Volume 44, Issue 1

Analytical chemistry research has shifted towards environmentally friendly substitutes that reduce waste and avoid hazardous substances. These efforts align with broader environmental goals and inspire sustainable and responsible science. The objective of this work is to develop and validate an analytical method and verify its greenness using specific tools, including analytical GREEnness (AGREE), analytical greenness metric for sample preparation (AGREEprep), green analytical procedure index, complex green analytical procedure index, analytical Eco-Scale, analytical method volume intensity, analytical method greenness score, and HPLC-EAT (Environmental Assessment Tool). Effective treatment of chronic cough relies heavily on adequately utilizing salbutamol (SAL) and guaifenesin (GUA) in the presence of sodium benzoate (SOB) preservative. The isocratic elution mode used the Zorbax Eclipse Plus C18 column (15 cm × 4.6 mm, 3.5 µm). It could move 1.5 mL·min −1 , hold 50 µL, have a column temperature of 30°C, and have an autosampler temperature of 5°C. It could detect UV light at 276 nm and had a mobile phase of 80:20 v/v buffer solution and acetonitrile. We have successfully established highly accurate calibration curves for the three components SAL, GUA, and SOB within the optimal range of 2–50 µg·mL −1 . The coefficient of correlation ( r ) for these curves was at an impressive 0.9999 for SAL and GUA, while it was 0.9998 for SOB. The recovery values were 100.15%, 100.47%, and 100.92% for SAL, GUA, and SOB, respectively. The selectivity and sensitivity to the ingredients were confirmed according to the International Council for Harmonisation guidelines, as no interference occurred from any of the used sample components. We implemented Six Sigma, resulting in precision and productivity. Graphical abstract

A bioanalytically validated potentiometric method was proposed for the assay of bisphenol A (BPA) using a MWCNT-modified graphite ion selective electrode. The sensitivity of measurements was significantly enhanced by using MWCNTs as an ion-to-electron transducer layer. A precise linear analytical curve was developed to determine BPA in a specified linear range of 10,000–0.01 μmol·L −1 , with a detection limit of 0.000104 μmol·L −1 . After confirming that the results obtained with the proposed potentiometric sensor are not affected by the presence of possible interferents, the method was successfully applied to determine BPA concentration in different saliva samples, giving good accuracy and precision. Graphical abstract

It is risky for the environment and public health to have antibiotic residues in wastewater from agricultural sources, such as poultry slaughterhouses and rabbit farms. The goal of the present investigation is to use ten sustainability metrics to create an accurate and environmentally friendly high-performance liquid chromatography approach for the detection of oxytetracycline, tetracycline, and cephradine residues in wastewater from poultry slaughterhouses, rabbit farms, and pharmaceutical factories. A mobile phase consisting of phosphate buffer solution pH 4.2 (45%) and 55% methanol was used with a C18 column (4.6 mm i.d., 250 mm, 5 µm, Agilent Co.) to accomplish the separation, with a 1.0 mL·min −1 flow rate and UV detection at 257 nm. The calibration curves exhibited linearity and covered concentration ranges of 2–50, 0.3–10, and 1–45 µg·mL −1 . The correlation coefficient was 0.9999, while accuracy results varied between 85% and 115%. The current work’s accuracy was assessed using the Six Sigma approach, which revealed a process capability index exceeding 1.3%. The latest investigation proposes the Blue Applicability Grade Index, a new technique that improves environmental metrics in real-world analytical chemistry. The procedures underwent effective validation per International Council for Harmonization standards. Graphical abstract

Lead-cooled fast reactors (LFR), such as the ALFRED Demonstrator, are pivotal in advancing nuclear technology. This study presents a method for quantifying trace-level impurities generated through various nuclear reactions in lead coolant. It combines inductively coupled plasma mass spectrometry with Sr-resin-based matrix separation to analyze trace impurities in lead matrices. The Sr-resin effectively removes lead, a highly interfering matrix, enhancing the precision and reliability of detecting trace elements. The study evaluates the effectiveness of lead matrix removal and assesses the method’s reliability for monitoring trace impurities in LFR systems. The results indicate the method’s suitability for tracking small changes in lead composition during the operation of lead-cooled facilities.

A sensitive liquid chromatography–mass spectrometric method was developed to determine three angiotensin-converting enzyme (ACE) inhibitors, enalapril (ENA), ramipril (RAM), and perindopril (PER) at picogram levels in rabbit plasma. The method employs two derivatization reagents: 3-bromomethyl-propyphenazone (BMP) and a hydrazonoyl chloride (UOSA54). These reagents significantly enhanced the detection sensitivity of the analytes, with response factors increasing by 7–114 orders of magnitude compared to underivatized compounds. The ACE inhibitors were extracted from plasma using liquid–liquid extraction and then derivatized with either BMP or UOSA54. The BMP-derivatized analytes were analyzed using positive electrospray ionization-MS (ESI-MS) mode, while the UOSA54-derivatized analytes were analyzed using negative ESI-MS mode. The method demonstrated excellent sensitivity, with limits of quantification ranging from 0.03 to 30 ng·mL −1 for BMP-derivatized analytes and 0.3 to 300.0 ng·mL −1 for UOSA54-derivatized analytes. The calibration curves were linear, spanning a wide range of concentrations, with correlation coefficients ( r 2 ) close to unity for all analytes. The extraction recovery of the developed method ranges from 88% to 100%, outperforming other extraction procedures. The method’s applicability was validated through pharmacokinetic studies in rabbits, where it successfully quantified ACE inhibitors over 24 h post-oral administration. Pharmacokinetic parameters revealed distinct profiles for each ACE inhibitor: ENA exhibited a C max of 45.2 ± 3.1 ng·mL −1 , T max of 0.5 h, and AUC 0–24h of 210 ± 15 ng·h·mL −1 ; RAM showed a C max of 62.5 ± 4.2 ng·mL −1 , T max of 1 h, and AUC 0–24h of 315 ± 20 ng·h·mL −1 ; PER displayed the highest C max (78.3 ± 5.6 ng·mL −1 ), longest T max (2 h), and largest AUC 0–24h (410 ± 25 ng·h·mL −1 ). This method represents a significant advancement in ACE inhibitor analysis, offering unparalleled sensitivity and reliability for pharmacokinetic studies and therapeutic monitoring of these important cardiovascular drugs. Graphical abstract Derivatization of ACE inhibitors with either BMP or UOSA54, followed by liquid chromatography-mass spectrometric analysis.

An innovative green reverse phase high-performance liquid chromatography method was developed and validated for the concurrent quantification of methocarbamol (MTC) and etoricoxib (ETC) in rat plasma using diclofenac potassium as an internal standard. This method introduces significant advancements over existing chromatographic techniques, including a rapid analysis time (8-min run time) and cost efficiency due to low solvent consumption (total solvent use of 444 mL), achieved through optimized chromatographic conditions. The method employs a Hypersil BDS C8 column (4.6 mm × 250 mm, 5 µm) with an isocratic mobile phase (buffer pH 2.5:methanol, 34:66 v/v) at 1.5 mL·min −1 and 274 nm detection. Linearity (1–50 µg·mL −1 , R 2 > 0.999) was demonstrated with sensitive detection limits (LOD = 0.20 µg·mL −1 [MTC], 0.25 µg·mL −1 [ETC] and LOQ = 0.60 µg·mL −1 [MTC], 0.75 µg·mL −1 [ETC]). Environmental sustainability was rigorously confirmed using eight green metrics (AGREE, ComplexGAPI, AMVI), yielding an analytical eco-scale score of 84, surpassing conventional methods in eco-friendliness . In vivo studies on complete Freund’s adjuvant-induced rheumatoid arthritis rats revealed the MTC–ETC combination’s potent anti-inflammatory and anti-arthritic effects, including reduced serum c-reactive protein levels ( p < 0.05) and preserved hepatorenal function. Validated per United States Food and Drug Administration guidelines, this method offers a fast, economical, and eco-conscious solution for pharmacokinetic studies and therapeutic monitoring, positioning the MTC–ETC combination as a promising, safe therapy for rheumatoid arthritis. Graphical abstract

An electrochemical sensor for cinchocaine (CIN) detection was developed based on surface molecular imprinting technology utilizing screen-printed gold electrodes modified with TiO 2 nanoparticles and electropolymerized polypyrrole. A novel sensor was developed using a dual-stage methodology, which entailed initial CIN template immobilization and subsequent electrochemical pyrrole polymerization incorporating titanium dioxide nanoscale particles. The sensor exhibited enhanced electroactive surface area (0.075 cm 2 ) and improved electron transfer kinetics (heterogeneous rate constant 8.2 × 10 −3 cm·s −1 ) compared to unmodified electrodes. Under optimized conditions (pH 5.0, 15-min incubation), the sensor demonstrated two linear response ranges from 0.1–10 and 10–100 μM, with a detection limit of 0.035 μM. The sensor showed excellent selectivity against common interferents, including a 100-fold excess of inorganic ions and a 50-fold excess of structurally similar compounds. Analysis of clinical samples yielded excellent recoveries (97.2–102.3%) with relative standard deviations below 4.3%. The simple fabrication process, rapid response time, and minimal sample preparation requirements make this sensor particularly suitable for point-of-care applications.

The sustainability and effectiveness of the chemical industry are greatly enhanced by white and green chemistry. Ten sustainability tools have been developed based on green and white metrics. Several tools can be used to determine how environmentally friendly, innovative, and forthright reversed-phase ultra-performance liquid chromatography (RP-UPLC) and ultraviolet (UV) techniques can simultaneously analyze and separate metformin (MET) and dapagliflozin (DAP) in pure and dosage forms. In addition to the green analytical procedure index and complex green analytical procedure index, analytical greenness, analytical greenness metric for sample preparation, eco-scale assessment, analytical method greenness score, high-performance liquid chromatography-environmental assessment tool, analytical method volume intensity, RGB12, and blue applicability grade index, several tools can be used to evaluate the effectiveness of these techniques. In the RP-UPLC methods under investigation, the isocratic technique was used to configure the optimal system. For RP-UPLC processes, a Waters XSelect HSS T3 C18 column (10 cm × 0.21 cm, 5 μm) was utilized. The sample and column oven temperatures were adjusted to 5°C and 35°C, respectively. The mobile phase in an RP-UPLC procedure was phosphate buffer and ethanol (55:45, v/v) adjusted to pH 7.0 with a 2 min duration, 2.0 μL injection volume, 0.5 mL·min −1 flow rate, and 225 nm UV detection. The second technique was the mean centering of ratio spectra (MCR) method, efficiently resolving the medications’ spectral overlapping at 257.7 and 240.9 nm for MET and DAP, respectively. For every drug, the correlation coefficient between the calibration curves for the UPLC and MCR techniques was more significant than 0.999. With primary recovery rates varying from 99.5% to 100.9%, the strategy produced good results. A validation process has been initiated pursuant to the principles of the International Council for Harmonisation. Graphical abstract

Combining non-sedating antihistamines (NSAs) with montelukast (MON) has been found to significantly enhance the therapeutic efficacy against daytime and composite nasal symptoms, including rhinorrhea, sneezing, and itching. This article reviews the current analytical methods employed for the identification and quantitative determination of MON in combination with NSAs in various marketed formulations. The most commonly used methods for the determination of MON and NSAs in combination are chromatographic methods (high-performance liquid chromatography [HPLC] and thin-layer chromatography) and spectrometry methods (spectrofluorometry and spectrophotometry). Recent preferences in the analysis of MON and NSAs in combination samples prove the primacy of HPLC (61%) and confirm the general trends moving toward more sensitive methods, with a higher resolution potential, consumption of small quantities of samples and reagents, and requiring less analysis time. Graphical abstract

This review examined various analytical approaches for extracting some persistent organic pollutants (POPs) from environmental and food matrices containing lipid components. The impact of the lipid component on the extraction of such hazardous chemicals from fatty matrices is well-known due to their lipophilicity. The analysis of the scientific literature revealed different approaches, typically characterized by the use of a solvent mixture that leads to the co-extraction of lipid components, followed by one or more laborious clean-up steps to remove the interferents from the matrix. Despite the differences in the approaches used, the observed recoveries are high, >80%. Additionally, it was found that the same technique could extract different contaminants from various matrices, resulting in a loss of selectivity of the method used. The uncertainties suggested in this review consider (i) the actual extraction of POPs with polar solvents (e.g., acetonitrile) from lipid component, for which POPs may have higher retention; (ii) the use of laborious, long cleaning steps (e.g., polar and non-polar adsorbent phases) could affect recoveries; (iii) the absence of studies investigating the concrete and constant distribution of POPs between extractive solvent/lipid component and solvent/adsorbent phase. Further, the recent application of eutectic solvents was discussed as a promising approach towards a green chemistry procedure.

Photocatalysis is expected to solve both energy and environmental problems at the same time. Photocatalysis technology has received increasing attention, and systematically understanding the reaction mechanism of the photocatalytic process is very important for better utilization of solar energy. With the aim of establishing property-performance relationships and discovering the reaction mechanisms, several characterization techniques have been adopted to evaluate the properties of semiconductor photocatalysts, such as UV–visible absorption spectroscopy, photoluminescence spectroscopy, Raman spectroscopy, electrochemical impedance spectroscopy, and cyclic voltammetry. In this review, the principles and characteristics of different characterization techniques are demonstrated with concrete examples to give a clear picture and promote the research of photocatalysis in the future.

In human history, metals have had a significant yet ironic function. Their growing industrial usage has made a significant contribution to technological advancement; on the other hand, their requirement for humans, particularly in situations where certain metal ions are lacking, has just now come to light. In this review, we have examined various analytical methods employed in the detection of lithium, spanning from conventional approaches to contemporary technologies. Traditional methods encompass gravimetric analysis, titrimetry, flame testing, chromatography, and colorimetry. On the other hand, modern techniques involve the utilization of sophisticated instruments such as X-ray diffraction, X-ray fluorescence, atomic absorption spectroscopy, inductively coupled plasma optical emission spectroscopy, inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry, laser-induced breakdown spectroscopy, ultraviolet/visible spectroscopy, X-ray photoelectron spectroscopy, and sensor technology. Graphical abstract

The introduction of ionic liquids has emerged as an effective method to enhance the properties of polymer/filler composites, marking significant progress in creating advanced materials for specialized applications. It is crucial to understand and modify the chemical properties of polymer/filler/ionic liquid composites to improve their performance in various domains. These properties significantly affect the composites’ appropriateness for specific uses. In this short review, various polymer matrices, fillers, and ionic liquids used in these composites are identified. Additionally, the influence of ionic liquids on the composites’ chemical properties, analyzed using Fourier transform infrared (FTIR) spectroscopy, is shortly covered. This review spans a decade of research, covering developments from 2013 to 2023 in polymer/filler/ionic liquid composites. It contributes to a deeper understanding of FTIR absorption spectra of the composites. In summary, the increase in peak intensities in the FTIR spectra of polymer/filler/ionic liquid composites correlates with enhanced general characteristics. Furthermore, wavenumber shifts toward higher values in these composites, relative to neat polymers, indicate improvements in specific properties. These enhancements are attributed to the intermolecular interactions among polymers, fillers, and ionic liquids. Graphical abstract