Green Analytical Chemistry Principles Research Articles

Approach for concurrent detection and removal of diclofenac in wastewater: Integration of MOF with Poly(deep eutectic solvent) imprinting method

Diclofenac in medical wastewater poses a significant threat to the environment and human health. A simple and efficient enrichment strategy has been established for the selective identification and removal for diclofenac in environmental water samples applying MOF based polymeric deep eutectic solvent (Poly(DES)@MOF). Poly(DES)@MOF was synthesized using a surface imprinting method. The components included MOF-199 as the support material, diclofenac as the template, and a deep eutectic solvent (DES) composed of choline chloride and methacrylate (1:2) as the functional monomer. Density functional theory calculated the Gibbs free energy change during the reaction process, confirming that DES improved the binding performance and selectivity of polymer. Related experiments have shown that Poly (DES) @ MOF has high adsorption capacity, reaching equilibrium within 2 h. In real sample experiments, the maximum adsorption capacity of diclofenac in lake water by the extraction device was 19.39 mg·g−1, with an average recovery rate between 99.4 % and 105.8 %. After 5 repeated uses, the performance did not show significant degradation. After evaluating the principles of green analytical chemistry using agree software, the total score was 0.68, reflecting the high greenness of this study. This study combined molecular imprinting technology and computer theory simulation of MOF based and DES mediated polymerization processes to construct an extraction device that was easy to operate and could extract diclofenac from environmental water samples with high selectivity and adsorption capacity. It showed great potential in the field of environmental monitoring and provided a new approach for the detection of other pollutants in the environment.

Eco-friendly spectrofluorimetric determination of peramapanel; application in pharmaceutical dosage forms and spiked human plasma

A rapid and sensitive spectrofluorimetric method has been developed for the determination of perampanel in pharmaceutical preparations (assay method) and human plasma (bioanalytical method). The fluorescent product was measured at an excitation wavelength (λex) 294 nm and emission wavelength (λem) 430 nm. The assay method was validated as per the International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH) Q2(R1) guidelines. For the assay method, the fluorescence intensity versus concentration plot was found to be linear over the concentration range 25–175 ng/mL.In case of bioanalytical method, for the extraction of drug from human plasma, a lucid liquid-liquid extraction method using ethyl acetate was employed. The bioanalytical method was validated according to the United States Food and Drug Administration (USFDA) guidelines and it was applied for the quantification of the drug in human plasma with reasonable accuracy and precision. For the bioanalytical method, the fluorescence intensity versus concentration plot was found to be linear over the concentration range 5–150 ng/mL. The impact of endogenous compounds of the plasma matrix on drug fluorescence was also assessed. To assess the greenness of the developed method, Green Analytical Procedure Index (GAPI) and Analytical GREEnness (AGREE) tools were applied and it was inferred that the developed method adheres closely to the principles of green analytical chemistry.

Risk assessment based on spectrophotometric signals used in eco-friendly analytical scenarios for estimation of carvedilol and hydrochlorothiazide in pharmaceutical formulation

Special attention is given to the pharmacological treatment of combined medication of Carvedilol and hydrochlorothiazide which is the most effective and the most beneficial therapy for hypertensive patients with diabetes and various metabolic comorbidities. This work represents spectrophotometric platform scenarios based on factorized spectrum (FS) using interpoint data difference resolution scenarios (IDDRS) coupled with spectrum subtraction method (SS) for the concurrent quantification of carvedilol (CAR) and hydrochlorothiazide (HCT) when present together in a combination without the need for any initial physical separation steps. This IDD resolution scenario based on manipulating the zero-order spectra (D0) of both drugs in the mixture with various spectral features at different wavelength regions (200–400 nm), region I (220–250 nm), region II (240–300 nm) and region III (270–320 nm) via absorbance resolution (AR) and induced absorbance resolution (IAR) methods coupled with corresponding spectrum subtraction (SS). The calibration curves were established across the linearity ranges of 2.0–12.0 µg/mL at 242.50 nm and 4.0–40.0 µg/mL at 285.5 nm for CAR and 1.0–11.0 µg/mL at 226.10 nm and 2.0–20.0 µg/mL at 270.5 nm for HCT. Moreover, methods’ validation was confirmed via ICH guidelines. A Multicenter comparison between sensitivity, specificity in respect resolution sequence were applied using different wavelength regions with various concentration ranges was applied and finally spectral resolution recommendation is issued and cumulative validation score (CVS) is calculated as an indicator in the risk analysis. In quality control laboratories, the studied approaches are applicable for conducting analysis on the mentioned drugs. In addition, the selection of spectrophotometry aligns with the principles of green analytical chemistry, an approach that resonates with the overarching theme of minimizing environmental impact. Via four metric tools named: analytical greenness (AGREE), green analytical procedure index (GAPI), analytical eco-scale, and national environmental method index (NEMI), methods’ greenness profile was guaranteed.

Carbon-13-isotopomics and metabolomics of fatty acids from triacylglycerols: overcoming the limitations of GC-C-IRMS for short- and medium-acyl chains.

Carbon-13 isotopomics of triacylglycerol (TAG) fatty acids or free fatty acids in biological matrices holds considerable potential in food authentication, forensic investigations, metabolic studies, and medical research. However, challenges arise in the isotopic analysis of short- and medium-chain (C4 to C10) fatty acid methyl esters (SMCFAMEs) through gas chromatography-combustion-isotope ratio mass spectrometry (GC-C-IRMS). The high volatility of these esters results in losses during their preparation, leading to isotopic fractionation. Moreover, the methoxy group added to acyl chains requires the correction of δ13C values, thereby increasing the uncertainty of the final results. Analyzing free fatty acids (FFAs) addresses both issues encountered with SMCFAMEs. To achieve this objective, we have developed a new protocol enabling the isotopomics of individual fatty acids (FAs) by GC-C-IRMS. The same experiment also provides the FA profile, i.e., the relative percentage of each FA in the TAG hydrolysate or its concentration in the studied matrix. The method exhibited high precision, as evidenced by the repeatability and within-lab reproducibility of results when tested on TAGs from both animal and vegetal origins. Compared to the analysis of FAMEs by GC-C-IRMS, the current procedure also brings several improvements in alignment with the principles of green analytical chemistry and green sample preparation. Thus, we present a two-in-one method for 13C-isotopomic and metabolomic biomarker quantitation within quasi-universal TAG compounds, encompassing the short- and medium-acyl chains.

Eco-friendly method by Eco-Scale Assessment for quantification of tinidazole in tablets

Tinidazole (TIN), an antimicrobial, is commonly prescribed for the treatment of giardiasis, trichomoniasis and amoeba infections. It presents a monograph in official compendiums by titration and the literature presents some analytical methods, which mostly use methanol and acetonitrile, options opposed to the principles of Green Analytical Chemistry (GAC) and the current trend in chemical-pharmaceutical analyses. Among the principles of GAC, the generation of less waste, the choice of less toxic reagents and solvents, the use of fewer materials, the assessment of costs involved, faster steps and processes are included. In this context, the objective was to develop and validate an eco-friendly method by spectrophotometry in ultraviolet region (UV) for quantitative evaluation of TIN in tablets. Additionally, the proposed method was evaluated for greenness by the Eco-Scale Assessment (ESA). Purified water and ethanol (90:10, v/v) as a diluent, quartz cubette at 318 nm were used. The method was linear in the range of 7–22 µg/mL (0.9999), precise (RSD < 5 %), selective through sample adjuvants and by the forced degradation, exact (100.47 %) and robust against changes in reading wavelength. As for the greenness of the method, it proved to be a green alternative to quantify TIN in tablets according to the ESA.

Ionic liquid-reinforced Hydroxyapatite@nano-TiO2 as a green platform for Immuno-electrochemical sensing applications

In contemporary society, developing dependable point-of-care (POC) biosensors for the timely detection of cancer markers is crucial. Among various sensor types, screen-printed electrode (SPE)-based sensors, particularly electrochemical ones, stand out as promising candidates for POC applications. Despite ongoing efforts to create numerous SPE-based sensors, there is a continuous pursuit to enhance their sensitivity and analytical capabilities. This study presents an advanced electrochemical sensor designed to sensitively detect the hepatocellular carcinoma (HCC) marker Alpha-fetoprotein (AFP) in saliva. The sensor employs a gold SPE modified with hydroxyapatite, TiO2 nanoparticles, 1-butyl-3-methylimidazolium bis(trifluoromethyl sulfonyl)imide ionic liquid (IL), and AFP monoclonal antibodies. After thorough characterization and optimization using cyclic voltammetry (CV) and differential pulse voltammetry (DPV), the biosensor exhibited a broad detection range (0.01–400 ng/mL), a low limit of detection (LOD) at 0.058 ng/mL, and demonstrated high selectivity, repeatability, reproducibility, and stability. Furthermore, when tested with spiked human saliva samples, the biosensor displayed excellent recovery and robustness, showcasing its potential for noninvasive and POC diagnosis of HCC. In an environmentally conscious evaluation, the biosensor's greenness was assessed using the AGREE metric, yielding a high score of 0.85. This score indicates the biosensor's alignment with the principles of green analytical chemistry, underlining its eco-friendly attributes. This innovative electrochemical sensor contributes to the ongoing efforts for efficient and reliable POC diagnostic tools and aligns with a broader commitment to developing environmentally friendly solutions.

Microplastics in dairy products and human breast milk: Contamination status and greenness analysis of available analytical methods

The prevalence of microplastics (MPs) in food items is of significant concern due to their potential to cause various human health issues when ingested. Milk and dairy products are widely consumed for their nutritional value and have been found to contain MPs, as evidenced by numerous research studies. This review paper examines the current contamination levels of MPs in dairy products and breast milk, as well as evaluates the environmental impact of the analytical methods used for MPs analysis. The highest contamination levels in dairy products and human breast milk have been found up to 2590 MPs/L. Hence policymakers should enforce stringent regulations to ensure food quality. Additionally, it has been noted that existing analytical methods for detecting MPs in dairy products often fail to adhere to the principles of green analytical chemistry, with many scorings below 0.58 on the AGREE scale. These findings emphasize the urgent necessity for the development of rapid and green analysis methods for detecting MPs in dairy products and breast milk.

Sustainable approaches to analyzing phenolic compounds: a green chemistry perspective.

Innovative and eco-friendly methodologies for the determination of phenolic compounds, showing a paradigm shift in analytical chemistry toward sustainability. Phenolic compounds, valued for their diverse health benefits, have historically been analyzed using methods that often involve hazardous solvents and energy-intensive processes. This review focuses on green analytical chemistry principles, emphasizing sustainability, reduced environmental impact, and analytical efficiency. The use of DES, specifically Ch: Chl-based DES, emerges as a prominent green alternative for extracting phenolic compounds from various sources. The integration of UAE with DES enhances extraction efficiency, contributing to a more sustainable analytical approach. Furthermore, the review highlights the significance of DLLME and SPME in reducing solvent consumption and simplifying extraction procedures. These techniques exemplify the commitment to making phenolic compound analysis environmentally friendly. The incorporation of portable measurement tools, such as smartphones, into analytical methodologies is a notable aspect discussed in the review. Techniques like UA-DLLME leverage portable devices, making phenolic compound determination more accessible and versatile. Anticipating the future, the review foresees ongoing advancements in sustainable analytical approaches, driven by collaborative efforts across diverse disciplines. Novel solvents, extraction techniques, and portable measurement methods are expected to play pivotal roles in the continuous evolution of green analytical methodologies for the analysis of phenolic compounds. The review encapsulates a transformative journey toward environmentally responsible and efficient analytical practices, paving the way for further research and application in diverse analytical settings.

Optimization and Evaluation of Potentiometric Sensing Membranes for Vildagliptin Determination: A Sustainable Approach Incorporating Whiteness and Greenness Assessment

In the current environmental context, incorporating green analytical chemistry principles into analytical chemistry analysis shows great promise. In drug analysis, the most important objective is to develop techniques that are cost-efficient, eco-friendly, and of high quality. Our study highlights the novelty of utilizing greenness and whiteness approaches in developing a solid-state electrochemical sensor for Vildagliptin (VILD) detection. The sensor employs potentiometric transduction and underwent a dual-phase adjustment process. Initially, various ionophores were evaluated to enhance sensor specificity, followed by the incorporation of a multi-walled carbon nanotube layer as a mediator for ion-to-electron conversion. The selected ionophore was then employed to complete the assessment of VILD. The linearity range obtained was 1.00 × 10−5 M – 1.00 × 10−2 M with a limit of detection of 7.94 × 10−6 M. This sensor demonstrated effectiveness in the selective determination of VILD in bulk powdered material and pharmaceutical formulations. Environmental impact evaluation was performed using the Green Analytical Procedure Index (GAPI) and the Analytical Greenness Calculator (AGREE), comparing it to a previous method. Additionally, The RGB model assessed both method’s whiteness. Our investigation reveals the proposed method as an excellent eco-friendly approach compared to the reported method.

Alfalfa biomass as a green source for the synthesis of N,S-CDs via microwave treatment. Application as a nano sensor for nifuroxazide in formulations and gastric juice

BackgroundResearchers have investigated different techniques for synthesis of carbon dots. These techniques include Arc discharge, laser ablation, oxidation, water/solvothermal, and chemical vapor deposition. However, these techniques suffer from some limitations like the utilization of gaseous charged particles, high current, high temperature, potent oxidizing agents, non-environmentally friendly carbon sources, and the generation of uneven particle size. Therefore, there was a significant demand for the adoption of a new technology that combines the environmentally friendly aspects of both bio-based carbon sourcing and synthesis technique. ResultsMedicago sativa L (alfalfa)-derived N, S-CDs have been successfully synthesized via microwave irradiation. The N,S-CDs exhibit strong fluorescence (λex/em of 320/420 nm) with fluorescence quantum yield of 2.2 % and high-water solubility. The produced N,S-CDs were characterized using TEM, EDX, Zeta potential analysis, IR, UV–Visible, and fluorescence spectroscopy. The average diameter of the produced N, S-CDs was 4.01 ± 1.2 nm, and the Zeta potential was −24.5 ± 6.63 mv. The stability of the produced nano sensors was also confirmed over wide pH range, long time, and in presence of different ions. The synthesized N, S-CDs were employed to quantify the antibacterial drug, nifuroxazide (NFZ), by fluorescence quenching via inner filter effect mechanism. The method was linear with NFZ concentration ranging from 1.0 to 30.0 μM. LOD and LOQ were 0.16 and 0.49 μM, respectively. The method was applied to quantify NFZ in simulated gastric juice (SGJ) with % recovery 99.59 ± 1.4 in addition to pharmaceutical dosage forms with % recovery 98.75 ± 0.61 for Antinal Capsules® and 100.63 ± 1.54 for Antinal suspension®. The Method validation was performed in compliance with the criteria outlined by ICH. Significance and noveltyThe suggested approach primarily centers on the first-time use of alfalfa, an ecologically sustainable source of dopped-CDs, and a cost-effective synthesis technique via microwave irradiation, which is characterized by low energy consumption, minimized reaction time, and the ability to control the size of the produced CDs. This is in line with the growing global recognition of the implementation of green analytical chemistry principles.

Feasibility of matrix solid-phase dispersion combined with HR-CS FAAS for determination of copper in milk-based infant foods

This study proposes, for the first time, the development of an analytical method using the matrix solid-phase dispersion (MSPD) for extraction of copper from infant formulas and milk-based foods for further determination using high resolution-continuum source flame atomic absorption spectrometry (HR-CS FAAS). MSPD parameters were investigated, and by employing a 0.25 g sample, 0.25 g of diatomaceous earth as a solid support, 1 mol/L HNO3 as the extraction solution, and 1 min of blending, higher agreements with reference values were obtained. The limit of detection of the method was 0.35 µg/g. Accuracy was assessed by comparing the results using the following methods: i) proposed method (MSPD/HR-CS FAAS); and ii) decomposition of samples by microwave-assisted digestion (MAD) and quantification by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS). The MSPD extracts were also quantified using HR-CS GFAAS. No significant difference was found between the results. The agreements ranged from 95 to 103 %, and no significant difference was observed between the results. Copper concentrations ranged from 0.40 to 3.8 μg g−1 using the proposed method, with relative standard deviations lower than 10 %. The proposed method proved to be efficient for the determination of copper in infant formulas and milk powder, offering advantages such quickness, simplicity, low cost, low energy consumption, reduced waste generation (due to the use of an aqueous extraction solution), utilization of materials from renewable sources (diatomaceous earth as a solid support), and minimized analyst exposure when compared to conventional sample preparation methods. These attributes align with the principles of Green Analytical Chemistry.

Sustainable and Biomimetic Methodology for Extraction of High-Value-Added Compounds in Almond Hulls.

Almond trees are the most cultivated nut tree in the world. The production of almonds generates large amounts of by-products, much of which goes unused. Herein, this study aimed to develop a green chemistry approach to identify and extract potentially valuable compounds from almond by-products. Initially, a screening was performed with 10 different Natural Deep Eutectic Solvents (NADESs). The mixture lactic acid/glycerol, with a molar ratio 1:1 (1:50 plant material to NADES (w/v) with 20% v/v of water) was identified as the best extraction solvent for catechin, caffeoylquinic acid, and condensed tannins in almond hulls. Subsequently, a method was optimized by a Design of Experiment (DoE) protocol using a miniaturized extraction technique, Microwave-Assisted Extraction (MAE), in conjunction with the chosen NADESs. The optimal conditions were found to be 70 °C with 15 min irradiation time. The optimal extraction conditions determined by the DoE were confirmed experimentally and compared to methods already established in the literature. With these conditions, the extraction of metabolites was 2.4 times higher, according to the increase in total peak area, than the established literature methods used. Additionally, by applying the multiparameter Analytical Greenness Metric (AGREE) and Green Analytical Process Index (GAPI) metrics, it was possible to conclude that the developed method was greener than the established literature methods as it includes various principles of green analytical chemistry.

Advancing Green Chemistry in Antiviral Therapeutics: A Comprehensive Review.

Cytomegalovirus (CMV) is a prevalent virus across the world that belongs to the family Herpesviridae but remains dormant in the body unless the immune system is compromised. In addition, when the bacterium is compromised without any health risks, the infection spreads from one person to another person through body fluids, such as saliva, blood, etc. Ganciclovir is an anti- viral medication used in treating viral infections, especially in the treatment of CMV in people with acquired immune deficiency syndrome and immunity at risk. The quality control of ganciclovir in industries is carried out by using anti-green solvents in large volumes; these solvents are not safe in consideration of environmental factors and analysts. Also, the waste generation by these solvents causes hazardous effects on the environment. Further, using 12 green analytical chemistry principles promotes the awareness of analytical judgments among the research groups. It is a revolutionary step in the analytical field to enhance the safety of the environment, and analysts, apart from safety, help to control waste production and conserve energy-reducing occupational hazards. Many works have been carried out for the quality control of ganciclovir using different solvents, such as acetonitrile, methanol, etc. Despite this, there are no existing methods with green solvents or procedures to reduce energy and waste generation. Therefore, the purpose of this review is to understand the drug profile of ganciclovir and the methods developed.

Paper-supported polystyrene membranes for micro-solid phase extraction of date-rape drugs from urine: A sustainable analytical approach

BackgroundThe rapid development of micro-solid phase extraction (μ-SPE) procedures with new sorption materials, in particular, based on using natural materials, is currently reported. The production of these sorbents and the entire extraction procedure should support the implementation of Green Analytical Chemistry (GAC) principles. Promising materials are sorbents based on paper, which can be relatively easily modified, among others: by covering it with a polymer membrane. In this work, the practical application of paper-supported polystyrene used in the analysis of urine samples containing selected date-rape drugs (DRD) substances, and evaluation of the entire procedure using GAC metrics is presented. ResultsThe paper-supported polystyrene membranes were successfully fabricated and characterized. The successful polystyrene coating on the paper was confirmed through ATR-FTIR measurements, ensuring even coverage. The μ-SPE procedure using this material facilitated extraction with a throughput of approximately 120 samples per hour in just a few steps. Throughout the research, a mixture of 100 mM acetic acid:methanol:acetonitrile (70:15:15, v/v/v) was selected as an optimal background electrolyte for capillary electrophoresis – mass spectrometry analysis. Validation results of this method demonstrated its suitability, exhibiting good linearity (R2 > 0.95), low limits of detection (3.1–15 ng mL−1), acceptable precision (<15 %), and recovery for all tested analytes. Furthermore, the greenness evaluation conducted with six different metrics: AGREEprep, AGREE, ComplexGAPI, SPMS, hexagonal metric, and WAC indicated the overall eco-friendliness and sustainability of the method, with minor concerns regarding energy consumption. SignificanceThe use of cellulose paper with polystyrene membranes for μ-SPE provides a versatile and eco-friendly extraction method for detecting DRDs in urine samples. The presented work is an example of the use of GAC metrics in the evaluation of the analytical procedure. The optimized PT-μ-SPE/CE–MS method allows for minimized reagent usage and waste production. Moreover, the method proves to be sustainable and efficient for forensic toxicology analysis.

Fast and eco-friendly analytical method to determine bisphenols, parabens, benzophenone-3 and triclosan in human urine by ultra-performance liquid chromatography coupled to mass spectrometry

Bisphenols, parabens, benzophenone-3 and triclosan are synthetic chemicals commonly used in various products such as cosmetics, pharmaceuticals and food items, leading to human exposure through ingestion, dermal contact and inhalation. Once entering the body, they are rapidly absorbed, metabolised, and excreted in urine due to their short half-lives. Recognized as potential endocrine-disrupting chemicals (EDCs), they have raised concerns among researchers and regulatory bodies. In response to the concerns regarding environmental harm and risks, innovative analytical strategies are required based on the new criteria focused on the twelve principles of Green Analytical Chemistry. Therefore, a new methodology for the environmentally friendly, fast, efficient and simultaneous determination of nine potential EDCs in human urine, including three bisphenols (A, F and S), four parabens (methyl paraben, ethyl paraben, propyl paraben and butyl paraben), benzophenone-3 and triclosan, has been developed and validated. It is based on a dilute-and-shoot method and ultra-performance liquid chromatography coupled to tandem mass spectrometry analysis. The relative recoveries ranged from 80 % to 120 % with a precision lower than 20 % for all analytes. The concentration ranges obtained encompass the published levels of the compounds in urine and the limits of quantification were between 0.2 and 0.5 ng·mL−1. The proposed method is the most environmentally friendly and practical so far and it was successfully applied for the determination of these compounds in 20 human urine samples from adults residing in the Valencian Region (Spain), and initial findings suggest that methyl paraben, benzophenone-3 and ethyl paraben were the predominant compounds.

Green synthesis of MIL53(Al)-modified paper-based analytical device for efficient extraction of neonicotinoid insecticides from environmental water samples

BackgroundThere is a need to develop low-cost, reliable and portable devices to enhance the efficiency of microextraction techniques in complex samples. Metal-organic frameworks (MOFs) have proven to be promising sorbents due to their well-documented properties. However, their green preparation and combination with paper-based substrates have not been satisfactorily explored to fabricate sustainable sorptive phases. ResultsIn this work, the hybridization of a paper substrate (as a sustainable support) with MOFs (as a sorptive phase) was carried out by one-pot approach. Concretely, the selected MOF, MIL-53(Al), was in-situ growth onto the paper surface in aqueous solution without the need for high temperature or pressure, thereby aligning with the Green Analytical Chemistry principles. The optimized composite (MIL-53(Al)@cellulose paper) was characterized and evaluated as extraction sorbent for five neonicotinoids (NEOs) (thiamethoxam, clothianidin, imidacloprid, acetamiprid, and thiacloprid). Furthermore, its feasibility was demonstrated by isolating these pollutants from environmental water samples, followed their determination by HPLC coupled to diode array detection. The whole method showed satisfactory analytical performance with recoveries between 86 and 114 %, suitable precision (with RSD lower than 14 %), and limits of detection ranged from 1.0 to 1.6 μg L−1. Besides, the greenness of the method was assessed by application of different existing metrics. The developed extraction device was affordable (<0.08 €/device) and mechanical and chemically stable, being possible its reuse more than 11 cycles, thus demonstrating its suitability for rapid screening of pesticides in environmental samples. SignificanceThis report presents, for the first time, the green synthesis of MIL-53(Al)cellulose paper composite and its application as a sorptive phase for the extraction of NEOs from environmental water samples. We believe that the proposed strategy for fabricating these sustainable paper-based sorptive phases paves the way for further hybridizations with other MOFs or materials. Additionally, it opens up large possibilities for their application in extraction of pollutants or other hazardous compounds in aquatic environments.

Green analytical chemistry-based spectrophotometric techniques for ternary component analysis of pain relievers

BackgroundThe management of pain presents a significant challenge in healthcare, particularly in cases where conventional therapies prove inadequate. In response to this need, this study aims to devise two innovative UV spectrophotometric techniques rooted in the principles of green analytical chemistry for the analysis of Aceclofenac (ACE), Paracetamol (PAR), and Tramadol (TRM) in both bulk and tablet forms.ResultsUtilizing advanced mathematical methodologies such as the double divisor ratio spectra method and area under the curve, the concentrations of these drugs were accurately determined. Validation of the developed methods adhered to the guidelines outlined by the International Council for Harmonisation in the Q2 (R1), revealing linear calibration curves for ACE (8–12 µg/mL), PAR (22.75–35.75 µg/mL), and TRM (2.62–4.12 µg/mL). Furthermore, statistical analyses employing Student’s t test and F test were conducted to ensure the robustness of the proposed method. The evaluation of environmental impact through green metric tools confirmed the eco-friendliness of the proposed methodologies.ConclusionThe assessment performed utilizing green metric tools has substantiated the environmental sustainability of the proposed approach. Thus, this methodology offers accurate and reliable outcomes for the determination of three drugs, as indicated by the complete overlap observed in the zero-order spectra.

Green Surfactant Assisted-Solidified Floating Organic Drop Micro-Extraction (SA-SFODME) for the Preconcentration of Trace Lead with Determination by Flame Atomic Absorption Spectrometry (FAAS)

Determination of trace lead from environmental samples was carried out by solidified floating organic drop microextraction for preconcentration before analysis by flame atomic absorption spectrometry. The determination of lead from environmental samples, even at trace levels, was possible with an ordinary flame atomic absorption spectrometer (FAAS). The lead formed a hydrophobic complex with the anionic surfactant sodium dodecyl benzene sulfonate (SDBS), and this hydrophobic complex was extracted into the 1-dodecanol drop. Parameters affecting analytical performance have been studied. The optimum pH value was 3.5. The optimum sample volume, SDBS concentration, and extraction solvent volume were 75 mL, 50 mM in dodecanol, and 75 µL, respectively. The optimum extraction time was determined as 30 min, the optimum extraction temperature was 45 °C, the optimum mixing speed was 650 rpm and the ideal extraction phase volume was 0.50 mL. Methanol has been shown to be effective when used as a diluent. Using the optimum conditions, the enhancement factor was 106, and the limit of detection (3s) and precision were 3.3 ng/mL and 2.3% (n = 9,15 ng/mL), respectively. The limit of quantification (LOQ) (10s) was 10 ng/mL and the linear working range was 15-100 ng/mL. The accuracy was evaluated by certified reference material analysis. The optimized method was applied to the determination of Pb(II) from environmental water samples. This method follows the principles of green analytical chemistry.

Automated H2O2 monitoring during photo-Fenton processes using an Arduino self-assembled automatic system

A cheap and easy to use Arduino self-assembled automatic system was employed to continuously monitor the hydrogen peroxide consumption during the photo-Fenton degradation of caffeine, selected as model target compound. The automatic system made it possible to measure the H2O2 concentration in the reaction cell via a colorimetric reaction and to take samples for HPLC analysis minimising the operator manual intervention and exposure to UV radiation. The obtained results were compared in terms of LOD and LOQ with H2O2 measurements manually performed using UV–Vis spectrophotometry, evidencing better analytical performance when using the automatic system; LOD and LOQ were respectively 0.032 mM and 0.106 mM for the automatic system against 0.064 mM and 0.213 mM for UV–Vis spectrophotometry. Furthermore, the photo-Fenton treatment was optimised by means of a Design of Experiments (DoE) investigating the effect of added H2O2 concentration, iron concentration and caffeine initial concentration on system performances. The use of the automatic device for such monitoring provided several advantages: automation (with consequent reduction of the workload), measurement increased precision, reduced reagents consumption and waste production in agreement with the principles of Green Analytical Chemistry.

An ecologically sustainable RP-HPLC method for the trinary estimation of phenylephrine HCl, chlorpheniramine maleate, and dextromethorphan hydrobromide using AQbD and degradation studies

The aim of this research was to eventually come up with the simultaneous estimation of Phenylephrine HCl, Chlorpheniramine maleate and Dextromethorphan hydrobromide and its degradant products by Reverse Phase High Performance Liquid Chromatography [RP-HPLC] with green analytical chemistry principles. An Agilent Inertsil ODS 3 (250 mm x 4.6 mm, 5 μm) was used to achieve separation. A 0.45 μm membrane filter was used to filter the solutions. Phosphate buffer and ethanol were employed as the mobile phase. The injection volume was set to 10 μL, the flow rate was set to 1 mL/min and the detection wavelength was set to 220 nm. The gradient elution was used. Phenylephrine HCl had a retention time of 6.8 minutes, chlorpheniramine maleate of 3.5 minutes and dextromethorphan hydrobromide of 12.2 minutes. Phenylephrine HCl, chlorpheniramine maleate and dextromethorphan hydrobromide had linear concentration ranges of 1-6 μg/ml, 1-6 μg/ml, and 2-12 μg/ml, respectively. Phenylephrine HCl, chlorpheniramine maleate and dextromethorphan hydrobromide had correlation coefficients of R2 of 0.999, 0.998, and 0.998, respectively. The method that was developed was environmentally friendly, according to the results of the greenness evaluation tools. Optimized using Central composite design and greenness of the method evaluated using green evaluation techniques.