Analytical Greenness Research Articles

Microextraction experimental and forcefield theoretical modelling study on exploring a silica-enriched oil palm frond biomass for the determination of polycyclic aromatic hydrocarbons in Psidium guajava

In this study, a dispersive micro-solid phase extraction (D-µ-SPE) based on oil palm frond-based silica (OPF-SiO2) sorbent was investigated for the determination of four polycyclic aromatic hydrocarbons (PAHs) in Psidium guajava integrated with high-performance liquid chromatography (HPLC-DAD). The physicochemical characterization of the acid-treated and thermally extracted OPF-SiO2 by FTIR showed peaks at 806 cm−1 and 446 cm−1 allotted to siloxane stretching vibrations and siloxane terminating vibrations, while the FESEM spectrum of EDX analysis corroborated the presence of silicon in OPF-SiO2. Likewise, the XRD diffractograms displayed prominent peaks at 2θ = 24°, indicating a predominantly amorphous silica structure. The XRF analysis further corroborated this result, which revealed that silica constituted 78 % of the major elemental composition. The established optimized condition of D-µ-SPE extraction of PAHs required 60 mg of sorbent, an extraction time of 15 min using acetonitrile as the elution solvent, and a 5 min desorption time. The prepared sorbents exhibited a high affinity for PAHs through van der Waals and hydrogen bonding. The D-µ-SPE was linear between 50 and 5000 µg kg−1 for naphthalene, fluorene, anthracene, and pyrene (R2 = 0.9921–––0.9997). The RSDs were acceptable for intraday (0.65–1.52 %, n = 3) and interday (0.60–1.92 %) analyses, coupled with low detection limits (2.33–4.90 µg kg−1) and satisfactory relative recovery (95.05–108.88 %). The experimental results supported the subsequent forcefield theory calculations for the PAHs and the OPF-SiO2 composite’s interactions. Analytical GREEnness (AGREE) with a metric score 0.60 indicates that the developed approach is green.

A stability-indicating liquid chromatography - diode array detection method for quantification of febuxostat in pharmaceuticals: a recent application to chemometrics based method development and comparative greenness assessment

With an increased demand for anti-gout drugs, the need for a quality-controlled drug product also arises. In this context, a new liquid chromatography method was developed for quantifying febuxostat that integrates chemometrics principles and assesses the method's eco-friendly nature. Systematized risk assessment identified that organic proportion, flow rate, and pH are the critical method variables and were subsequently optimized using a Box-Behnken design. The validation studies were performed using the optimized chromatographic conditions of 80% organic solvent, 1.0 mL/min flow rate, and a pH value of 6.8 on a C-18 column. The analyte eluted at 2.2 min and was monitored at 262 nm using photodiode array detection. After applying the forced degradation conditions, febuxostat degraded from 1.32 to 11.98% of its initial content. Statistical evaluation found that accuracy, precision, detection and quantitation limits, solution stability, and system suitability were acceptable. The lack of interfering degradation peaks ensured the stability-indicating nature of the method and method specificity. The application of three greenness metrics tools, such as the Green Analytical Procedure Index (GAPI), Analytical Greenness (AGREE) metrics, and analytical eco-scale (AES), revealed excellent method greenness. The current chromatographic method is apt for the routine quality control of febuxostat present in pharmaceutical formulations.

Koncept ekološki prihvatljivih hromatografskih metoda - studija slučaja na primeru razdvajanja dronedaron hidrohlorida i njegovih degradacionih proizvoda

Recently, concern about the environmental impact of drug analysis methods has increased significantly. Reversed-phase high-performance liquid chromatography (RP-HPLC), the predominant technique in drug analysis, relies heavily on organic solvents such as acetonitrile, which is known for its chromatographic efficiency, but also for its toxicity and flammability. To address these concerns, it is essential to minimize the use of toxic organic solvents. The aim of this study is to explore greener RP-HPLC modifications and evaluate their applicability in the pharmaceutical industry. Methods were developed for the separation of dronedarone hydrochloride and its degradation products based on experimental design, including micellar liquid chromatography (MLC), b-cyclodextrin (CD) modified RP-HPLC and ultra-high performance liquid chromatography (UHPLC). The eco-friendliness of these methods was assessed using the analytical eco-scale score, green analytical procedure index (GAPI) and analytical greenness (AGREE). AGREE appears to be the most suitable, as it revealed the greatest differences between the compared methods, as well as insights into critical aspects of the methods. UHPLC and b-CD modified RP-HPLC have been shown to be superior to MLC, and both methods can be a good choice, depending on whether the ease of implementation or energy efficiency is considered to be a more important criterion.

Eco-friendly spectrophotometric methods for concurrent analysis of phenol, 2-aminophenol, and 4-aminophenol in ternary mixtures and water samples: assessment of environmental sustainability.

Recently, there has been a high demand for green procedures in analytical chemistry, particularly those utilizing eco-friendly solvents. In this context, three feasible derivative UV spectrophotometric methods namely, derivative ratio-zero crossing spectra (DRZCS), double divisor ratio spectra (DDRS), and successive derivative subtraction coupled with constant multiplication (SDS-CM) were developed to quantify a ternary mixture of phenol (P), 2-aminophenol (2-AP), and 4-aminophenol (4-AP) in real water samples simultaneously, using ethanol as a solvent. The established methods demonstrated a good linear range, covering 2-60 μg mL-1 for P and 2-50 μg mL-1 for 2-AP and 4-AP, in all approaches with a high correlation coefficient (R2 ≥ 0.9995). In compliance with ICH guidelines, the methods exhibited acceptable precision and accuracy, as indicated by good spike recovery with low relative standard deviations. The eco-friendliness of the UV spectrophotometric approach was assessed using analytical eco-scale (AES), analytical greenness (AGREE), and analytical greenness metrics for sample preparation (AGREEprep). These evaluations confirmed the eco-friendliness of the proposed methods in terms of solvents, energy consumption, and waste generation. The proposed procedure proved to be efficient in quantifying each component in laboratory-synthesized mixtures and real water samples, thanks to its simplicity, accuracy, sensitivity, and cost-effectiveness.

Method development and optimization for dispersive liquid-liquid microextraction factors using the response surface methodology with desirability function for the ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry determination of organic contaminants in water samples: risk and greenness assessment.

A simple, cost effective, and efficient dispersive liquid-liquid microextraction method was developed and optimized for the determination of organic contaminants in different environmental water matrices followed by UHPLC-QTOF-MS analysis. In the preliminary experiments, the univariate optimization approach was used to select tetrachloroethylene and acetonitrile as extraction and disperser solvents, respectively. The significant factors influencing DLLME were screened using full factorial design, and the optimal values for each variable were then derived through further optimization using central composite design with desirability function. The optimal conditions were achieved with 195 μL of tetrachloroethylene as the extraction solvent, 1439 μL of acetonitrile as the disperser solvent, and a sample pH of 5.8. Under these conditions, the method provided detection limits ranging from 0.11-0.48 μg L-1 and recoveries ranging from 23.32-145.43% across all samples. The enrichment factors obtained ranged from 11.66-72.72. The proposed method was then successfully applied in real water samples. Only benzophenone was detected in the concentration range of 0.79-0.88 μg L-1 across all the water samples. The calculated risk quotient resulting from benzophenone exposure in water samples showed a low potential risk to human health and the aquatic ecosystem. The method was also evaluated for its environmental friendliness using various metrics tools such as Analytical Eco-Scale (AES), Green Analytical Procedure Index (GAPI), Analytical GREEnness (AGREE), Analytical Greenness for Sample Preparation (AGREEprep), and Sample Preparation Metric of Sustainability (SPMS). Only AES qualified the method as green while it was considered acceptable and sustainable when assessed using SPMS.

Integration of paper-based analytical devices with digital microfluidics for colorimetric detection of creatinine.

Digital microfluidics (DMF) is a platform that enables the automated manipulation of individual droplets of sizes ranging from nanoliter to microliter and can be coupled with numerous techniques, including colorimetry. However, although the DMF electrode architecture is highly versatile, its integration with different analytical methods often requires either changes in sample access, top plate design, or the integration of supplementary equipment into the system. As an alternative to overcome these challenges, this study proposes a simple integration between paper-based analytical devices (PADs) and DMF for automated and eco-friendly sample processing aiming at the colorimetric detection of creatinine (CR, an important biomarker for kidney disease) in artificial urine. An optimized and selective Jaffé reaction was performed on the device, and the reaction products were delivered to the PAD, which was subsequently analyzed with a bench scanner. The optimal operational parameters on the DMF platform were a reaction time of 45 s with circular mixing and image capture after 5 min. Under optimized conditions, a linear behavior was obtained for creatinine concentrations ranging from 2 to 32 mg dL-1, with limits of detection and quantitation equal to 1.4 mg dL-1 and 2.0 mg dL-1, respectively. For the concentration range tested, the relative standard deviation varied from 2.5 to 11.0%, considering four measurements per concentration. CR-spiked synthetic urine samples were subjected to analysis via DMF-PAD and the spectrophotometric reference method. The concentrations of CR determined using both analytical techniques were close to the theoretical values, with the resultant standard deviations of 2-9% and 1-4% for DMF-PADs and spectrophotometry, respectively. Furthermore, the recovery values were within the acceptable range, with DMF-PADs yielding 96-108% and spectrophotometry producing 95-102%. Finally, the greenness of the DMF-PAD and spectrophotometry methods was evaluated using the Analytical Greenness (AGREE) metric software, in which 0.71 and 0.51 scores were obtained, respectively. This indicates that the proposed method presents a higher greenness level, mainly due to its miniaturized characteristics using a smaller volume of reagent and sample and the possibility of automation, thus reducing user exposure to potentially toxic substances. Therefore, the DMF-PADs demonstrated great potential for application in the clinical analysis of creatinine, aiding in routine tests by introducing an automated, simple, and environmentally friendly process.

Green and High Throughput Assay Using 96-Microwell Base to Determine Metformin Hydrochloride in the Tablet Dosage Form.

Metformin (MET) is an oral antidiabetic drug widely used as the primary treatment for type 2 diabetes mellitus (T2DM). While various spectrophotometric assays exist for determining MET in pharmaceutical formulations, they often have limited throughput for quality control purposes. This study describes the validation of a 96-microwell plate spectrophotometer method using charge-transfer complexes (CTCs) with chloranilic acid (CLA) and 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) for the quality control and detected of MET. This reaction was carried out in 96-microwell plates, and the absorbance of the colored complexes of CLA and DDQ were measured at 530 nm and 460 nm, respectively, using an absorbance microplate reader. This study aims to identify and quantify the use of a 96-microwell plate spectrophotometer analytical technique for assessing complicated formulations. The method was successfully used for the quantification of MET in the tablet dosage form. The results showed good correlation coefficients (0.996 and 0.997) with CLA and DDQ, respectively. The present method showed high precision with RSD % not exceeding 2.17%. The accuracy of the method was obtained by recovery percentage, with percentage values less than ±5%. The Analytical Greenness Metric (AGREE) was used to evaluate greenness of the assays. The result show that the microwell assay method is greenness and suitable for handling large samples on a daily used with high throughput analysis. The use of the 96-microwell-plate method is superior to the existing method in terms of simplicity of the procedure, the low economic cost, and its consumption of low amounts of reagents and organic ethanol solvent, making it an environmentally friendly method. Therefore, these advantages make them suitable and rapid alternatives method to current methods for routine metformin analysis in quality control laboratories.

A Novel quality-by-design optimized spectrofluorimetric approach for estimation of the oral synthetic adiponectin receptor agonist AdipoRon in different biological matrices: Compliance with greenness metrics

The current study introduces the first analytical approach for the quantitative analysis of adipoRon, a synthetic adiponectin receptor agonist, using a facile, rapid, sensitive, and green spectrofluorimetric method. Nitrogen-doped carbon quantum dots (N-CQDs) were synthesized by adopting a fast microwave-assisted procedure using accessible and natural substrates (orange juice and urea). The suggested synthetic method produced CQDs with narrow particle size distribution (2–10 nm), high fluorescence stability, and good quantum yield (29.3%). The produced fluorescent QDs were used as fluorescent sensors and were quantitatively quenched by increasing adipoRon concentrations. A two-level full factorial design (22 FFD) was used to identify the most critical experimental factors affecting the relative fluorescence intensity of N-CQDs. The fluorescence quenching of N-CQDs by the drug was measured at 417 nm after excitation at 325 nm. Under the optimized conditions, the quenching of N-CQDs' fluorescent intensity displayed acceptable linearity with the adipoRon concentration range of 5.0–20.0 μg/mL with limits of quantitation and detection of 0.843 μg/mL and 0.278 μg/mL, respectively. Owing to the high sensitivity, the suggested method was efficiently applied for adipoRon estimation in different biological matrices, including spiked human plasma, real rat plasma, and liver homogenate samples with high % recoveries (87.41–103.17%) and low %RSD values (<2.87%). The method's greenness was evaluated using two metric tools, the complementary green analytical procedure index (ComplexGAPI) and the Analytical GREENNESS metric approach (AGREE), and the results showed that the method was excellent green. The proposed methodology was validated according to the ICHQ2 (R1) recommendations.

Ecological assessment and development of analytical methods for concurrent quantification of valsartan and sacubitril: whiteness comparative study based on relative scoring.

Sustainable analytical chemistry is gaining great interest in global environmental pollution control. In addition, valsartan (VAS) and sacubitril (SAB) have been recently approved by the FDA as a fixed-dose combination "LCZ696". It showed efficacy and safety enough to extend its application from heart failure to hypertension control. VAS/SAB dual therapy is considered expensive; however, its prescription has increased significantly worldwide. This prescription increased the demand for developing sustainable analytical methods that simultaneously analyze VAS and SAB. Highly sensitive and selective spectrofluorimetric methods have been developed for this purpose. A synchronous spectrofluorimetric technique was applied. In one method, it was followed by spectral derivatization at the first-order level. The signals were recorded at 230 and 211 nm for VAS and SAB, respectively. Synchronous spectrofluorimetry was coupled to a dual-wavelength mathematical approach in the second method. Signals were derived by subtracting synchronous responses at 241 nm, 226 nm, and 239 nm from the response at 208 nm for VAS and SAB, respectively. Method validation was carried out following ICH guidelines. VAS showed linear calibration curves spanning the range of 60-200 and 80-600 ng mL-1 for the derivative and dual wavelength-assisted approaches, respectively. SAB achieved linear responses in the range of 17-190 and 30-350 ng mL-1 for the first and second methods, respectively. The green profile of the proposed methods was confirmed using the analytical eco-scale (AES), green analytical procedure index (GAPI), and analytical greenness metric (AGREE) tools. The proposed hybrid methods proved highly sustainable through the whiteness RGB 12 algorithm evaluation approach. Whiteness was comparatively assessed for the proposed and reported methods based on relative scoring depending on the parameters of each method. Despite this scoring approach being accurate as a relative score for comparative purposes, it gave rise to underestimated absolute scores. Therefore, to obtain a proper conclusion from the comparative whiteness study, all the methods were ranked according to their whiteness score, illustrating the excellent whiteness ranks of the proposed methods. Upon complete comparison with the reported methods, the suggested ones showed several advantages concerning analytical performance and the greenness level. The proven affordability and simplicity encourage their wide industrial application in developing countries.

RP-HPLC method for quantification of cefotaxime sodium by using design of experiment, a green analytical approach: Analytical method development, validation, and application

The current work integrates design of experiment (DoE) techniques for developing, validating, and quantifying Cefotaxime sodium through RP-HPLC. Four independent factors were considered: flow rate, mobile phase ratio, oven temperature, and injection volume. A full factorial design was applied to optimize the parameters and determine the significant variables. Using the DoE approach, a more environmentally friendly separation and quantification were achieved with the help of the Venusil XBP. C8 column (5 um × 4.6 × 250 mm), a flow rate of 0.8 ml/minute, and a mobile phase ratio consisting of a binary combination of A:B (15:65). The organic phase (A) consisted of acetonitrile, while the aqueous phase (B) consisted of ammonium acetate, and the pH was adjusted to 6.1 with the aid of glacial acetic acid. The injection volume was set at 20 μl, and the elution was performed at a wavelength of 235 nm using a UV detector. The method was validated according to International Conference on Harmonisation guidelines, and it successfully determined the amount of Cefotaxime in Cefotaxime-loaded nanosponges. Tools such as Analytical Greenness metric (AGREE), “National Environmental Method Index” (NEMI), and “Green Analytical Procedure Index” (GAPI) were used to assess the greenness of the proposed method, along with a comparison of the proposed method with other reported HPLC methods. The proposed method proved to be eco-friendly, with better qualitative and quantitative results, as well as greener NEMI and GAPI quadrants. It also achieved a higher AGREE score (0.68) than the reported method (0.44).

Optimization of analytical method greenness scores: a case study of amino acid enantioseparations with carbonated aqueous systems

Analytical and preparative separation techniques, although perceived as less detrimental compared to industrial manufacturing processes, present a substantial concealed environmental threat.

Core-shell molecularly imprinted polymer sensor for enrofloxacin determination in various matrices: a novel, sustainable One Health analytical strategy.

Antibiotics are essential in treating infectious diseases in both humans and animals, and they are also utilized to enhance animal growth. However, their widespread use has led to significant environmental concerns. After administration of antibiotics, a substantial portion of them is excreted by animals, contaminating various environmental compartments. This problem is examined from the One Health perspective which seeks to balance human, animal, and environmental health for the benefit of global well-being. Enrofloxacin (ENR) is a commonly used antibiotic in veterinary medicine. Despite its efficacy in animal health, ENR is not approved for human use due to its associated toxicities. To address ENR detection, a sensor built upon a core-shell molecularly imprinted polymer (MIP) was created for the determination and testing of ENR in different matrices. Offering a miniaturized and reproducible tool for determining antibiotic residues in biological and environmental samples helps in revolutionizing the way we monitor and control antibiotic usage and contamination in various settings. The fabricated sensor demonstrated an optimum response time and functioned effectively across the pH range of 2.0 to 5.0. The potential profile displayed a linear correlation within a varying concentration spectrum of 1.0 × 10-5 M to 1.0 × 10-2 M characterized by a slope of 57.21 mV per decade. Furthermore, a comprehensive assessment of the environmental sustainability of the developed method was carried out using the Analytical Greenness calculator, AGREE algorithm. Lastly, an examination of the method's level of environmental friendliness was pursued using the newly developed RGB12 model to evaluate its "whiteness" level.

Insights into the sustainability of liquid chromatographic methods for favipiravir bioanalysis: a comparative study.

The introduction of favipiravir as a broad-spectrum antiviral agent, particularly in treating influenza and exploring its potential against COVID-19, emphasizes the necessity for efficient analytical methods. Liquid chromatography has emerged as a commonly utilized technique for quantifying favipiravir in biological fluids. However, the environmental and health concerns linked to classical analytical methods mean a transition toward green analytical chemistry is required. This study investigates the environmental impact of 19 liquid chromatographic methods utilized in the bioanalysis of favipiravir. Recognizing the importance of eco-friendly practices in pharmaceutical analysis, the study employs three widely accepted greenness assessment tools: Analytical Eco-Scale (AES), Green Analytical Procedure Index (GAPI), and Analytical Greenness Calculator (AGREE). Moreover, it incorporates a comprehensive evaluation on a global scale utilizing the whiteness assessment tool Red-Green-Blue 12 (RGB 12). The comprehensive evaluation aims to extend beyond traditional validation criteria and considerations of green chemistry, providing insights into the development of practically efficient, eco-friendly and economical analytical methods for favipiravir determination. This study emphasizes the necessity of planning for the environmental impact and overall sustainability of analytical methods before laboratory trials. Additionally, the integration of greenness/whiteness evaluation in method validation protocols is strongly advocated, emphasizing the importance of critical and global evaluations in analytical chemistry.

Greenness assessment of analytical methods for determination of cannabinoids in oils using NEMI, Analytical Eco-Scale, AGREE and GAPI.

The cannabis plant is being increasingly researched due to its numerous therapeutic properties leading to the need for analytical techniques to assess substances present in extracts of the cannabis plant in carrier oils, such as medium chain triglycerides (MCT) oil. Awareness of the environmental impact of activities related to analysis led to the development of greenness assessment metrics. This study aimed to assess the environmental impact of analytical techniques applied in the analysis of cannabinoids in oil using Green Analytical Chemistry metrics. The first phase of the study consisted of a systematic literature review to identify high performance liquid chromatography and ultra high performance liquid chromatographic methods of analysis for cannabinoids in oil. In the second phase, the identified methods were assessed using the National Environmental Method Index (NEMI), Analytical Eco-scale, Analytical Greenness Calculator (AGREE) and Green Analytical Procedure Index (GAPI). Out of 124 identified studies, 8 were considered for the comparative analysis. The identified analytical methods consisted of high performance liquid chromatography (HPLC) using high resolution MS (n = 1), DAD (n = 2), UV (n = 1), UV and MS (n = 2) and MS/MS (n = 2) as detectors. When the analytical methods were assessed using the Analytical Eco-Scale, 7 out of 8 methods achieved a score ranging between 50 and 73, categorising them as acceptable green methods of analysis. One method achieved a total score of 80, categorising the method as an excellent green analysis. The application of Green Analytical Chemistry and respective metrics during the development of analytical methods contributes towards a reduction in the environmental footprint which results from related activities.

MÉTRICAS DA QUÍMICA ANALÍTICA VERDE NA AVALIAÇÃO DE MÉTODO ECOLÓGICO PARA DETERMINAÇÃO DE DEFENSIVOS AGRÍCOLAS POR CLAE-DAD

GREEN ANALYTICAL CHEMISTRY METRICS IN THE EVALUATION OF AN ECOLOGICAL METHOD FOR THE DETERMINATION OF PESTICIDES BY HPLC-DAD. In recent years, the Brazilian government has authorized several agricultural pesticides, increasing the possibility of pollution of different ecosystems and the food consumed by a large part of the population. The analytical determination of pesticides can be carried out using different techniques associated with various methods. Their development and validation have been based on obtaining better reliability, meeting the requirements of environmental legislation, and adapting to the principles of Green Chemistry. Thus, a chromatographic method was developed for the separation and determination of eight agricultural pesticides (aldicarb, ametrine, atrazine, bendiocarb, carbaryl, hexazinone, methiocarb, and methomyl) in compliance with Green Chemistry criteria, using ethanol as the mobile phase, which it is an ecologically less aggressive solvent. The developed method showed efficient separation and excellent results for green analysis metrics with high scores on the Eco-scale and good presentation in the National Environmental Methods Index (NEMI), Green Analytical Procedure Index (GAPI), and Analytical Greenness Calculator Metric (AGREE) pictograms. The validation parameters indicated the linearity of the method with good precision, selectivity, and sensitivity with detection and quantification limits in the ranges of 0.50 to 0.94 mg L-1 and 0.74 to 1.81 mg L-1, respectively.

Cost-effective eggshell-modified LDH composite for caffeine adsorption, cytotoxicity and antimicrobial activity: exploring the synergy and economic viability in search processes.

The rise of pharmaceutical residues poses a serious threat to ecological and aquatic environments, necessitating the development of cost-effective, convenient, and recyclable adsorbents. Given the high global consumption of eggs, a significant amount of waste eggshell is produced. The techniques outlined here aim to manage eggshell waste by transforming it into highly valuable products, addressing the issue of eggshell waste in communities and industries. This approach supports the concept of zero-waste operations to create value-added goods, contributing to sustainable development. In the future, this method of waste management and material recycling may be adopted as an alternative. CaO-based ZnFe-layered double hydroxide (LDH) is identified as an efficient adsorbent for caffeine (COF) residues due to its biodegradability and biocompatibility. We extensively analyzed the synthesized CaO, ZnFe-LDH, and CaO/ZnFe-LDH composites before the adsorption processes using FT-IR, XRD, SEM, EDX, BET surface area, PZC, TGA/DTG, and after the adsorption processes using FT-IR. We investigated factors affecting the adsorption process, such as pH, adsorbent dose, COF concentrations, and time. Six non-linear adsorption isotherm models were studied at pH 7 for the composite and pH 9 for LDH, showing maximum adsorption capacities (q max) of 152.35 mg g-1 for LDH and 194.87 mg g-1 for CaO/ZnFe-LDH. Kinetic studies were also conducted. Interestingly, the MTT assay conducted on WI-38 cells revealed minimal toxicity, with most tests indicating cell viability above 60%. The synthesized CaO, ZnFe-LDH, and CaO/ZnFe-LDH composite exhibit robust antimicrobial properties against two pathogens, including Gram-negative bacteria (Escherichia coli) and Gram-positive bacteria (MRSA). The MIC values for the synthesized materials range from 0.87 to 7 µg mL-1, varying with the microbial species. Two green metrics were applied: the analytical Eco-scale and the Analytical GREEnness Calculator (AGREE).

A sustainable methodology employing the extract of red dragon fruit peel as a fluorescence probe for detection of indigo carmine (E132) in food samples: evaluation of the method's greenness, whiteness, and blueness.

Indigo carmine dye is one of the most widely used dyes in various fields. In this study, the ethanolic extract of red dragon fruit peel (Ex-RDFP) was employed as a green fluorescence probe for measuring the synthetic dye indigo carmine. At a fluorescence excitation of 290.5 nm, the Ex-RDFP exhibits a fluorescence emission band at 341.5 nm. Meanwhile, the indigo carmine dye possesses an absorption spectrum at a maximum peak of 290 nm. Consequently, the fluorescence intensity of the Ex-RDFP was reduced upon the addition of indigo carmine solution due to the inner filter effect mechanism. This quenching in the fluorescence intensity of Ex-RDFP was substantially associated with the indigo carmine concentration at a linear scale of 1.0-7.0 μg mL-1 (r 2 = 0.9993). Furthermore, the limit of detection and the limit of quantitation of the method were found to be 0.209 μg mL-1 and 0.635 μg mL-1, respectively. The optimal analytical conditions, such as solvent used for dilution, pH, reaction time, volume of the reagent, and temperature, were examined and carefully studied. In addition, the proposed method was successfully applied to detect indigo carmine dye in various natural syrup samples, including lemon syrup, apple syrup, cantaloupe syrup, pineapple syrup, and guava syrup, with acceptable recovery values. The method's beneficial sustainability footprint was found by using an extensive greenness analysis that incorporated the modified National Environmental Methods Index (NEMI), the complex Green Analytical Procedure Index (GAPI), and the Analytical Greenness Calculator (AGREE) prep algorithms. In addition, "whiteness" and "blueness" were also assessed with the newly released (Red Green Blue 12) RGB12 and Blue Applicability Grade Index (BAGI) computational methods, emphasizing the benefit of the proposed method in terms of analytical efficiency, sustainability, and economy. The suggested technique is the answer to the worldwide popularity of ecologically conscious solutions by providing a green-and-white substitute for traditional techniques and advancing towards creating more sustainable quality control procedures in the future.

Efficient and eco-friendly detection of gabapentin using nitrogen-doped carbon quantum dots: an analytical and green chemistry approach.

This study presents the development of an eco-friendly and highly selective mitrogen-doped carbon quantum dot based sensor (N-CQDs) for the detection of gabapentin - a commonly misused drug. A detailed characterization of N-CQDs spectral features and their interaction with gabapentin is provided. The optimal conditions for sensing, including pH value, buffer volume, N-CQDs concentration, and incubation time, were established. The results showed excellent fluorescence quenching at 475 nm (λex = 380 nm) due to the dynamic quenching mechanism, and the sensor demonstrated excellent linearity in the 0.5-8.0 μg mL-1 concentration range with correlation coefficients of more than 0.999, a limit of detection (LOD) of 0.160 and limit of quantification (LOQ) of 0.480 μg mL-1. The accuracy of the proposed sensor was acceptable with a mean accuracy of 99.91 for gabapentin detection. In addition, precision values were within the acceptable range, with RSD% below 2% indicating good repeatability and reproducibility of the sensor. Selectivity was validated using common excipients and pooled plasma samples. The proposed sensor accurately estimated gabapentin concentration in commercial pharmaceutical formulations and spiked plasma samples, exhibiting excellent comparability with previously published methods. The 'greenness' of the sensing system was evaluated using the Analytical GREEnness calculator, revealing low environmental impact and strong alignment with green chemistry principles with a greenness score of 0.76. Thus, the developed N-CQDs-based sensor offers a promising, eco-friendly, and effective tool for gabapentin detection in various situations, ranging from clinical therapeutics to forensic science.

Different spectrophotometric methods for simultaneous quantitation of Vericiguat and its alkaline degradation product: a comparative study with greenness profile assessment

Investigations concerning novel drugs and their induced degradation products are necessary for clinical research and quality control in the pharmaceutical industry. Four spectrophotometric techniques have been performed for simultaneous quantitation of Vericiguat (VER) and its alkali-induced degradation product (ADP) without prior separation. Method A is a dual wavelength method (DW) that estimates the absorbance difference at 314–328 nm, and 246–262 nm for VER and ADP; respectively. Method B uses a ratio difference method (RD) to estimate the ratio spectrum’s amplitude difference (DP318-342) and (DP284-292) for VER and ADP; respectively. Method C uses a first derivative ratio method (1DD) to estimate the peak ratio spectrum amplitude of the first derivative at 318 and 275 nm for VER and ADP; respectively. Method D uses the mean centering of the ratio spectra (MCR) to estimate amplitude values for VER and ADP at 337 and 292 nm; respectively. In a concentration range of 5.00–50.00 µg/mL for VER and 5.00–100.00 µg/mL for ADP, the methods were validated following ICH criteria and utilized to estimate VER in bulk and its dosage form. The methods’ greenness was assessed via three tools: the green analytical procedure index (GAPI), analytical eco-scale, and analytical greenness assessment (AGREE).

Greenness, whiteness, and blueness assessment with spider chart solvents evaluation of HPTLC-densitometric method for quantifying a triple combination anti-Helicobacter pylori therapy

Tackling environmental, economic, and practical issues necessitate analytical methods aligned with green and white chemistry principles. This study quantified a challenging combination of three anti-Helicobacter pylori drugs: omeprazole (OMZ), tinidazole (TNZ), and clarithromycin (CLR) using a novel high-performance thin-layer chromatographic approach. The eco-friendly mobile phase comprised a mixture of ethyl acetate and ethanol (6.5:3.5, v/v), with densitometric detection at 290 nm, yielding compact spots for OMZ (Rf 0.27), TNZ (Rf 0.63), and CLR (Rf 0.73). The method demonstrated excellent linearity (r2 > 0.999) over ranges of 0.5–20, 1–50, and 1–25 μg spot−1 for OMZ, TNZ, and CLR, respectively. Method validation showed good precision (<2 %), accuracy (101.94, 100.65, 101.06 %), and the limit of detections (0.161, 0.269, and 0.283 μg spot-1), for OMZ, TNZ, and CLR, respectively. To ensure sustainability, hazardous solvents were replaced with greener alternatives selected using the Green Solvents Selecting Tool and assessed via greenness index spider charts. The greenness evaluation of the developed method achieved a greener National Environmental Method Index (NEMI), and Complementary Green Analytical Procedure Index (ComplexGAPI) quadrants with higher Analytical Greenness Metric (AGREE) (0.81) and lower carbon footprint (0.037) revealing the method's favorable environmental profile. We further applied the concepts of 'blueness' and 'whiteness' assessment using the recently introduced Blue Applicability Grade Index (BAGI) and Red-Green-Blue 12 (RGB 12) algorithms. The high BAGI score (90) indicated excellent applicability, while the RGB12 score (88.9) confirmed cost-effectiveness and sustainability. This novel HPTLC approach offers a rapid, green-and-white alternative to conventional techniques for pharmaceutical analysis.