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.

Efficient and environmentally friendly spectrofluorimetric determination of cariprazine: An analytical and green chemistry approach.

Cariprazine represents a new generation of antipsychotic medication, characterized by its heightened affinity for the D3 receptor. It has recently obtained approval as an adjunctive treatment option for patients diagnosed with major depressive disorder. In this study, a novel approach utilizing fluorescence spectroscopy was developed to analyze cariprazine. The methodology involves the transformation of cariprazine into a fluorescent compound by means of chemical derivatization with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl). Following excitation at 470 nm, the fluorescent derivative displayed peak fluorescence emission at 550 nm. The factors influencing the derivatization process were optimized. Upon reaching the optimal reaction conditions, a linear correlation (r2 = 0.9995) was observed between the fluorescence intensity and concentrations of cariprazine ranging from 20 to 400 ng/ml. Detection and quantitation limits were determined to be 5.85 and 17.74 ng/ml, respectively. The approach was accurate and precise, with percent recovery values ranging from 98.14% to 99.91% and relative standard deviations of less than 2%. Application of the method to the analysis of cariprazine in bulk and commercial capsules forms yielded accurate results. Moreover, adherence to environmentally friendly analytical practices was evident through alignment with the principles of green analysis, as demonstrated by the analytical eco-scale, AGREE, and GAPI greenness assessment tools.

Water as a green solvent for sustainable sample preparation: single drop microextraction of N-nitrosamines from losartan tablets.

Water, renowned for its sustainability and minimal toxicity, is an ideal candidate for environmentally friendly solvent-based microextraction. However, its potential as an extractant solvent in miniaturized sample preparation remains largely unexplored. This paper pioneers using water as the extraction solvent in headspace single-drop microextraction (HS-SDME) for N-nitrosamines from losartan tablets. Autonomous HS-SDME is executed by an Arduino-controlled, lab-made Cartesian robot, using water for the online preconcentration of enriched extracts through direct injection into a column-switching system. Critical experimental parameters influencing HS-SDME performance are systematically explored through univariate and multivariate experiments. While most previously reported methods for determining N-nitrosamines in pharmaceutical formulations rely on highly selective mass spectrometry detection techniques to handle the strong matrix effects typical of pharmaceutical samples, the water-based HS-SDME method efficiently eliminates the interfering effects of a large amount of the pharmaceutical active ingredient and tablet excipients, allowing straightforward analysis using high-performance liquid chromatography with ultraviolet detection (HPLC-UV-Vis). Under optimized conditions, the developed method exhibits linear responses from 100 to 2400 ng g-1, demonstrating appropriate detectability, precision, and accuracy for the proposed application. Additionally, the environmental sustainability of the method is assessed using the AGREEprep methodology, positioning it as an outstanding green alternative for determining hazardous contaminants in pharmaceutical products.

Advances and Applications of Hybrid Graphene-Based Materials as Sorbents for Solid Phase Microextraction Techniques.

The advancement of traditional sample preparation techniques has brought about miniaturization systems designed to scale down conventional methods and advocate for environmentally friendly analytical approaches. Although often referred to as green analytical strategies, the effectiveness of these methods is intricately linked to the properties of the sorbent utilized. Moreover, to fully embrace implementing these methods, it is crucial to innovate and develop new sorbent or solid phases that enhance the adaptability of miniaturized techniques across various matrices and analytes. Graphene-based materials exhibit remarkable versatility and modification potential, making them ideal sorbents for miniaturized strategies due to their high surface area and functional groups. Their notable adsorption capability and alignment with green synthesis approaches, such as bio-based graphene materials, enable the use of less sorbent and the creation of biodegradable materials, enhancing their eco-friendly aspects towards green analytical practices. Therefore, this study provides an overview of different types of hybrid graphene-based materials as well as their applications in crucial miniaturized techniques, focusing on offline methodologies such as stir bar sorptive extraction (SBSE), microextraction by packed sorbent (MEPS), pipette-tip solid-phase extraction (PT-SPE), disposable pipette extraction (DPX), dispersive micro-solid-phase extraction (d-µ-SPE), and magnetic solid-phase extraction (MSPE).

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.

Current green capillary electrophoresis and liquid chromatography methods for analysis of pharmaceutical and biomedical samples (2019-2023) - A review.

Separation analytical methods, including liquid chromatography (LC) and capillary electrophoresis (CE), in combination with an appropriate detection technique, are dominant and powerful approaches preferred in the analysis of pharmaceutical and biomedical samples. Recent trends in analytical methods are focused on activities that push them to the field of greenness and sustainability. New approaches based on the implementation of greener solvents, non-hazardous chemicals, and reagents have grown exponentially. Similarly, recent trends are pushed in to the strategies based on miniaturization, reduction of wastes, avoiding derivatization procedures, or reduction of energy consumption. However, the real greenness of the analytical method can be evaluated only according to an objective and sufficient metric offering complex results taking into account all twelve rules of green analytical chemistry (SIGNIFICANCE mnemonic system). This review provides an extensive overview of papers published in the area of development of green LC and CE methods in the field of pharmaceutical and biomedical analysis over the last 5 years (2019-2023). The main focus is situated on the metrics used for greenness evaluation of the methods applied for the determination of bioactive agents. It critically evaluates and compares the demands of the real applicability of the methods in quality control and clinical environment with the requirements of the green analytical chemistry (GAC). Greenness and practicality of the summarized methods are re-evaluated or newly evaluated with the use of the dominant metrics tools, i.e., Analytical GREEnness (AGREE), Green Analytical Procedure Index (GAPI), Blue Applicability Grade Index (BAGI), and Sample Preparation Metric of Sustainability (SPMS). Moreover, general conclusions and future perspectives of the greening procedures and greenness evaluation metrics systems are presented. This paper should provide comprehensive information to analytical chemists, biochemists, and it can also represent a valuable source of information for clinicians, biomedical or quality control laboratories interested in development of analytical methods based on greenness, practicality, and sustainability.

Lignin-based emulsive liquid-liquid microextraction for detecting triazole fungicides in water, juice, vinegar, and alcoholic beverages via UHPLC-MS/MS.

A universal, green, and rapid lignin-based emulsive liquid-liquid microextraction (ELLME) method was established to detect nine triazole fungicides in water, juice, vinegar, and alcoholic beverages via UHPLC-MS/MS. By employing an environmentally friendly emulsifier (lignin), the proposed ELLME was compatible with more extractants, and not restricted to fatty acids. Due to the high amphiphilic properties and three-dimensional structure of lignin, the emulsion was quickly formed through several aspirate-dispense cycles of the green extractant (guaiacol) and lignin solution. And a micropipette was used for rapid microextraction. The limit of detection was 0.0002-0.0057 µg L-1. The extraction recoveries and relative standard deviation were 81.7%-102.0% and 0.9%-7.1%, respectively. Finally, three green metric tools were used to verify the greenness of the whole procedure. The proposed lignin-based ELLME successfully emulsified green solvents, indicating that emerging solvents may be excellent alternatives as extractants in ELLME for pesticide residue analysis in food samples.

Novel RP-HPLC-DAD approach for simultaneous determination of chlorphenoxamine hydrochloride and caffeine with their related substances.

Ensuring the quality control of active pharmaceutical ingredients is crucial for drug products being introduced into the market. Even for established drugs, it is necessary to maintain a cutting-edge impurity control system. To analyze caffeine and chlorphenoxamine hydrochloride in their binary mixture, as well as theophylline and chlorphenoxamine N-oxide as related substances, a reversed phase-high performance liquid chromatography combined with a diode array detector system was created. The chromatographic separation was conducted using a C18 X-select Waters® column. The mobile phase consisted of 20.0 mM potassium dihydrogen phosphate modified to pH 3 with o-phosphoric acid and methanol. A gradient elution program was adopted at a flow rate of 1.3 mL/min and detected at a wavelength of 222 nm. The present methodology demonstrates a concentration ranging from 2-60, 1-80, 0.5-20 to 0.4-20 µg/mL for chlorphenoxamine hydrochloride, caffeine, chlorphenoxamine N-Oxide and theophylline, respectively. Chlorphenoxamine N-Oxide, being an impurity of chlorphenoxamine was prepared by refluxing intact drug with 5% H2O2 for 24 h at 100 °C. One of the objectives of the analytical community is to promote the adoption of green analysis methods, which involve the development of environmentally friendly techniques. The levels of greenness and whiteness were evaluated using four specific tools: Eco-Scale System, GAPI, AGREE, and RGB tool. Furthermore, we have evaluated the greenness of the analytical method presented and compared its performance and greenness to that of the approach described in the literature. In this study, results from CPX and CAF analysis were compared to those obtained in a previous study. The result shows that there is no notable variation in precision and accuracy. The proposed method was validated in accordance with the requirements of ICH.

Enhancing Sustainable Analytical Chemistry in Liquid Chromatography: Guideline for Transferring Classical High-Performance Liquid Chromatography and Ultra-High-Pressure Liquid Chromatography Methods into Greener, Bluer, and Whiter Methods.

This review is dedicated to sustainable practices in liquid chromatography. HPLC and UHPLC methods contribute significantly to routine analytical techniques. Therefore, the transfer of classical liquid chromatographic methods into sustainable ones is of utmost importance in moving toward sustainable development goals. Among other principles to render a liquid chromatographic method green, the substitution of the organic solvent component in the mobile phase with a greener one received great attention. This review concentrates on choosing the best alternative green organic solvent to replace the classical solvent in the mobile phase for easy, rapid transfer to a more sustainable normal phase or reversed-phase liquid chromatography. The main focus of this review will be on describing the transfer of non-green to green and white chromatographic methods in an effort to elevate sustainability best practices in analytical chemistry. The greenness properties and greenness ranking, in addition to the chromatographic suitability of seventeen organic solvents for liquid chromatography, are mentioned to have a clear insight into the issue of rapidly choosing the appropriate solvent to transfer a classical HPLC or UHPLC method into a more sustainable one. A simple guide is proposed for making the liquid chromatographic method more sustainable.

Deep eutectic solvent for the extraction of polycyclic aromatic compounds in fuel, food and environmental samples.

Polycyclic aromatic compounds (PACs) encompass a wide variety of organic analytes that have mutagenic and carcinogenic potentials for human health and are recalcitrant in the environment. Evaluating PACs levels in fuel (e.g., gasoline and diesel), food (e.g., grilled meat, fish, powdered milk, fruits, honey, and coffee) and environmental (e.g., industrial effluents, water, wastewater and marine organisms) samples are critical to determine the risk that these chemicals pose. Deep eutectic solvents (DES) have garnered significant attention in recent years as a green alternative to traditional organic solvents employed in sample preparation. DES are biodegradable, have low toxicities, ease of synthesis, low cost, and a remarkable ability to extract PACs. However, no comprehensive assessment of the use of DESs for extracting PACs from fuel, food and environmental samples has been performed. This review focused on research involving the utilization of DESs to extract PACs in matrices such as PAHs in environmental samples, NSO-HET in fuels, and bisphenols in foods. Chromatographic methods, such as gas chromatography (GC) and high-performance liquid chromatography (HPLC), were also revised, considering the sensibility to quantify these compound types. In addition, the characteristics of DES and advantages and limitations for PACs in the context of green analytical chemistry principles (GAC) and green profile based on metrics provide perspective and directions for future development.

Optimizing Antimony Speciation Analysis via Frontal Chromatography-ICP-MS to Explore the Release of PET Additives.

Antimony (Sb) contamination poses significant environmental and health concerns due to its toxic nature and widespread presence, largely from anthropogenic activities. This study addresses the urgent need for an accurate speciation analysis of Sb, particularly in water sources, emphasizing its migration from polyethylene terephthalate (PET) plastic materials. Current methodologies primarily focus on total Sb content, leaving a critical knowledge gap for its speciation. Here, we present a novel analytical approach utilizing frontal chromatography coupled with inductively coupled plasma mass spectrometry (FC-ICP-MS) for the rapid speciation analysis of Sb(III) and Sb(V) in water. Systematic optimization of the FC-ICP-MS method was achieved through multivariate data analysis, resulting in a remarkably short analysis time of 150 s with a limit of detection below 1 ng kg-1. The optimized method was then applied to characterize PET leaching, revealing a marked effect of the plastic aging and manufacturing process not only on the total amount of Sb released but also on the nature of leached Sb species. This evidence demonstrates the effectiveness of the FC-ICP-MS approach in addressing such an environmental concern, benchmarking a new standard for Sb speciation analysis in consideration of its simplicity, cost effectiveness, greenness, and broad applicability in environmental and health monitoring.

Microchip isotachophoresis for green and sustainable pharmaceutical quality control: Method validation and application to complex pharmaceutical formulations.

Universal microchip isotachophoresis (µITP) methods were developed for the determination of cationic and anionic macrocomponents (active pharmaceutical ingredients and counterions) in cardiovascular drugs marketed in salt form, amlodipine besylate and perindopril erbumine. The developed methods are characterized by low reagent and sample consumption, waste production and energy consumption, require only minimal sample preparation and provide fast analysis. The greenness of the proposed methods was assessed using AGREE. An internal standard addition was used to improve the quantitative parameters of µITP. The proposed methods were validated according to the ICH guideline. Linearity, precision, accuracy and specificity were evaluated for each of the studied analytes and all set validation criteria were met. Good linearity was observed in the presence of matrix and in the absence of matrix, with a correlation coefficient of at least 0.9993. The developed methods allowed precise and accurate determination of the studied analytes, the RSD of the quantitative and qualitative parameters were less than 1.5% and the recoveries ranged from 98 to 102%. The developed µITP methods were successfully applied to the determination of cationic and anionic macrocomponents in six commercially available pharmaceutical formulations.

Green method by National Environmental Methods Index and Eco-Scale Assessment for evaluation of gatifloxacin-based product by HPLC.

The literature reveals gaps in the availability of green analytical methods for assessing products containing gatifloxacin (GFX), a fluoroquinolone. Presently, method development is supported by tools such as the National Environmental Methods Index (NEMI) and Eco-Scale Assessment (ESA), which offer objective insights into the environmental friendliness of analytical procedures. The objective of this work was to develop and validate a green method by the NEMI and ESA to quantify GFX in eye drops using HPLC. The method utilized a C8 column (4.6 × 150 mm, 5 µm), with a mobile phase of purified water containing 2% acetic acid and ethanol (70:30, v/v). The injection volume was 10 µL and the flow rate was 0.7 mL/min in isocratic mode at 25°C, with detection performed at 292 nm. The method demonstrated linearity in the range of 2-20 µg/mL, and precision at intra-day (relative standard deviation [RSD] 1.44%), inter-day (RSD 3.45%), and inter-analyst (RSD 2.04%) levels. It was selective regarding the adjuvants of the final product (eye drops) and under forced degradation conditions. The method was accurate (recovery 101.07%) and robust. The retention time for GFX was approximately 3.5 min. The greenness of the method, as evaluated by the NEMI, showed four green quadrants, and by ESA, it achieved a score of 88.

Eco-friendly cobalt-doped carbon quantum dots for spectrofluorometric determination of pregabalin in pharmaceutical capsules.

The misuse of pregabalin has become a significant issue over the last decade. Consequently, there is a growing demand for a sensitive and selective method for its determination. In this study, an eco-friendly cobalt-doped carbon quantum dots (CQDs) have been fabricated and applied as nanoprobes for the fluorometric determination of pregabalin. The CQDs were synthesized through mixed doping with non-metallic atoms such as nitrogen and sulfur, and a metal ion, cobaltous ion, via a microwave-assisted method in just 1.5 min. The synthesized Co-NS-CQDs exhibited advantageous characteristics, including rapid response times, compatibility with various pH levels, exceptional detection limits, high sensitivity, and excellent selectivity. The Co-NS-CQDs exhibited a high quantum yield (55 %) relative to NS-CQDs (38 %), with blue emissive light at 438 nm. The assessment of pregabalin was based on its enhancement effect on the native fluorescence intensity of CQDs. The proposed method had a good linearity over the range of 25-250 µg/mL, with a limit of detection of 4.17 µg/mL and a limit of quantitation of 12.63 µg/mL, respectively. The prepared NS-CQDs have been successfully applied for the pregabalin determination in pharmaceutical capsules, with excellent % recovery (98-102 %). The greenness of the developed method has been investigated using different greenness metrics, in comparison with the reported RP HPLC method. The greenness characteristics of the method originated from the synthesis of CQDs, utilizing sustainable, readily available, and cost-effective starting materials.

High-throughput and green optical sensing of thiocyanate in human saliva based on microplates and an overhead book scanner as detector.

An instrumental-free, high-throughput assay has been developed for the quantification of thiocyanate in human saliva. The proposed green method is based on the rapid reaction of the analyte with Fe(III) under acidic pH in a microplates format to form a colored complex that is captured as an image by an overhead book scanner. Optimization included the effects of the amount concentration of Fe(III), acidity and reaction time / complex stability using a total volume of 300 µL per well. Validation towards the matrix effect was focused on the specific application and was performed using both artificial and human saliva. The linearity of the developed assay was up to 500 µM thiocyanate offering a lower limit of quantification (LLOQ) of 30 µM. The green potentials were evaluated by both the Green Analytical Procedure (GAPI) and Blue Applicability Grade (BAGI) indexes. The thiocyanate content in the saliva of non-smoking volunteers ranged between 750 and 1350 µΜ, while elevated concentrations were verified in smoking individuals (1860-3080 µΜ). Statistical agreement with a corroborative method was assessed using the Bland-Altman plot.

Rapid screening of drugs in environmental water using metal organic framework/Ti3C2Tx composite coated blade spray-mass spectrometry.

Simultaneous rapid screening of multiple drugs of abuse in environmental water facilitates effective monitoring and trend assessments. Herein, a novel porphyrin-based metal organic frameworks modified Ti3C2Tx nanosheets (Cu-TCPP/Ti3C2Tx) composite was prepared and utilized as solid-phase microextraction (SPME) coating for the simultaneous analysis of 21 drugs from water samples. The composite was embedded with matrix-compatible polyacrylonitrile binder to prepare a coated blade with thin and uniform coating layer. Ambient mass spectrometry (MS) technique was used to create a coated blade spray-MS (CBS-MS) method for the quantitative determination of drugs in water samples. High throughput and automated sample preparation were achieved with the use of a Concept 96-well plate system, enabling analysis of 21 drugs of abuse within 1 min per sample, while using only 8 µL of organic solvent for desorption and CBS-MS detection. The developed method showed favorable linearity (R2 ≥ 0.9983) in the range of 0.05 to 10 ng mL-1, low limits of detection (1.5-9.0 ng L-1), sufficient recovery (67.6-133.2%), as well as satisfactory precision (RSDs≤13.5%). This study not only delivers a novel and efficient SPME coating composite, but also demonstrates the excellent performance of a high-throughput, efficient, and green analytical method for determination of drugs in environmental water.

Search for new green natural solid phases for sample preparation for PAHs determination in seafood samples followed by LC and GC-MS/MS analysis.

Polycyclic aromatic hydrocarbons (PAHs) are carcinogenic organic pollutants found in various environments, notably aquatic ecosystems and the food chain, posing significant health risks. Traditional methods for detecting PAHs in food involve complex processes and considerable reagent usage, raising environmental concerns. This study explores eco-friendly approaches suing solid phases derived from natural sources in matrix solid phase dispersion. We aimed to develop, optimize, and validate a sample preparation technique for seafood, employing natural materials for PAH analysis. Ten natural phases were compared with a commercial reference phase. The methodology involved matrix solid phase dispersion and pressurized liquid extraction, followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). Three solid phases (perlite, sweet manioc starch, and barley) showed superior performance in LC-MS/MS and were further evaluated with gas chromatography-tandem mass spectrometry (GC-MS/MS), confirming perlite as the most effective phase. Validation followed Brazilian regulatory guidelines and European Community Regulation 2021/808/EC. The resulting method offered advantages in cost-effectiveness, reduced environmental impact, cleaner extracts, and enhanced analytical performance compared to the reference solid phase and LC-MS/MS. Proficiency analysis confirmed method reliability, with over 50% alignment with green analytical chemistry principles. In conclusion, this study developed an environmentally sustainable sample preparation technique for seafood analysis using natural solid phases, particularly perlite, for PAH determination.

Exploring the potentialities of a biodegradable polymeric film in sample preparation: An optimized "white" protocol to extract and quantify emerging contaminants in water.

BACKGROUND: The introduction of white analytical chemistry encourages the development of methods characterized by a balance among greenness, productivity/feasibility and analytical performances. In the environmental analysis of emerging contaminants (ECs), for which high sensitivity and specificity are mandatory, the use of green and sustainable sample preparation needs to be coupled to a reliable analytical determination. Herein, an extraction method based on the use of a biodegradable polymeric film (Mater-Bi) and coupled to LC-MS/MS analysis was developed for the sensitive determination of ECs in wastewater. RESULTS: The interaction among a range of ECs and the Mater-Bi film (a commercially available patented blend of polybutylene-terephthalate, starch and fatty acids) was investigated by two sequential experimental designs, to simultaneously study several factors and optimize extraction efficiency. The final method, resembling a fabric phase sorptive extraction, involved pH and ionic strength modification of the sample, 1h extraction and desorption in ethanol. Satisfactory recoveries from real wastewater were obtained for sixteen analytes (56-116 %), as well as excellent precision (inter-day relative standard deviations below 10 % for most compounds). Matrix effect was in the range 88-116 % at the lower pre-concentration factor, but also acceptable in most cases at the higher pre-concentration factor. LODs in matrix, from 0.004 to 0.159 µg L-1, were lower than or comparable to those from recent studies employing green extraction procedures. The method demonstrated its applicability to samples from wastewater treatment plants, allowing quantification of pharmaceuticals and UV filters at the µg L-1 and ng L-1 levels, respectively. SIGNIFICANCE: For the first time, the synthetic biopolymer Mater-Bi, so far unexplored for the use in analytical chemistry, was exploited for a green, simple and extremely cheap extraction protocol. The optimized method is suitable for several ECs, guaranteeing very good accuracy, precision and specificity, also thanks to the LC-MS/MS analysis. The evaluation by green and white analytical chemistry metrics highlighted its superiority to conventional extraction methods.

A technique based on infrared spectroscopy for determining sulfanilamide levels sustainably: Progress and comparisons of greenness and whiteness using ComplexGAPI, AGREE, and RGB.

The study aimed to determine the potential of the infrared (IR) spectrophotometric technique for measuring the content of sulphanilamide with the sulfonamide group. The study aimed to obtain the IR spectra of sulfanilamide and use the -SO2 band at 1114.37 for the quantitative assay, determining its area under the curve (AUC). The study gives an alternative approach to existing analytical techniques that require vast amounts of organic solvents, which are costly and can be toxic, thus impacting the environment and increasing the analysis cost. The study evaluated the method's whiteness and greenness by utilizing the Complex green analytical procedure index, analytical GREEness calculator and Red Green Blue algorithm tool. The linierity was found to be 5 to 30 µg/ml. The present study has developed an infrared (IR) spectroscopic method that employs a straightforward sample preparation technique in methanol. The IR spectroscopic method's linearity range was determined to be 5-30 µg/ml. The p-value was 0.001 at 95 % confidence level assuring better recovery. This method is evaluated according to the Q2R1 ICH guideline. It is applicable to routine quality control analysis without pre-extraction using green IR spectroscopy. In conclusion, the study demonstrated that IR spectrophotometric techniques can quantify sulfanilamide while reducing the use of organic solvents, contributing to the green-and-white analytical chemistry approach. The developed methods are reliable, accurate, and cost-effective and have the potential to be implemented in routine analysis of sulfanilamide.