Today, the wide utilization of triazole fungicides due to environmental damage and its side effects has raised global concern. Thus, in this investigation, polyacrylonitrile/MnCo-layered double hydroxides nanofiber was synthesized and applied as an effective and novel adsorbent at thin-film solid-phase micro-extraction technique for the quick and concurrent extraction of five triazole fungicides in fruit and vegetable samples before quantitative analysis by high-performance liquid chromatography-ultraviolet. The incorporation of MnCo-layered double hydroxides with porous structure and abundant functional groups in a polymer medium improves the extraction efficiency of nanofibers owing to hydrogen bonding and π-π interactions formed between analytes and synthesized nano-adsorbent. Various important elements that affect the extraction efficiency of the intended analytes were optimized using a time-variable approach. Under the optimum conditions, the limit of detection and quantification range from 0.1 to 0.15 and 0.3-0.5 ng mL-1, respectively.
RESUMO
Today, antidepressants are widely used and it is important to determine their trace amounts due to harmful consequences. Here, a new nano sorbent was reported for the simultaneous extraction and determination of three types of antidepressant drugs (Clomipramine (CLO), Clozapine (CLZ), and Trimipramine (TRP) by the thin-film solid-phase micro-extraction (TFME-µSPE) method followed by the Gas Chromatography-flame ionization detector (GC-FID) analysis. So, the compound poly (vinyl alcohol) (PVA)/citric acid(CA)/ß-cyclodextrin/Bi2S3@g-C3N4 nano sorbent was constructed by electrospinning technique. Then, nano sorbent was studied to optimize the many parameters impacting the extraction performance. Electrospun nanofiber has a large surface area, high porosity, and homogeneous morphology with a uniform bead-free structure. In optimal conditions, the limits of detection and quantification were calculated to be 0.15-0.03 ng mL-1 and 0.5-0.1 ng mL-1, respectively. The dynamic linear range (DLR) was in the range of 0.1 to 1000 ng mL-1 for CLO and CLZ, and 0.5 to 1000 ng mL-1 for TRP with correlation coefficients (R2) of 0.999. The relative standard deviations (RSDs) were achieved in the range of 4.9-6.8% (intra-day, n = 4) and 5.4-7.9% (inter-day, n = 3) in the period of 3 days. Finally, the capability of the method was evaluated to simultaneously measure trace amounts of antidepressants aqueous sample with desirable extraction efficiency (78 to 95%).