Eco-friendly liquid chromatography method for the quantification of ibrutinib in a pharmaceutical dosage form.

The objective of this study was to quantitatively determine Bruton's tyrosine kinase inhibitor ibrutinib in its capsule dosage form and assess the homogeneity of the dosage form using green chromatography. The chromatographic method using gradient elution mode was optimized and validated in accordance with the International Council for Harmonization guidelines. The analysis was conducted on a Zodiac C18 column (75 × 4.6 mm and 3.5 µm) using a mobile phase consisting of pH 5.5 potassium phosphate buffer (mobile phase A) and 90% ethanol in milli-Q water (mobile phase B), with a flow rate set at 0.6 mL/min. Based on the validation data, the accuracy results fell within the range of 99.1%-100.6%. The relative standard deviation (% RSD) from precision for both the assays and the uniformity of dosage by content uniformity were determined to be 0.82 and 1.16, respectively. The correlation coefficient obtained from the linearity experiment was 0.999, indicating a strong linear relationship. The greenness of the developed method was assessed using various tools, including the National Environmental Methods Index (NEMI) pictogram, Modified NEMI, Analytical Eco-score calculation, Green Analytical Procedure Index (GAPI) pictogram, Analytical GREEnness (AGREE), and AGREE preparation (AGREEprep). The obtained greenness profile suggests that the optimized LC method is an excellent greener method, supported by the analytical eco-score of 86.

The ecological impact of liquid chromatographic methods reported for bioanalysis of COVID-19 drug, hydroxychloroquine: Insights on greenness assessment.

Hydroxychloroquine is a drug that has been widely used during the early stages of COVID-19 pandemic. Different liquid chromatographic methods have been reported for the analysis of hydroxychloroquine in various biological matrices such as human plasma, serum, whole blood, oral fluid, rat plasma and tissues. In this comparative study, the most popular tools used for assessing the greenness profile: National Environmental Methods Index (NEMI), Eco-Scale Assessment (ESA), Green Analytical Procedure Index (GAPI) and Analytical Greenness metric (AGREE) were utilized to evaluate the ecological impact of eighteen liquid chromatographic methods developed for the bioanalysis of COVID-19 drug; hydroxychloroquine. NEMI is the simplest tool for evaluating the greenness profile of developed methods, but it is the least informative approach as all the reported methods had the same NEMI pictograms. On the other hand, GAPI is a dependable tool providing a complete picture about the method greenness starting from sampling until the final determination. ESA and AGREE tools are digitally presented and more easily applied. Therefore, their utilization for greenness assessment is highly recommended. Selection of the highest eco-friendly analytical procedure is of a paramount importance for protecting human health and the environment. Considering the greenness of the analytical procedures is highly recommended before proceeding to routine use in order to minimize the chemical hazards to the environment. The most eco-friendly analytical procedures for the analysis of hydroxychloroquine in biological samples according to ESA, GAPI and AGREE tools will be highlighted and discussed.

Utility of Silver-nanoparticles for Nano-fluorimetric Determination of Vancomycin Hydrochloride in Pharmaceutical Formulation and Biological Fluids: Greenness Assessment.

Vancomycin hydrochloride (VANH) is a glycopeptide antibiotic commonly employed in the prophylaxis and therapy of various gram-positive bacterial life-threatening infections. Due to the narrow therapeutic window of VANH, its serum levels should be well-monitored to avoid its toxicity and to optimize its therapy. Herein, an innovative silver-nanoparticles enhanced fluorescence technique was designed for VANH rapid analysis in its pharmaceutical formulation and biological fluids. This technique is based on reinforcement of VANH fluorescence intensity with silver-nanoparticles that were synthesized by a redox reaction between VANH and silver nitrate in NaOH alkaline medium using polyvinylpyrrolidone as a stabilizer. The produced silver-nanoparticles were characterized by using UV-visible spectroscopy where they have an intense absorption maximum at 415 nm and transmission electron microscope (TEM) micrograph where they are spherical in shape with smooth surface morphology and size of 10.74 ± 2.44 nm. The fluorescence intensity was measured at 394 nm after excitation at 259 nm. Under optimum conditions, a good linear relationship was accomplished between the VANH concentration and the fluorescence intensity in a range of (1-36) ng/mL with a limit of detection of 0.29 ng/mL. Greenness assessment was performed using two assessment tools namely; eco-scale scoring and green analytical procedure index revealing excellent greenness of the proposed technique. The proposed technique was validated according to the International Conference on Harmonisation (ICH) recommendations and statistically compared with the reported HPLC method revealing no significant difference concerning accuracy and precision at p = 0.05. The proposed technique depended primarily on water as a cheap and eco-friendly solvent.

Unique green chromatography method for the determination of serotonin receptor antagonist (Ondansetron hydrochloride) related substances in a liquid formulation, robustness by quality by design-based design of experiments approach.

Serotonin receptor antagonist drug Ondansetron hydrochloride injectable formulation containing all related substances was identified and quantified by a single, simple, sensitive, eco-friendly, and green high-performance liquid chromatography method. The disseverment of all impurities was achieved with the Discovery Cyano (250 × 4.6) mm, 5 µm column. The gradient program was composed of pH 5.7 phosphate buffer as mobile phase A and acetonitrile as mobile phase B. The flow rate, column compartment temperature, and detection wavelengths were 0.9 mL/min, 30°C, and 216 nm, respectively. The method was validated as per current regulatory guidelines. The obtained %relative standard deviation for the precision results was between 0.55 and 2.72% for all impurities. The correlation coefficient values from the linearity experiment for impurities and analyte were more than 0.995. The accuracy results were obtained between 88.4 and 113.0% for all impurities. Both sample and standard solutions showed 24 h stability at benchtop and refrigerator conditions. All impurities and analytes met the specificity and mass balance for all forced degradation conditions. Quality-by-design-based design of experiments was utilized to establish the method's robustness. Method greenness was assessed by using the current advanced tool green analytical procedure index, National Environmental Methods Index, and analytical eco-scale.

A Quality by Design and green LC technique for the determination of mast cell stabilizer and histamine receptor antagonist (Olopatadine HCl) in multiple formulations.

Mast cell stabilizer and histamine receptor antagonist olopatadine hydrochloride (OPT) assay method predicated on LC have been established for the analysis in multiple formulations. The current method dealt with ophthalmic solution, nasal spray, and tablet formulation products. The isocratic chromatography method was optimized and validated with a Boston green C8 column (150 × 4.6 mm, 5 µm i.d.). Sodium dihydrogen phosphate buffer (pH 3.5) with acetonitrile in the ratio of 75:25 (v/v) was used as a mobile phase at a flow rate of 1.0 mL min-1 and at the column temperature of 30°C, and the detection was done at 299 nm. The method was validated as per International Council for Harmonisation (ICH) guidelines and United States Pharmacopoeia (USP). The accuracy results ranged from 99.9 to 100.7%, % relative standard deviation (RSD) from the precision was 0.5, and correlation coefficient from the linearity experiment was > 0.999. Solution stability was established for 24 h at room temperature and refrigerator conditions, and it was found that the solutions were stable. Using quality by design-based experiment designs, critical quality attributes were studied and it was found that the method was robust. In all the forced degradation studies peak purity was passed, and no interference was found at the retention time of the active component. The method validation data demonstrated that the developed method is linear, precise, accurate, specific, robust, and stable for the determination of OPT from multiple formulations. Analytical eco-scale tool, Green Analytical Procedure Index (GAPI) tool, and the National Environmental Method Index (NEMI) were used to evaluate the greenness of the method, and the analytical eco-score of 77 for the presented method was found to be excellent.

Environmental impact of the reported chromatographic methods for the determination of the first FDA-Approved therapy for COVID-19 Patients, Remdesivir: A comparative study.

Remdesivir (REM) is considered the first therapeutic option approved by US Food and Drug Administration (FDA) for clinical care in case of hospitalized patients suffering in COVID-19 epidemic. In the presented multilateral comparative search, four eco friendlessness approaches -National Environmental Methods Index (NEMI), Eco-Scale Assessment (ESA), Green Analytical Procedure Index (GAPI), and Analytical Greenness metric (AGREE) are tested to assess 16 analytical chromatographic procedures reported for the analysis of the commonly used antiviral drug; Remdesivir (REM). The values of testing more than one approach when estimating the eco-friendly characters for analytical methods are illustrated in this study. On the light of the outcomes, ESA and AGREE approaches are recommended as they are easily applied and digitally presented. Furthermore, GAPI is also a reliable tool in terms of comprehensiveness for the whole analytical procedures, from sampling till the final assessment. NEMI is the easiest and fastest greenness evaluation tool; however, the information it provides is particularly of limited scope and sometimes inaccurate. To ensure greenness of chromatographic analytical methods, there must be clear planning beforehand, to reduce chemical hazards sent to environment. Additionally, it is highly recommended in method validation protocols to consider the greenness of a given analytical procedure before releasing to routine use. The LC-MS/MS analysis for the active metabolite of REM (Nuc) reported by Avataneo et al. and Du et al. proved to be the best bio-analytical methods regarding the environmental aspects depending on the GAPI and AGREE tools. However, the HPLC method for REM analysis in intravenous solution reported by Jitta et al. proved to be the greenest analytical method for determination of REM in the pharmaceutical dosage forms according to the ESA, GAPI, and AGREE tools.

Implementing Green Analytical Methodologies Using Solid-Phase Microextraction: A Review.

Implementing green analytical methodologies has been one of the main objectives of the analytical chemistry community for the past two decades. Sample preparation and extraction procedures are two parts of analytical method development that can be best adapted to meet the principles of green analytical chemistry. The goal of transitioning to green analytical chemistry is to establish new methods that perform comparably-or superiorly-to traditional methods. The use of assessment tools to provide an objective and concise evaluation of the analytical methods' adherence to the principles of green analytical chemistry is critical to achieving this goal. In this review, we describe various sample preparation and extraction methods that can be used to increase the greenness of a given analytical method. We gave special emphasis to modern microextraction technologies and their important contributions to the development of new green analytical methods. Several manuscripts in which the greenness of a solid-phase microextraction (SPME) technique was compared to other sample preparation strategies using the Green Analytical Procedure Index (GAPI), a green assessment tool, were reviewed.

Assessing the Greenness and Environmental Friendliness of Analytical Methods: Modern Approaches and Recent Computational Programs.

Environmental measures have drawn more attention recently as a means of identifying cost-effective, safe, and green approaches in analytical methods. As a result, white and green analytical chemistry was developed. Greenness, whiteness, and chemical risks are all measured under the general expression "environmental measurements." For the first time, the greenness, whiteness, and chemical risk-measuring programs are presented along with their histories, concepts, advantages, and disadvantages. The six scales that were published between 2020 and 2023, including the Analytical Greenness Calculator (AGREE), the Analytical Greenness Metric for Sample Preparation (AGREEprep), the Complementary Green Analytical Procedure Index (ComplexGAPI), Red-Green-Blue (RGB12), blue applicability grade index (BAGI), and the Chloroform-oriented Toxicity Estimation (ChlorTox) scales are discussed. Also, the applications of several analytical methods have been compared. Lastly, patterns for the future were suggested. We hope this review is helpful for analysts to stay up-to-date with recent greenness, whiteness, and chemical risk scales. Additionally, the most appropriate procedure has been chosen, applied, and compared easily.

Green analytical chemistry metrics: A review.

Green analytical chemistry encourages reducing the use of toxic chemicals/reagents, using energy-efficient equipment, and generating minimal waste. The recent trends in analytical method development focus on the miniaturization of the sample preparation devices, the development of solventless or solvent-minimized extraction techniques, and the utilization of less toxic solvents. The twelve principles of GAC serve as a basic guideline for inducing greenness in the analytical procedures. Despite these guidelines, in many conditions, some undesired steps are unavoidable. Therefore, it is important to evaluate the greenness of analytical procedures to assess and, if possible, reduce their impact on the environment and workers. Several metrics have been developed for the evaluation of the greenness of analytical procedures. Analytical Eco-Scale, Green Analytical Procedure Index, and Analytical Greenness Metric are among some important tools for assessing the greenness of analytical procedures. All these metrics take different aspects of the analytical procedure into account to provide the green index of the procedure. This review covered these metrics, their principles, and examples of their application to selected analytical procedures. The advantages and limitations of these metrics with the perspective of common reader/user are presented. We believe that this paper will inspire many new perspectives and developments in this area.

An eco-friendly modified methodology for the resolution of binary pharmaceutical mixtures based on self-deconvolution of the UV spectrophotometric spectra in the Fourier domain: Application of Fourier self-deconvolution in UV spectroscopy.

UV spectrophotometry is a rapid and robust technique in resolving several challenging pharmaceutical combinations. Several mathematical treatments are available for the resolution of complex multicomponent UV spectra as; wavelet transformation, derivatization, and deconvolution-curve fitting models. Fourier self deconvolution (FSD) is a mathematical computational methodology for resolving interfering signals in many disciplines and applications. In the current work, we describe a modified FSD based methodology in resolving different binary pharmaceutical mixtures, which overcome the complexity of applying the traditional deconvolution-curve fitting technique on UV spectroscopic spectral data. The current approach differs from the conventional FSD by using the individual spectra of each component as a probing tool to avoid artifacts or errors on the deconvoluted spectra for accuracy of determinations. The utilized approach managed to resolve the binary mixtures of telmisartan/hydrochlorothiazide and ramipril/hydrochlorothiazide in their pharmaceutical dosage forms. The advantage of the current methodology over the traditional deconvolution-curve fitting is the simplicity of application, less time consuming, no need for sophisticated software, and higher sensitivity as revealed by the limit of detection (LOD). The linear ranges for telmisartan, ramipril, and hydrochlorothiazide were 1-25 µg/ml, 5-35 µg/ml, and 1-10 µg/ml, respectively, and the LOD values were in the ranges of 0.067-0.747 µg/ml. The developed FSD approach was validated as per the ICH recommendations regarding the accuracy, precision, linearity, selectivity, and limits of detection and quantitation. The recoveries obtained from the proposed approach were statistically compared with the corresponding reported methods and found no statistical difference between the obtained results.