Development and validation of synchronous spectrofluorimetric method for the simultaneous determination of duvelisib and moxifloxacin: greenness metric assessment and application to a pharmacokinetic study in rats.

Duvelisib (DUV) is a potent anticancer drug whereas Moxifloxacin (MOX) is an antimicrobial drug with anti-proliferative potency against cancerous cells, which is empirically administered in cancer treatment. DUV and MOX combination is commonly prescribed to combat infections in patients while they are under chemotherapy treatment. This study describes, for the first time, the development of a simple and green synchronous spectrofluorimetric (SSF) method for the simultaneous estimation of DUV and MOX in plasma. DUV and MOX were quantified at 273 and 362 nm, respectively without interference between each other at Δλof 120 nm. The experimental variables influencing fluorescence intensities were thoroughly investigated and the optimum conditions were established. At pH 3.5, the optimum synchronous fluorescence intensity (SFI) was achieved in water solvent by using sodium acetate buffer solution. Calibration curves for DUV and MOX, correlating the SFI with the corresponding drug concentration, were linear in the range of 50-1000 ng mL-1for both drugs, with good correlation coefficients. The method was extremely sensitive, with limits of detection of 24 and 22 ng mL-1, and limits of quantitation of 40 and 45 ngmL-1for DUV and MOX, respectively. The SSF method was validated according to the Food and Drug Administration (FDA) guidelines for validation of analytical procedures, and the validation parameters were acceptable. The proposed SSF method was applied to the pharmacokinetic and bioavailability studies in rats' plasma after single concurrent oral administration of both drugs. The results of the study revealed that caution should be taken with DUV dose when concurrently administered with MOX. The greenness of SSF method was assessed by three different metric tools namely Analytical Eco-scale, Green Analytical Procedure Index, and Analytical Greenness Calculator. The results confirmed that SSF method is an eco-friendly and green analytical approach. In conclusion, the proposed SSF method is a valuable tool for pharmacokinetic/bioavailability studies and therapeutic drug monitoring of simultaneously administered DUV and MOX.

New Chromatographic Techniques for Sensitive Mebendazole Quantification in the Presence of Degraded Product, Commercial Tablets Application, and Greenness Assessment.

BACKGROUND: Before it spreads to other tissues, mebendazole (MBZ), a highly effective broad-spectrum anthelmintic, is used to treat worm infestations caused by roundworms, hookworms, whipworms, threadworms (pinworms), and the gastrointestinal form of trichinosis. OBJECTIVE: The development of new methods for sensitive quantification of MBZ in the presence of its degraded product is the main objective of the presented research. METHOD: Validated chromatographic techniques with high sensitivity (HPTLC and UHPLC) are used. The HPTLC method was adopted on silica gel HPTLC F254 plates using ethanol, ethyl acetate, and formic acid (3: 8: 0.05, by volume) as a developing system. Furthermore, the UHPLC method is a green isocratic method with a mobile phase containing methanol and 0.1% sodium lauryl sulphate (20:80, v/v). RESULTS: The suggested chromatographic methods are greener than the reported ones in terms of the used greenness assessment methods. To validate the developed methods, International Council on Harmonization (ICH/Q2) guidelines were followed. Successful application of the proposed methods was revealed by the simultaneous analysis of MBZ and its major degradation product, 2-amino-5-benzoylbenzimidazole (ABB). The linear ranges were 0.2-3.0, 0.1-2.0 µg/band for the HPTLC method and 2.0-50, 1.0-40 µg/mL for the UHPLC method for MEB and ABB, respectively. CONCLUSIONS: The suggested methods were used to analyze the studied drug in its commercial tablets. Both pharmacokinetic studies and quality control laboratories can make use of the suggested techniques. HIGHLIGHTS: Green and accurate HPTLC and UHPLC methods for the determination of MBZ and its major degradation products.

Application of Three Ecological Assessment Tools in Examining Chromatographic Methods for the Green Analysis of a Mixture of Dopamine, Serotonin, Glutamate and GABA: A Comparative Study.

The assessment of greenness of analytical protocols is of great importance now to preserve the environment. Some studies have analyzed either only the neurotransmitters, dopamine, serotonin, glutamate, and gamma-aminobutyric acid (GABA), together or with other neurotransmitters and biomarkers. However, these methods have not been investigated for their greenness and were not compared with each other to find the optimum one. Therefore, this study aims to compare seven published chromatographic methods that analyzed the four neurotransmitters and their mixtures using the National Environmental Method Index, Analytical Eco-Scale Assessment (ESA), and Green Analytical Procedure Index (GAPI). As these methods cover both qualitative and quantitative aspects, they offer better transparency. Overall, GAPI showed maximum greenness throughout the analysis. Method 6 was proven to be the method of choice for analyzing the mixture, owing to its greenness, according to NEMI, ESA, and GAPI. Additionally, method 6 has a wide scope of application (13 components can be analyzed), high sensitivity (low LOQ values), and fast analysis (low retention times, especially for glutamate and GABA).

Comparative study of four greenness assessment tools for selection of greenest analytical method for assay of hyoscine N-butyl bromide.

Several assessment tools were recently introduced for the evaluation of the greenness of analytical methods. Each tool has advantages, disadvantages, and a unique assessment protocol. The final results obtained from each assessment tool may lead to a dissimilar conclusion about the selection of the greenest method, which makes the decision confusing as to which an assessment tool relies on. Accordingly, in this comparative case study, four greenness assessment tools-National Environmental Methods Index (NEMI), Eco-Scale Assessment (ESA), Green Analytical Procedure Index (GAPI), and Analytical GREEnness metric (AGREE)-were tested to evaluate 16 chromatographic methods described in the literature for the assessment of the commonly used antispasmodic drug Hyoscine N-butyl bromide (HNBB). The importance of applying more than one assessment tool when evaluating the greenness of analytical methods is explained in this study. Despite NEMI tool simplicity, it was the least effective in providing information about the analytical method as 14 out of 16 methods had the same NEMI pictogram. ESA and AGREE provided reliable numerical assessments that differed in their total scores whereas the total scores were out of 100 and 1 for each, respectively. AGREE has the merits over ESA with respect to automation and highlighting the weakest points in analytical techniques that need further improvements in terms of greenness. GAPI and AGREE provide fully descriptive three-colored pictograms. The main disadvantage of GAPI is complexity compared to NEMI and ESA. AGREE has the merits of simplicity and automation over GAPI. Based on the results, recommendations are made for ESA, GAPI, and AGREE tools, which provide reliable and precise results about the greenness of the method. Planning for the greenness of analytical methods should be assured before practical trials in a laboratory for reduction of chemical hazards released into the environment. Moreover, inclusion of the evaluation of greenness of analytical methods in method validation protocols is strongly recommended.

Impurity profiling high-performance-thin-layer chromatography method involving the assay of essential human micronutrient niacin with eco-scale assessment.

Currently, analytical scientists are paying special attention to reducing reliance on hazardous chemicals in various analytical methods. By embracing this concept, we developed an eco-friendly high-performancethin-layer chromatography (HPTLC) method as an alternative for the conventional HPLC method for the determination of an essential human micronutrient, niacin (NIA), which is used improve the lipid profile of patients. Furthermore, the proposed HPTLC method is capable of determining the structurally related impurities of NIA such as pyridine-2,5-dicarboxylic acid, isonicotinic acid, pyridine, and 5-ethyl-2-methylpyridine, which exhibit nephrotoxic and hepatotoxic effects. The separation of this challenging mixture was achieved on HPTLC sheets using a mixture of ethyl acetate/ethanol/ammonia solution (6:4:0.05, v/v/v), and then the dried plates were scanned at 254 nm. The analytical eco-scale assessment protocol was used to assess the greenness profile of the presented method and compare it with the reported HPLC method. The suggested method was found to be greener with regard to the consumption of solvents and the yielding of waste. The results suggest that the described method can be safely implemented for the routine analysis of NIA pharmaceutical dosage without the interference of potential impurities in quality control laboratories.