Solid-phase extraction of Pb2+ ion from environmental samples onto L-AC-Ag-NP by flame atomic absorption spectrometry (FAAS)

The development of a solid-phase extraction (SPE) procedure for the pre-concentration of trace amounts of Pb²⁺ ion on 2-furan-2-yl-1-furan-2-ylmethyl-1H-benzoimidazole loaded on activated carbon modified with silver nanoparticles (L-AC-Ag-NP) was presented. The metal ion retained on the sorbent was quantitatively determined via complexation with the ligand. The complexed metal ion was efficiently eluted using 10 mL of 4 mol L^?1 sulphuric acid in 10 w/v% acetone. The influences of the analytical parameters, including pH, amounts of the ligand and the solid phase, eluent conditions and sample volume, on the recoveries of the metal ion were optimised. Using the optimised parameters, the linear response of the SPE method for Pb²⁺ ion were in the ranges of 0.2–160 µg L^?1, and the detection limit for Pb²⁺ ion was 0.034 µg L^?1. The proposed method exhibits a pre-concentration factor (PF) of 80 and an enhancement factor of 30 for Pb²⁺ ion. The presented results demonstrate the successful application of the proposed method for the determination of Pb²⁺ ion in some real samples with high recoveries (>93%) and reasonable relative standard deviation (RSD < 2%).     

Solid phase extraction of antidepressant drugs amitriptyline and nortriptyline from plasma samples using core-shell nanoparticles of the type Fe3O4@ZrO2@N- cetylpyridinium,and their subsequent determination by HPLC with UV detection

The solid phase extraction (SPE) is described for preconcentration of the antidepressant drugs amitriptyline and nortriptyline prior to their determination by HPLC with UV detection. It is based on the use of water-dispersible core-shell nanoparticles (NPs) of the Fe₃O₄@ZrO₂@N-cetylpyridinium type. The positively charged surfactant N-cetylpyridinium forms mixed aggregates with the drugs on the surface of the core-shell and thereby improves the adsorption of amitriptyline and nortriptyline through hydrophobic and/or ionic interactions. Their extraction depends on the type and amount of surfactant, sample pH, extraction time, desorption conditions, sample volume and amount of NPs that were optimized by application of experimental design. The enrichment factors are 220 and 250, respectively, for amitriptyline and nortriptyline, and the detection limits are 0.04 and 0.08 ng·mL‾¹. This protocol enables accurate and precise quantification of the two drugs in complex and low content samples. It was applied to the determination of the two drugs in plasma samples with relative recoveries in the range from 89 to 105 % and RSDs less than 4 %.

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Simultaneous removal of Cu2+ and Cr3+ ions from aqueous solution based on Complexation with Eriochrome cyanine‐R and derivative spectrophotometric method

TiO₂ nanoparticles deposited on activated carbon (TiO₂–NP–AC) was prepared and characterized by XRD and SEM analysis. Subsequently, simultaneous ultrasound‐assisted adsorption of Cu²⁺ and Cr³⁺ ions onto TiO₂‐NPs‐AC after complexation via eriochrome cyanine R (ECR) has been investigated with UV–Vis and FAA spectrophotometer. Spectra overlapping of the ECR‐Cu and ECR‐Cr complex was resolve by derivative spectrophotometric technique. The effects of various parameters such as initial Cu²⁺ (A) and Cr³⁺ (B) ions concentrations, TiO₂‐NPs‐AC mass (C), sonication time (D) and pH (E) on the removal percentage were investigated and optimized by central composite design (CCD). The optimize conditions were set as: 4.21 min, 0.019 mg, 20.02 and 13.22 mg L^?1 and 6.63 for sonication time, TiO₂–NP–AC mass, initial Cr³⁺ and Cu²⁺ ions concentration and pH, respectively. The experimental equilibrium data fitting to Langmuir, Freundlich, Temkin and Dubinin–Radushkevich models show that the Langmuir model is a good and suitable model for evaluation and the actual behavior of adsorption process and maximum adsorption capacity of 105.26 and 93.46 mg g^?1 were obtained for Cu²⁺ and Cr³⁺ ions, respectively. Kinetic evaluation of experimental data showed that the adsorption processes followed well pseudo second order and intraparticle diffusion models.     

Preparation of chitosan functionalized end‐capped Ag‐NPs and composited with Fe3O4‐NPs: Controlled release to pH‐responsive delivery of progesterone and antibacterial activity against pseudomonas aeruginosa (PAO‐1)

In this work, functionalized chitosan end‐capped Ag nanoparticles (NPs) and composited with Fe₃O₄‐NPs was prepared as pH‐responsive controlled release carrier for gastric‐specific drug delivery. The structure of prepared material was characterized by FE‐SEM, XRD, EDS and FT‐IR analysis. The loading behavior of the progesterone onto this novel material was studied in aqueous medium at 25°C and their release was followed spectrophotometrically at 37°C in seven different buffer solutions (pH 1.2, 2.2, 3.2, 4.2, 5.2, 6.2 and 7.2) to simulate intestine and gastric media which experimental results reveal more release rate in pH 1.2 (gastric medium) with respect to other buffers. This observation is attributed to dependency of the CS‐IMBDO‐Ag‐Fe₃O₄‐NPs and progesterone structure with buffer pH that candidate this new material as prospective pH‐sensitive carrier for gastric‐targeted drug delivery. On the other hand, the antibacterial properties of this material against gram‐negative bacterium pseudomonas aeruginosa (PAO‐1) in agar plates was studied and accordingly based on broth micro dilution the minimum bactericidal concentration (MBC) and minimum inhibitory concentration (MIC) with respect to standard CLSI in different concentrations of CS‐IMBDO‐Ag‐Fe₃O₄‐NPs was calculated. The results reveal that MIC and MBC values are 50 and 1250 μg/mL, respectively. In addition, extracts of Portulaca oleracea leaves was prepared and its antibacterial activity in single and binary system with CS‐IMBDO‐Ag‐Fe₃O₄‐NPs as synergies effect against PAO‐1 was tested and results shown that these materials have significant synergistic effect for each other.     

Photocatalytic Activity of Supported Metal Nanoparticles and Single Atoms

Photocatalysis has been known as one of the promising technologies due to its eco-friendly nature. However, the potential application of many photocatalysts is limited owing to their large bandgaps and inefficient use of the solar spectrum. One strategy to overcome this problem is to combine the advantages of heteroatom-containing supports with active metal centers to accurately adjust the structural parameters. Metal nanoparticles (MNPs) and single atom catalysts (SACs) are excellent candidates due to their distinctive coordination environment which enhances photocatalytic activity. Metal-organic frameworks (MOFs), covalent organic frameworks (COFs) and carbon nitride (g-C₃N₄) have shown great potential as catalyst support for SACs and MNPs. The numerous combinations of organic linkers with various heteroatoms and metal ions provide unique structural characteristics to achieve advanced materials. This review describes the recent advancement of the modified MOFs, COFs and g-C₃N₄ with SACs and NPs for enhanced photocatalytic applications with emphasis on environmental remediation.     

Podophyllotoxin extraction from Linum usitatissimum plant and its anticancer activity against HT‐29, A‐549 and MDA‐MB‐231 cell lines with and without the presence of gold nanoparticles

In recent years, gold nanoparticles (Au‐NPs) have been taken into consideration in nanomedicine due to their excellent biocompatibility, chemical stability and promising optical properties. In this research, podophyllotoxin conjugated with gold nanoparticles (Au‐NPs‐POT) was synthesized and the conjugation of POT with Au‐NPs was confirmed using scanning electron microscopy, mass spectrometry and Fourier transform infrared spectroscopy. The anticancer effects of the product on preclinical models of lung, colon and breast cancers were investigated using MTT test. The analyses showed a direct dose–response relationship. It was found that higher concentrations of POT have more positive effects on the inhibition of cancer cell growth. At POT concentrations of 1, 2.5, 5, 7.5, 10, 15 and 20 ng ml^?1, approximately 50% of the growth of colorectal, lung and breast cancer cell lines was inhibited, while similar results were obtained in the presence of 1, 2, 3, 4 and 5 μg ml^?1 Au‐NPs‐POT. Au‐NPs‐POT exhibited the lowest cytotoxicity due to the presence of POT. The anticancer feature of Au‐NPs‐POT proved the potential to develop better anticancer therapeutics and to open new avenues for treatment of cancers.     

Optimization of solid phase dispersive field‐assisted ultrasonication for the extraction of auramine O and crystal violet dyes using central composite design

Simultaneous preconcentration and determination of auramine o (AO) and crystal violet (CV) dyes from aqueous solution was conducted by ultrasound assisted (dispersive) solid phase microextraction (UASPME) based on SnO₂/SnS composite loaded activated carbon (SnO₂/SnS‐NCs‐AC). The prepared of SnO₂/SnS‐NCs‐AC was characterized by FESEM and XRD analysis. Main and interaction influences of operational parameters such as pH, sonication time, amounts of sorbent, and type of eluent on extraction efficiency were investigated by central composite design and optimized with desirability function approach (DFA). ANOVA was conducted and shows that optimized values were found at 15.33 min sonication time, 0.019 g SnO₂/SnS‐NCs‐AC mass, pH 5.46 and among different solvents, dimethyl formamide was selected as an efficient eluent. Under this conditions recoverees percentage were obtained 82.85% and 86.70% for AO and CV, respectively. Based on F‐test under ANOVA all main effect and interaction effect of understudy parameters has the significant effect on the responses. At optimum conditions, limit of detection (0.0015 and 0.001 mg/l), limit of quantitation (0.4 and 0.4 mg/l), limit of linearity (9.0 and 9.0 mg/l), enrichment factor (33.48 and 83.71) and percent relative standard deviation (3.44 and 4.20) were found to be for auramine o and crystal violet dyes, respectively. Finally, the method was successfully applied for the preconcentration and determination of AO and CV in water samples and ER% of 89.0‐97.0 and 96.2–98.0% as acceptable range were found to be for AO and CV samples, respectively.