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A fast eco-friendly colorimetric method was developed for the determination of Tobramycin in drug substance, ophthalmic formulations, and spiked human plasma using silver nanoparticles optical sensor. Even though tobramycin is non-UV–visible absorbing, the developed method is based on measuring the absorbance quenching of silver nanoparticles resulting from the interaction with tobramycin. Different factors affecting the absorbance intensity were studied as; silver nanoparticle concentration, pH, buffer type, and reaction time using quality by design approach. Validation of the proposed method was performed according to ICH guidelines and was found to be accurate, precise, and sensitive. The linearity range of tobramycin was 0.35–4.0 μg/mL. The optical sensor was successfully applied for the determination of Tobramycin in ophthalmic formulations and spiked human plasma without pre-treatment. Additionally, the binding between Tobramycin and PVP- capped silver nanoparticles was studied using molecular docking software. The method was assessed and compared to colorimetric reported methods for the green character using Green Analytical Procedure Index (GAPI) and Analytical GREEnness calculator (AGREE) tools and found to be greener. [ABSTRACT FROM AUTHOR]

Rationale: Antibiotics have been detected worldwide in the aquatic environment. Moreover, certain classes of antibiotics have been repurposed for the management of COVID-19, which increased their use and presence in wastewater. Their occurrence even in low concentrations leads to the development of antibiotic resistance. Methodology: Magnetite pectin nanoparticles (MPNP) were fabricated and compared to an established model of mesoporous silica nanoparticles (MSNP). Our studied adsorbate is levofloxacin, a fluoroquinolone antibiotic, commonly used in managing COVID-19 cases. Results: The influence of various factors affecting the adsorption process was studied, such as pH, the type and concentration of the adsorbent, contact time, and drug concentration. The results illustrated that the optimum adsorption capacity for antibiotic clearance from wastewater using MPNP was at pH 4 with a contact time of 4 h; while using MSNP, it was found to be optimum at pH 7 with a contact time of 12 h at concentrations of 10 µg/mL and 16 g/L of the drug and nanoparticles, respectively, showing adsorption percentages of 96.55% and 98.89%. Drug adsorption equilibrium data obeyed the Sips isotherm model. Discussion and conclusion: HPLC assay method was developed and validated. The experimental results revealed that the MPNP was as efficient as MSNP for removing the antibacterial agent. Moreover, MPNP is eco-friendly (a natural by-product of citrus fruit) and more economic as it could be recovered and reused. The procedure was evaluated according to the greenness assessment tools: AGREE calculator and Hexagon-CALIFICAMET, showing good green scores, ensuring the process's eco-friendliness. [ABSTRACT FROM AUTHOR]

The presence of antibiotic traces in the aquatic system due to the inefficient treatment of the pharmaceutical wastewater represented threats, such as bioaccumulation and antibiotic-resistance, to the environment and human health. Accordingly, for the first time, the current work utilized the photocatalytic degradation and the adsorption approach for Levofloxacin (LEVO) in pharmaceutical wastewater using new designed nano aspects. Therefore, spherical Zinc oxide nanoparticles (ZnONP) sized 17 nm and ultrathin sheet-like structure graphene oxide nanosheets (GONS) with layer thickness ~5 nm were fabricated separately or in a combination between them then characterized via Transmission Electron Microscope (TEM), Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), Fourier Transforms Infrared Spectroscopy (FTIR), absorption spectra (UV-Vis) and Brunauer-Emmett-Teller (BET). Additionally, several parameters were investigated to evaluate the potential of the removal process, such as pH, the exposure time to UV radiation, the type and concentration of the nanoparticles (NPs) and the initial concentration of the drug using a mixed fractional factorial design. The most effective parameter for LEVO removal was the NPs type followed by the initial drug concentration. Furthermore, an RP-HPLC/UV method was developed and validated for measuring the percentage of removal for LEVO drug. The highest percentage removal for both 50 and 400 µg mL−1 LEVO was 99.2% and 99.6%, respectively, which was achieved using ZnONP/GONS combination at pH 9 ± 0.05 and UV light exposure time 120 min. In addition, the negative antibacterial activity of the treated wastewater sample confirmed the drug removal. The established protocol was successfully applied on wastewater samples collected from a pharmaceutical company that encouraged researchers to mainstream this design to be applied on other pharmaceutical wastewater drugs. [ABSTRACT FROM AUTHOR]

[Display omitted] • Eco-friendly chromatographic methods for determination of ondansetron in the presence of five impurities in different pharmaceutical dosage forms. • Validation of the developed methods as per ICH guidelines. • Application of the developed methods to oral films; a newly developed dosage form. • Verification of developed methods' greenness and whiteness using advanced assessment metrics. • Insilico toxicity profiling of impurities using pkcsm and preADMET softwares. Drug impurities are seen as a crucial threat to drug safety, specifically when dealing with mutagenic/ toxic impurities. Here, we present LC-MS/MS and HPTLC-densitometric methods for simultaneous quantification of Ondansetron and its four official impurities. For the LC-MS/MS, the isocratic elution was applied using methanol and water containing 0.1 % formic acid in a ratio (70:30 v/v) at a flow rate of 1 mL/min, a stationary phase C 18 column (4.6 × 50 mm, 5 µm) and mass detection using the MRM mode. For the HPTLC-densitometric method, the mobile phase consists of ethyl acetate: methanol in a ratio (6:4 v/v), and the UV detection was at 216 nm. The developed methods have been validated per ICH recommendations and then evaluated using five tools for whiteness and greenness assessment, offering promising results in comparison to reported chromatographic methods. Additionally, the toxicity profile of the impurities was expected by the online software; PreADMET and pkCSM. The developed methods are recommended for quality control due to their high analytical performance as well as their sustainability, simplicity, and cost-effectiveness, which improves the surveillance capability. [ABSTRACT FROM AUTHOR]

• Ecofriendly methods for determination of two commonly prescribed GIT drugs. • The use of Absorptivity coefficient as a resolution tool for overlapped spectra. • Resolution of the entire original zero order spectra of drugs under investigation. • Application of the Green Analytical Procedure Index for the applied methods. Three eco-friendly methods were applied and validated for simultaneous determination of two commonly prescribed drugs for gastro-intestinal treatment Ranitidine hydrochloride and Metronidazole in bulk powder and in their pharmaceutical preparations in the ratio of 3:5. The first two methods were based on smart spectra manipulating approaches to resolve the zero-order spectrum of each drug as single pure component and measuring their concentrations using the absorbance value at the corresponding λ max, 325 nm and 311 nm for Ranitidine and Metronidazole, respectively. Both methods named response correlation method and a- centering method depend on the presence of an isosbestic point between the superimposed spectra of both drugs. While the third method was a TLC-densitometric one which was performed on silica plates F254 using a mobile phase composed of methanol and ethyl acetate in a ratio (24:6 v/v). The results of the presented methods came out to be acceptable with respect to accuracy and precision and the selectivity was evaluated through analysis of synthetic mixtures of the both drugs in different ratios. All the results were validated according to the ICH guidelines. The green character of the developed methods was assessed using a new tool called Green Analytical Procedure Index (GAPI). [ABSTRACT FROM AUTHOR]

Paracetamol is an analgesic-antipyretic drug and Ibuprofen is a non-steroidal anti-inflammatory drug. They are co-formulated as tablets to improve analgesia, to simplify prescribing and to improve patient compliance. Three accurate, simple and sensitive spectrophotometric methods were developed for the simultaneous determination of Paracetamol and Ibuprofen in their co-formulated dosage form. The first method was the ratio difference, which was based on the measurement of the difference in absorbance between the two wavelengths (210.6 and 216.4 nm) for Ibuprofen and (236.0 and 248.0 nm) for Paracetamol. The second method was constant center method which depends on using the constant found in the ratio spectra. The third method was the mean centering of ratio spectra which measured the manipulated values at 240 nm and 237 nm for Ibuprofen and Paracetamol, respectively. Beer's law was obeyed in the concentration range of 2–50 μg/mL for Ibuprofen and 2–20 μg/mL for Paracetamol. The recovery % of the accuracy of both methods ranged from 99.64 to 100.56%. Factors affecting the resolution of the spectra were studied and optimized. The three methods are validated according to ICH guidelines and could be applied for the pharmaceutical preparation. [ABSTRACT FROM AUTHOR]

An analytical investigation was carried out to study the treatment and amplification of the spectral signals produced by critical concentrations with high accuracy and precision using two advanced approaches. The factorized-spectrum approach was applied through two novel methods which were: absorptivity centering technique via both: factorized zero order absorption spectrum (ACT-FSD0 ΔA) and factorized ratio spectrum (ACT-FSR ΔP). The proposed methods were found to be linear in the ranges of (15–100 μg/mL) and (3–40 μg/mL) for ASP and MTO, respectively. Those methods were compared to the methods following the geometrical standard addition approach: ratio H-point standard addition method (RHPSAM) and geometrical induced amplitude modulation (GIAM). The approaches were applied for the determination of the minor component metoclopramide in its mixture with the major component aspirin in the challengeable ratio of (1,90) respectively in a white multicomponent system. The results obtained from the proposed approaches were statistically compared with each other. The methods were validated according to ICH guidelines where the results were found to be within the acceptable limits. The methods were found to be accurate and reliable for the determination of metoclopramide critical concentration besides aspirin concentration. The results of single factor ANOVA analysis indicated that there is no significant difference among the developed methods. These methods provided simple resolution of this binary combination from synthetic mixtures and pharmaceutical preparation and can be conveniently adopted for routine quality control analysis. Unlabelled Image • Treatment & amplification of weak spectral signal of Metoclopramide in white system • 2 spectral approaches were adopted and compared for ASP & MTO in ratio (90,1). • Factorized spectrum approach: absorptivity centering (ACT-FSD0) and (ACT-FSR) • Geometric standard addition: GIAM and RHPSAM. • Statistical comparison and discussion for limitation and advantages. [ABSTRACT FROM AUTHOR]

[Display omitted] • A bare and cobalt oxide nanoparticles modified coated graphite electrodes were constructed for determination of Sulfacetamide sodium. • Determination of Sulfacetamide sodium in its pharmaceutical dosage form and spiked rabbit aqueous humor samples. • The addition of nanoparticles improved the performance of the electrodes. • Very low detection limits were reached using the modified coated graphite sensor. • The proposed method was assessed for greenness using GAPI greenness assessment tool. This study presents the fabrication of an innovative coated graphite electrode modified with cobalt oxide nanoparticles, for potentiometric determination of Sulfacetamide sodium. The functionalized nano-electrode was compared to a classical one; to study the advantages of addition of nanoparticles which was found to improve the performance characteristics of the electrode including improved sensitivity and selectivity, as well as, extended operational lifespan. The functionalized nano-electrode was more sensitive than the classical one with linearity range (1 × 10−7–1 × 10−2 M) and a limit of detection down to 2.24 × 10−8 M. This small modification increased the electrode's potential stability by preventing the formation of a water layer on the surface of the solid contact electrode. The electrochemical performance of the proposed sensors was evaluated according to the IUPAC recommendation data and was found to be within the acceptable ranges. These developed potentiometric platforms were applied to quantitatively analyze Sulfacetamide sodium in its pure solutions, pharmaceutical dosage form and spiked rabbit aqueous humor with satisfactory recovery percentages without pre-extraction procedure nor interference of the co-formulated drug; Prednisolone acetate and excipients. The proposed method was statistically compared with the reported method in literature and no statistically significant difference was found. The proposed method was evaluated for its environmental sustainability utilizing the Green Analytical Procedure index (GAPI) as a greenness assessment tool. [ABSTRACT FROM AUTHOR]