Innovative assembled optode device for enhanced in-situ ceric ions (Ce4+) evaluation and preconcentration in its real human, foods, water, and alloy samples.

Cerium (Ce) are the most widely distributed rare earth element. However, humans exposed to Ce through inhalation have been reported to experience heat sensitivity, itching, and heightened taste and odour perception. The present study aims to develop an optical sensor device with a short response time and high selectivity for Ce amongst other ions in various environments. The potential applicability of a 6-hydroxy-5-((4-hydroxy-2-methylphenyl)diazenyl)pyrimidine-2,4(1H,3H)-dione (HHMDPD) assembled ligand as aceric ion (Ce4+)-selective caption optode was examined. After generating an ion pair with Tetra-n-octylammonium bromide (TOABr) and immobilizing on a tri-acetyl cellulose (TAC) membrane, the solubility of the HHMDPD ligand is improved. The constructed optode membrane reacts with Ce4+ by turning its orange colour to violet in Thiel buffer (pH of 5.5), which can be detected spectrophotometrically at λmax 667 nm. The measurement linearity was in the range of 0.70 - 18.7 × 10-6 mol/L of Ce4+ concentration with detection and quantification limits of 0.23 × 10-6 and 0.70 × 10-6 mol/L, respectively. Whatever the Ce4+ concentration in its real samples, the response time of the constructed device was 5.0 min. Additionally, it recorded repeatability and reproducibility with a %RSD of 1.37 and 2.55, respectively (n = 3). The proposed optode device exhibited complete reversibility, for multiple measurements, which could be easily achieved with the aid of a solution of HCl, 0.01 mol/L. The applicability of the proposed device has been effectively extended to analyze synthetic mixes corresponding to different Ce4+ real human, foods, water, and magnesium-based Ce4+ alloys.

Functionalized Carbon Nanotubes for Delivery of Ferulic Acid and Diosgenin Anticancer Natural Agents.

It was investigated whether loading multi-wall carbon nanotubes (CNTs) with two natural anticancer agents: ferulic acid (FUA) and diosgenin (DGN), may enhance the anticancer effect of these drugs. The CNTs were functionalized with carboxylic acid (CNTCOOH) or amine (CNTNH2), loaded with the above pro-drugs, as well as both combined and coated with chitosan or chitosan-stearic acid. Following physicochemical characterization, the drug-loading properties and kinetics of the drug's release were investigated. Their effects on normal human skin fibroblasts and MCF-7 breast carcinoma cells, HepG2 hepatocellular carcinoma cells, and A549 non-small-cell lung cancer cells were evaluated in vitro. Their actions at the molecular level were evaluated by assessing the expression of lncRNAs (HULC, HOTAIR, CCAT-2, H19, and HOTTIP), microRNAs (mir-21, mir-92, mir-145, and mir-181a), and proteins (TGF-ß and E-cadherin) in HepG2 cells. The release of both pro-drugs depended on the glutathione concentration, coating, and functionalization. Release occurred in two stages: a no-burst/zero-order release followed by a sustained release best fitted to Korsmeyer-Peppas kinetics. The combined nanoformulation cancer inhibition effect on HepG2 cancer cells was more pronounced than for A549 and MCF7 cells. The combined nanoformulations had an additive impact followed by a synergistic effect, with antagonism demonstrated at high concentrations. The nanoformulation coated with chitosan and stearic acid was particularly successful in targeting HepG2 cells and inducing apoptosis. The CNT functionalized with carboxylic acid (CNTCOOH), loaded with both FUA and DGN, and coated with chitosan-stearic acid inhibited the expression of lncRNAs and modulated both microRNAs and proteins. Thus, nanoformulations composed of functionalized CNTs dual-loaded with FUA and DGN and coated with chitosan-stearic acid are a promising drug delivery system that enhances the activity of natural pro-drugs.

A modified selective optical sensor for selenium determination based on incorporating xylenol orange in a poly(vinyl chloride) membrane.

A novel optical sensor has been developed to measure selenium ions. The sensor membrane was created by mixing xylenol orange (XO) and sodium tetraphenylborate (NaTPB) with a plasticized poly(vinyl chloride) membrane that contained o-nitrophenyl octyl ether (o-NPOE) as a plasticizer. XO was previously established for use in a colorimeter to measure selenium in water and other media. At pH 6.6, the color of the detecting membrane changed from orange to pink when in contact with Se4+ ions. Various variables affecting the uptake efficiency were evaluated and optimized. Under optimum conditions (i.e., 30% PVC, 60% o-NPOE, and 5.0% of both XO and NaTPB for 5.0 min as the response time), the proposed sensor displayed a linear range 10-175 ng mL-1 with the detection and quantification limits of 3.0 and 10 ng mL-1, respectively. Also, the precision (RSD%) was better than 2.2% for six replicate determinations of 100 ng mL-1 Se4+ in various membranes. For the detection of Se4+, the selectivity of the sensor membrane was investigated for a number of possible interfering inorganic cations, but no appreciable interference was found. With the use of a 0.3 M HCl solution, the sensor was successfully restored, and the response that may have been reversible and reproducible exhibited an RSD% of less than 2.0%. The sensor has been successfully used to analyze Se4+ ions in environmental and biological materials.

Green analytical chemistry and experimental design: a combined approach for the analysis of zonisamide.

Green analytical chemistry principles, as well as experimental design, are a combined approach adopted to develop sensitive reproducible stability indicating HPLC method for Zonisamide (ZNS) determination. The optimal conditions for three chromatographic parameters were determined using a central composite design of the response surface. Kromasil C18 column (150 mm × 4.6 mm, 5 µm) was utilized with ethanol, H2O (30:70 v/v) as a mobile phase at a flow rate of 1 mL/min at 35 °C. Good reproducibility and high sensitivity were achieved along (0.5-10 µg/mL) concentration range. In contrast, the TLC-densitometric method was performed on aluminum plates precoated with silica gel 60F254 as a stationary phase and chloroform: methanol: acetic acid (8:1.5:0.5 by volume) as a developing system. Reproducible results were obtained in the range of (2-10 µg/band). The chromatograms of HPLC and TLC were scanned at 280 nm and 240 nm, respectively. The suggested methods have been validated following ICH guidelines, and no statistically significant differences were detected between the results of the current study and the official USP method. It was also found that using experimental design implements the green concept by reducing the environmental impact. Finally, Eco-Scale, GAPI and AGREE were used to assess the environmental impacts of the suggested methods.

Two Versatile Pencil Graphite-Polymer Sensor Electrodes Coupled with Potentiometry and Potentiometric Titration Methods: Profiling Determinations of Vitamin V in Tablets and Urine Samples.

Herein, we developed a new pencil graphite ion-selective electrode strategy for the broadly used erectile dysfunction medication, sildenafil citrate (SC, vitamin V), for its automated potentiometry and potentiometric titration profiling in marketed tablets and human urine samples. The method was based on ion-pair complexation between SC and sodium tetraphenylborate (Na-TPB) or phosphotungstic acid (PTA), embedded into a pencil-fabricated graphite sensor electrode coated with poly(vinyl chloride, PVC) matrix, which is pre-plasticized with two different pre-studied plasticizers. The modern fabricated electrodes have a proven fast near-Nernstian response for SC over the concentration range of 1.0 × 10-6 to 1.0 × 10-2 and 1.0 × 10-5 to 1.0 × 10-2 M, with LODs of 6.5 × 10-7 and 5.5 × 10-6 over a pH 3-6 for (SC-TPB)- and (SC-PTA)-based membrane sensors, of O-nitrophenyl octyl ether (O-NPOE) and dioctyl phthalate (DOP), respectively. The selectivity coefficients for different interferents, including many inorganic cations, sugars, and/or nitrogenous compounds, were tested and confirmed. Applications of the proposed method were conducted on the determination of SC in its tablets and urine samples under the proper conditions. The percent recovery values were compared with those obtained by an official method and showed an RSD ≤ 0.3% (n = 5).

Smart stability indicating spectrophotometric methods for determination of modafinil: the promising treatment for post-covid neurological syndrome.

Modafinil (MDF) is one of the neurostimulants with a potential effect in the COVID-19 ICU ventilated patients and post-COVID neurological syndrome treatment. Four rapid, simple and cost-effective stability indicating spectrophotometric methods were used for estimation of MDF in the presence of its acidic degradation product, namely; ratio difference (RD), first derivative of the ratio spectra (1DD), mean centering (MCR) and ratio subtraction method (RS). These methods were validated according to ICH guidelines and all methods revealed a good linearity in concentration range of (5-30 µg/mL) in addition to a good accuracy and precision with mean percentage recovery of 99.97 ± 0.305 for (RD), 100.10 ± 0.560 for (1DD), 100.02 ± 0.483 for (MCR) & 99.18 ± 1.145 for (RS) method. Specificity of the proposed methods was assessed and MDF was determined in the presence of up to 80% of its acidic degradation product for RD, 1DD, MCR and RS methods. The proposed methods were successfully applied for the determination of MDF in bulk powder and its tablet dosage form with mean percentage recovery of 100.33 ± 0.915 for (RD), 100.62 ± 0.985 for (1DD), 99.70 ± 0.379 for (MCR) and 100.21 ± 0.313 for (RS) method. The results obtained were statistically compared with those of official HPLC method and showed no significant difference with relevance accuracy and precision.

PEG@ Carbon Nanotubes Composite as an Effective Nanocarrier of Ixazomib for Myeloma Cancer Therapy.

In this work, the preparation of a PEG@ multi-walled carbon nanotubes (MWCNTs) composite has shown a great potential effect in tumor therapy using graphite powder at room temperature. PEGylated MWCNTs were created and used as a carrier for targeting the antineoplastic drug Ixazomib to myeloma cancer cells (abnormal plasma cells). Ixazomib (MLN2238) was covalently encapsulated into functionalized carbon nanotubes modified with polyethylene glycol (PEG 600) to obtain MWCNTs-PEG-MLN2238. The Ixazomib@ MWCNTs-PEG composite shows promising results as an effective nanocarrier and using a small amount of MWCNTs-PEG-Ixazomib that has a low toxicity compared with that of Ixazomib alone. A multifunctional MWCNTs-PEG-Ixazomib composite is used to test biological effects on multiple myeloma cell lines RPMI 8226 using the MTT assay to enhance treatment efficiency. The cytotoxicity of free Ixazomib citrate (69% cell viability of RPMI8226 cells) was higher than that of MWCNTs-PEG-Ixazomib (91% cell viability) at the same maximum concentration of Ixazomib citrate (50 µg/ml). In this work, we performed a study of preparation of MWCNTs with an acceptable Ixazomib loading efficiency and determination of the drug systemic toxicity for the first time. In this study, the preparation of MWCNTs with acceptable Ixazomib loading efficiency and determination of the drug systemic toxicity was performed for the first time. The MTT assay results show decreasing the toxicity of Ixazomib after loading with the MWCNTs-PEG composite. The MWCNTs-PEG @ Ixazomib show promising results as an effective carrier of Ixazomib and lead to a decrease in the cost of using Ixazomib.

Greenness Assessment of Two Validated Stability-Indicating Chromatographic Methods for Estimating Modafinil Using the Analytical Eco-Scale.

BACKGROUND: Modafinil (MDF) is one of the drugs used for the treatment of narcolepsy. OBJECTIVE: This manuscript describes the development and validation of two chromatographic stability-indicating methods for MDF in the presence of its acid-induced degradation product. METHODS: MDF was degraded under different stress conditions and identification of the degradation product was performed using IR and mass spectroscopy. The first method involved TLC, in which plates precoated with silica gel G60 F254 were used and the developing system was dichloromethane- methanol (9:1, v/v). The second method was an eco-friendly (HPLC) method that utilized a C-18 column and ethanol-H2O (30:70, v/v) as a mobile phase with a flow rate of 1 mL/min and UV detection at 220 nm. RESULTS: Good linear relationships were obtained within the ranges 1-10 µg/band and 2-10 µg/mL for TLC-densitometry and HPLC, respectively. The obtained results were statistically compared with those of the official HPLC method and showed no significant difference with respect to their accuracy and precision at P = 0.05. Greenness scores represent excellent green analysis results in comparison with the reported studies. CONCLUSIONS: The proposed methods were validated according to ICH guidelines and were applied on bulk powder and pharmaceutical dosage forms using eco-friendly mobile phases in line with worldwide trends. HIGHLIGHTS: Chromatographic methods have been validated for the estimation of MDF in the presence of its degradation product. Clarification of the degradation pathway and elucidation of the structure were stated for the first time. This is the first published method using greenness assessment metrics for the analysis of MDF.