Green Procedure Research Articles

Green analytical quality by design RP-HPLC technique with fluorimetric detection for simultaneous assay of cinnarizine and dompridone.

A green and sensitive factorial design-assisted reversed-phase high-performance liquid chromatography (RP-HPLC) approach with fluorimetric detection has been developed for simultaneous determination of cinnarizine and domperidone in pure materials, commercial single and combined tablets. Both drugs are co-formulated in one dosage form and are commonly used for the effective treatment of motion sickness in the ratio of 4 : 3 for cinnarizine and domperidone, respectively. To achieve the developed method's best performance and reliability, a 23 full factorial design was applied during the optimization of chromatographic conditions. Subsequently, isocratic elution on a C18 column with a mobile phase mixture of methanol and 0.02 M potassium dihydrogen phosphate buffer (85 : 15 v/v, pH 3.0) was performed to achieve the best separation. Moreover, the flow rate of 0.8 ml min-1 was applied during the analysis with fluorescence detection at λex 283 nm/λem 324 nm. The elution process was time effective; it consumed less than 6 min for a complete run as retention time for cinnarizine and domperidone, was 4.5 and 3.5, respectively. Good linearity of the proposed method was achieved within the concentration ranges of 0.2-4.5 and 0.4-5.0 µg ml-1 for domperidone and cinnarizine, respectively. The suggested approach was carefully validated according to the International Council for Harmonization (ICH) guidelines. Moreover, green analytical procedure index (GAPI), national environmental methods index (NEMI), analytical greenness (AGREE) and analytical eco-scale methods were applied to assess and confirm method greenness.

Sensitive and rapid determination of tetracycline antibiotic by carrot juice-derived carbon dots as a fluorescent probe.

The antibiotic tetracycline can be efficiently used as medicine for the deterrence of bacterial infections in humans, animals, and plants. However, the unprecedented use of tetracycline is of great concern owing to its low biodegradability, extensive usage, and adverse impacts on the environment and water quality. In this study, a sensitive spectrofluorometric method was proposed for the direct determination of tetracycline, based on biocompatible fluorescent carbon dots (CDs). The synthesis of CDs was performed by adopting a green hydrothermal procedure from carrot juice without requiring surface passivation or outflowing any environmentally hazardous waste. X-ray diffraction analysis and transmission electron microscopy revealed amorphous spherical-shaped CDs that exhibited blue emission under blue illumination. The fabricated fluorescent probe directly detected tetracycline in the concentration range of 4.00 ×10-6 to 1.55 ×10-5mol L-1 with an LOD of 1.33 ×10-6mol L-1. The performance of the probe was assessed in a tap water sample, with recovery values between 80.70 and 103.60%. The method's greenness was evaluated using the Analytical Green metric approach (AGREE) and confirmed to be within the green range. The developed method is facile, rapid, cost-effective, and offers a wide linear range and satisfactory selectivity, making it potentially suitable for determining tetracycline in water applications.

Bridging Pharma and Sustainability: Green Electrochemical Analysis of Antiparkinsonian Drug in Pharmaceuticals and Plasma, Aligned with United Nations Goals via the NQS Index

This study presents a sustainable electrochemical investigation of pramipexole (PRA) in pharmaceuticals and human plasma, using cyclic and differential pulse voltammetry. Key parameters, including potential range, buffer pH, accumulation period, and scan rate were optimized, establishing efficient voltammetric methods for PRA analysis. The analytical range was 0.60–12.00 μg ml−1, with a detection limit of 0.14 μg ml−1 and a correlation coefficient of 0.9998. Recovery rates for PRA ranged from 98.60 ± 0.26% to 101.33 ± 0.38%, validating the methodology’s applicability in human plasma with an average recovery of 99.25 ± 0.45%. The study highlights the environmental sustainability of the developed voltammetric electrode, evaluated through SWOT analysis, and assesses the greenness impact using tools like Complementary Green Analytical Procedure Index (ComplexGAPI), Analytical greenness (AGREE) and Analytical greenness for sample preparation (AGREEprep). Significantly, this work aligns with numerous United Nations Sustainable Development Goals (UN-SDGs), specifically goals 3, 4, 5, 7, 9, 11, 12, 13, 14, 15, and 17, illustrating our commitment to sustainable pharmaceutical research. The sustainability of the method was further quantified using the newly introduced Need, Quality, Sustainability (NQS) index, demonstrating significant alignment with sustainable analytical practices.

QbD green analytical procedure for the quantification of tolvaptan by utilizing stability indicating UHPLC method

For the first time a new QbD-assisted green stability indicating ultra-high-performance liquid chromatography (UHPLC) method was developed and validated for quantifying Tolvaptan. The method is simple, quick, cost-effective, and stable, and it was used to formulate a quality target product profile (QTPP) with strategically defined critical analytical attributes (CAAs) to meet specific criteria. Chromatographic separation was undertaken using a 10 cm long column of ACE excel super C18 with an interior diameter of 2.1 mm and particle size of 1.7 µm. The analysis was performed under controlled conditions at 25 ℃ with the mobile phase flowing at a rate of 0.2 mL/min and detection occurring at 220 nm. Injected 3 µL of standard by using an isocratic mobile phase system consisting of acetonitrile and water in a 95:5 v/v ratio. The diluents, prepared by mixing acetonitrile with water at a 90:10 volumetric ratio, were utilized. The analyte’s retention time was determined to be 1.63 min. The developed method provided reliable results with accuracy exceeding 99% and a correlation coefficient exceeding 0.999 ranged between 10 and 150 µg/mL across the range for LOQ—150% levels. Notably, during forced degradation testing, Tolvaptan exhibited susceptibility to acidic hydrolysis. The method effectively separated degradation products during stress testing, demonstrating its stability-indicating status. Environmental sustainability assessment of the developed method was conducted through the investigation of various indicators of Complex GAPI, Analytical Eco scale and Analytical GREEness and it was concluded the optimized method aligns with environmentally friendly practices.

A total scoring system and software for complex modified GAPI (ComplexMoGAPI) application in the assessment of method greenness

Evaluating analytical methods with innovative metrics is essential to ensure the effectiveness of analytical procedures. Various approaches have been proposed to assess the performance of an analytical method and its environmental consequences, as sustainable environment and green chemistry ideology are of high importance nowadays. Considering greenness evaluation of developed analytical procedures, Green Analytical Procedure Index (GAPI), one of these metrics, utilizes five distinct colored pentagons to evaluate the environmental footprint of the analytical process at different stages. An additional tool named Complementary Green Analytical Procedure Index (ComplexGAPI) was introduced to expand on GAPI by adding additional fields pertaining to the processes performed prior to the analytical procedure itself. Nevertheless, the existing ComplexGAPI lacks a comprehensive scoring system for individual methods, which would allow for even easier comparison of procedures using this tool. In response to queries from ComplexGAPI users, this study introduces a refined tool named ComplexMoGAPI, merging the visual appeal of ComplexGAPI with precise total scores. The accompanying software streamlines the application, facilitating quicker and simpler evaluations. This software is available as an open source on bit.ly/ComplexMoGAPI. We believe that, following ComplexGAPI success, this ComplexMoGAPI tool will also gain attention and eventually trust and acceptance from the chemical community.

Ecofriendly UPLC-MS/MS method for simultaneous assay of veterinary drugs residues; erythromycin, sulfadiazine and trimethoprim in edible chicken tissues, evaluation of method greenness and whiteness

Antibiotics are the key veterinary drugs used in animal food production. The uncontrolled widespread use of antibiotics may lead to the accumulation of their residues in foodstuff such as milk, eggs, meat and muscles. An Ultra-performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) method was developed for simultaneous determination of triple combination of erythromycin thiocyanate (ERY), sulfadiazine sodium (SFD) and trimethoprim (TMP) in their dosage form and in different chicken tissues including muscles and liver samples. A Simple extraction and cleaning up procedure was applied using 0.1 N EDTA and methanol to remove the interfering substances and hence increase the efficiency of chromatographic separation. Moreover, separation was performed within 1.2 min on Agilent Poroshell 123EC-C18 column using a mobile phase mixture of methanol: water (90:10, v/v), at a flow rate of 0.5 mL/min using quadrupole tandem mass spectrometer detector. The method was validated according to Food and Drug Administration (FDA) guidelines and linearity was achieved in the range of 2.5–1000 ng/mL for ERY and TMP and in the range of for 5–2000 ng/mL for SFD using tamsulosin (TAM) as an internal standard. All the validation results were within the acceptable ranges. Moreover, Three green metric systems including Green Analytical Procedure Index (GAPI), Analytical Eco-Scale and Analytical GREEnness (AGREE) were used to assess the greenness of the developed method. As well as, the novel blue applicability grade index (BAGI) tool was applied to evaluate the practicality of the method. Results of these tools proved the low environmental impact of the method regarding solvent consumption, analysis time, amount of sample needed, sample treatment procedure, and waste product. The developed method has the privilege of high sensitivity and selectivity as well as short analysis time; hence it can be used to test the presence of the residues of studied drugs in various marketed meat samples to assure human safety and maintain public health. Moreover, it is the first developed method for their analysis in liver samples.

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.

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.

Efficient separation of catechyl lignin from castor seed coats via molten salt hydrate

The excellent acid-resistant property of catechyl lignin (C-lignin) allows for its isolation from biomass with intact structure, making it an “ideal lignin” for valorization. In this study, an effective method was developed to separate C-lignin from castor seed coats using acidic molten salt hydrate of LiBr (LiBr-AMSH). Under recommended conditions (60 wt% LiBr solution with 60 mM HCl, 150 °C, and 1 h), 96 wt% of solid sample (based on Klason lignin in castor seed coats) was obtained. Structural characterization indicated that isolated C-lignin consisted of 99 % benzodioxane (BD) structures. Additionally, the optimal conditions led to the achievement of a C-lignin yield of 12.8 wt% (based on raw material), demonstrating a notable accomplishment in terms of productivity. This study provides a green and efficient procedure for extracting C-lignin from castor seed coats while paving the way for valorization.

Sustainable HPLC technique for measurement of antidiabetic drugs: Appraisal of green and white metrics, content uniformity, and in vitro dissolution

Abstract Green chemistry and white chemistry are two approaches to chemistry that prioritize sustainability and environmental protection. The pursuit of green chemistry is to develop chemical processes and products that decrease or stop the use and generation of dangerous materials. In contrast, white chemistry focuses on developing energy-efficient, sustainable chemical processes that produce minimal waste. Our study evaluated the environmental friendliness of the suggested approach, using eight greenness appraisal techniques, including analytical eco-scale, analytical method volume intensity, HPLC-environmental assessment tool, analytical method greenness score, analytical greenness, analytical greenness metric for sample preparation, green analytical procedure index, and complexgreen analytical procedure index, in addition to the unique metric blue applicability grade index of white chemistry. We have developed and validated a highly effective and reliable method for concurrently analyzing designated pharmaceutical medications characterized in metformin (MET) and empagliflozin (EMP) formulations, including their degraded products. This method is cost-effective, specific, and environmentally friendly, utilizing reversed-phase high-performance liquid chromatography with an XBridge BEH C8 column (150 mm × 4.6 mm, 5 μm) at a flow rate of 1.0 mL·min−1, an injection volume of 5.0 μL, a column oven temperature of 50°C, a wavelength of 224 nm, and a mobile phase comprised of phosphate buffer adjusted at pH 6.8 and acetonitrile in gradient mode. In the HPLC method, linearity has been achieved over the concentration range of 10–106 and 30–1,050 µg·mL−1 for EMP and MET, respectively, with correlation coefficients more than 0.999 and good recoveries within 98–102%. An assessment of the content uniformity of finished products confirmed that they met the declaration’s acceptance standards (85–115%). A comparative study has been successfully conducted on generic and reference products, demonstrating their similarity. The suggested approach was validated by adhering to international council for harmonisation criteria.

Cutting-edge HPLC and MCR techniques for synchronically quantifying anticholinergic drugs in the presence of C12 and C14 homologs: Robust application to green and white chemistry.

Green and white chemistry are vital to revolutionizing the chemical industry through their unparalleled potential to enhance sustainability and efficiency. In this study, nine sustainability tools of both green and white metrics, including green analytical procedure index (GAPI), ComplexGAPI, analytical greenness, analytical greenness metric for sample preparation, Analytical Eco-Scale (ESA), analytical method greenness score, high-performance liquid chromatography- environmental assessment tool (HPLC-EAT), analytical method volume intensity, and blue applicability grade index (BAGI), have been developed for appraising environmental friendliness for both innovative and straightforward mean centering of ratio spectra (MCR) and reversed-phase high-performance liquid chromatography (RP-HPLC)strategies utilized for concurrent analysis and separation of cyclopentolate (CYC) and C12 and C14 homologs of benzalkonium chloride (BNZ) in pure and ophthalmic solution. The mobile phase, formed of buffer phosphate and acetonitrile (35:65, v/v), was adjusted to pH 6.3, and 215-nm UV detection was used. The experimental flow rate was 2.0 mL min-1, and the analytical column was L11 Inertsil Ph-3 (150 mm × 4.6 mm, 5 µm). All sequences were run at 25°C in the column oven. The MCR approach effectively resolved the drug's spectral overlapping. CYC and BNZ employed this approach at 227.5 and 220.4 nm, respectively. As part of the HPLC analysis, an isocratic method was employed with phosphate buffer and acetonitrile in the mobile phase at 35:65. A correlation coefficient greater than 0.999 was observed between the calibration curves for the HPLC and MCR methods in the ranges of 20-320 µg mL-1 and 5-30 µg mL-1 for all drugs. The technique yields excellent primary recovery rates, ranging from 97.2% to 100.5%. The recommended approach has been validated according to International Council for Harmonizationguidelines.

A practical and eco-friendly method for the determination of polycyclic aromatic hydrocarbons in açaí-based food products by vacuum-assisted sorbent extraction coupled to gas chromatography-mass spectrometry

For the first time, a method for the simultaneous analysis of fifteen polycyclic aromatic hydrocarbons (PAHs), including light and heavy PAHs, in açaí-based food products (AFPs) was developed using vacuum-assisted sorbent extraction (VASE) combined with gas chromatography-mass spectrometry (GC–MS). The method requires no organic solvents and is amenable to full automation. To achieve optimal analytical extraction conditions, VASE parameters including stirring rate, extraction time, desorption temperature, desorption time, preheat time, and preheat temperature were optimized using sequential multivariate optimization. The method was validated and yielded limits of quantification below 1 µg kg−1 for all analytes, with recoveries ranging from 65 % to 112 % and good precision (≤11 % relative standard deviation). Additionally, the greenness and practical aspects of the method were investigated using the Green Analytical Procedure Index (GAPI), eco-scale, and the Blue Applicability Grade Index (BAGI), respectively. The VASE-GC–MS approach is suitable for routine analysis and exhibits characteristics of a green analytical method. No PAHs were detected above the limits of detection in thirty samples of AFPs.

Anisaldehyde-based deep eutectic solvent dispersive liquid–liquid microextraction (DES-DLLME) followed by UPLC–MS/MS for simultaneous determination of selected parabens and bisphenols in food products: Method development and assessment of the ecological implications

A rapid and environmentally friendly method based on dispersive liquid–liquid microextraction (DLLME) technique, coupled with UPLC–MS/MS analysis was employed for simultaneous determination of selected bisphenols and parabens residues in food products. In this research, anisaldehyde and decanoic acid with a molar ration of 3:1 was prepared as a natural deep eutectic extracting solvent. Various extraction parameters such as the volume of the natural deep eutectic solvent, vortex duration, centrifugation duration, sample volume and pH were systematically explored and optimized. Determination coefficients of ≥0.9990 were achieved for the analyzed compounds under the optimal conditions. The limits detection were in the range of 0.0005 to 0.02 µg/L, while extraction recoveries ranged from 97.8 % to 100.2 % with relative standard deviations (%RSD) not exceeding 6.8 %. To assess the practical applicability of the proposed method, it was employed for the determination of five parabens and three bisphenols in eighty food products including soft drinks, energy drinks, sauces and juices collected from the Saudi market. The environmental implications of the proposed method were assessed using the following evaluation tools, Eco-Scale Assessment (ESA), Green Analytical Procedure Index (GAPI) and Analytical GREEnness metric (AGREE). To the best of our knowledge, this is the first study to determine the investigated analytes using anisaldehyde based deep eutectic solvent.

Nickel and Oxo-Vanadium Complexes of Adenine on Modified Mesoporous MCM-41 as Chemoselective, Efficient, and Reusable Catalysts in the Oxidation of Sulfides and Oxidative Coupling of Thiols.

A highly efficient superior catalyst of Ni (II) and VO (IV) metal complexes supported on MCM-41 has been synthesized and developed for chemoselective oxidation of sulfides to sulfoxides and oxidative coupling of thiols to their corresponding disulfides using H2O2 as a green and efficient procedure. All sulfoxides and disulfides were obtained in short reaction times with excellent yields. The over-oxidation of sulfides or thiols was not observed and all products were synthesized in high purity. These catalysts could be recovered and reused several times without any significant loss in their catalytic activity. Compared to the old catalysts in the literature, these catalysts showed better activity and selectivity for the synthesis of sulfoxide and disulfide derivatives, which shows the novelty of this work. At first, the mesoporous MCM-41 was synthesized, and further, its surface was modified by (3-chloropropyl)-triethoxysilane (CPTES). Then, the modified MCM-41 (nPrCl-MCM- 41) was functionalized by adenine. In the next step, the functionalized MCM-41 (6AP-MCM- 41) was used as support for the immobilization of nickel and oxo-vanadium as final catalysts (Ni-6AP-MCM-41 or VO-6AP-MCM-41). The structure and properties of these catalysts have been identified by XRD, SEM, TGA, FT-IR, and AAS spectral analyses. These catalysts were used in the chemoselective oxidation of sulfides and oxidative coupling of thiols. These complexes catalyzed all reactions well at room temperature. According to the results obtained, the hydroxyl groups of some derivatives, including 2-(methylthio) ethanol or 2,2-(phenylthio) ethanol, remained unchanged during the reaction. The method has been found to possess the advantages of low cost, high efficiency, high yields, recovery, and reusability for several runs without significant loss in the catalytic activity.

Bioinspired Carbon Dots-Based Fluorescent Sensor for the Selective Determination of a Potent Anti-Inflammatory Drug in the Presence of Its Photodegradation Products.

Herein, we synthesized biogenic carbon dots (CDs) with blue-shifted maximum excitation (λex/λem of 320/404 nm) from largely wasted tangerine seeds for the first time via a one-step hydrothermal method. The biogenic CDs exhibit a maximum excitation wavelength that overlaps with the absorption spectrum of ketorolac tromethamine (KETO) at 320 nm. The developed CDs serve as a turn-off fluorescent probe via an inner filter effect (IFE) quenching mechanism. The resulting CDs have high quantum yield (QY) (39% ± 2.89%, n = 5) and exhibited great performance toward KETO over a concentration range of 0.50-16.00 μg/mL with a limit of detection (LOD) = 0.17 μg/mL. The nanoprobe achieved a high % recovery in assaying KETO in tablet dosage form and had not been significantly affected by various interferents including co-formulated and co-administered drugs. The nanoprobe shows selectivity toward KETO, even in the presence of its photocatalytic degradation products. It can effectively investigate the elimination of KETO from aquatic systems and test its stability in pharmaceutical preparations. The developed nanoprobe underwent a comprehensive evaluation of its environmental impact using analytical eco-scale (AES), complex green analytical procedure index (Complex GAPI), and the Analytical GREEnness calculator (AGREE). The sustainability of the developed nano sensor was assessed and compared to the reported metal-based quantum dots probe for KETO using the innovative RGB 12 model, considering 12 white analytical chemistry (WAC) perspectives.

Innovative Molecularly Imprinted Electrochemical Sensor for Selective Nanomolar Detection of the Anti-COVID-19 Medication Molnupiravir

For the first time, a green ecofriendly approach is applied, to develop a molecularly imprinted polymer (MIP) electrochemical for the assay of the oral anti-viral molnupiravir (MLN) in various matrices as confirmed by referring to analytical eco-scale, green analytical procedure index (GAPI), Raynie and Driver, analytical greenness metric (AGREE), and national environmental index (NEMI). AuNPs were chronoamperometry deposited on the glassy carbon electrode surface (GCE) using 0.01 gm ml−1 gold solution (HAuCl4.3H2O) in 0.5 M H2SO4 at a constant potential of −0.4 V for 60 s. Then, the MIP was created by electropolymerizing OPDA on the surface of AuNPs GCE using cyclic voltammetry in the potential range between −0.5 and +1 V for 15 cycles (scan rate: 50 mV.s−1). To optimize the sensor’s performance, factors such as number of electropolymerization cycles, template: monomer ratio, binding and rebinding time, pH of rebinding buffer, extraction solvent, deposition time of Au nanoparticles, order of deposition on the electrode; surface, as well as differential pulse voltammetry parameters including accumulation potential and time, and potential step, were all investigated. The detection limit was set at 0.00098 ng ml−1 (3 × 10−12M) and the linearity range of MLN was between 0.033 ng ml−1 and 164 ng ml−1 (1 × 10−10–5 × 10−7 M). The MIP sensor was employed for MLN determination in its pharmaceutical product (capsules), spiked human plasma, and human urine samples with mean recovery % ± mean relative standard deviation (RSD) (99.82% ± 0.53), (99.88% ± 0.62), and (97.90% ± 0.70), respectively. The investigated sensor provided good reproducibility, repeatability, and durability. Acceptable selectivity regarding MLN when mixed with structurally comparable compounds was proved with mean recovery % ± mean RSD (97.10% ± 0.03). Additionally, when molnupiravir was exposed to oxidative, hydrolytic, and thermal stress conditions, good results in stability-indicating studies served as an indicator of sensor selectivity. The developed electrode is coupled with a portable potentiostat, making it a promising point-of-care diagnostic platform for on-site measurements.

Utility of green chemistry for feasible spectrofluorometric determination of trifluridine via metal complexation: Application to dosage forms

AbstractThe goal of the current research was to establish a quick and practical fluorometric technique for trifluridine analysis. The approach relied on the drug's complex formation with the zinc ion to produce a high‐fluorescence product. The fluorescence was further enhanced by adding sodium dodecyl sulfate, and it was observed at 450 nm following excitation at 400 nm. With a determination coefficient of 0.9994, the association between emission intensity and trifluridine concentration was linear between 1 and 125 ng mL−1. The quantitation limit was 0.987 ng mL−1 while 0.333 ng mL−1 was the detection limit. The buffer type, pH and concentration, type of surfactant and concentration, and finally the diluting solvent were among the reaction conditions that were closely examined. With great precision and reliability, the drug in question was quantified using this method in dosage formulations. The proposed method's level of greenness was assessed using two methodologies: the analytical greenness metric (AGREE) and the Green Analytical Procedure Index (GAPI).

A green micelle-enhanced first derivative synchronous fluorescence approach for determination of donepezil HCl and trazodone HCl in their pure state, pharmaceutical dosage form and spiked human plasma.

The study's objective is to establish an eco-friendly, sensitive and economical quantitative methodology for the concurrent analysis of donepezil HCl (DPZ) and trazodone HCl (TRZ) in raw materials, tablets and human plasma. The first derivative synchronous fluorescence spectroscopic (FDSFS) technique was applied at constant wavelength difference (∆λ = 120) for assessment of DPZ and TRZ at each other's zero-crossing point at 279 nm and 297 nm, respectively. The submitted technique was validated in accordance with ICH Q2 R1 guidelines and the linearity of the standard calibration curve was observed over the concentration range of 10-500 ng/ml for DPZ and 20-1,000 ng/ml for TRZ. The detection limits (LOD) were found to be 2.65 and 5.4ng/ml, and the limits of quantitation (LOQ) were 8.05 and 16.3ng/ml for DPZ and TRZ, respectively. This technique was used further to quantify the studied medications in their laboratory-prepared mixtures, commercial tablets and spiked plasma samples. The results obtained were not significantly different from those acquired from the comparison methods, indicating the high accuracy and precision of the proposed method. Furthermore, the ecological friendliness of the suggested method was evaluated and proven to be excellent using Green Analytical Procedure Index (GAPI) and Analytical GREEnness (AGREE) evaluation tools.

Estimating nitroxynil residues in food samples and surface water using two different sustainable chemical sensing techniques: Comparative greenness, whiteness, and blueness study

The presence of veterinary drug residues in edible animal tissues endangers human health and safety, accordingly, global nations enacted legislative restrictions to monitor their concentrations in food. In this work, we introduce two fluorimetric sensors for determining nitroxynil (NXL), a crucial veterinary medication, in various matrices. Sensor I, novel nitrogen and sulfur-doped carbon quantum dots (S,N-CQDs), was fabricated from strawberry and leek juices as cheap and sustainable natural resources. Only five minutes of microwave radiation were required as a rapid synthesizing technique without any drastic conditions or organic solvents. The S,N-CQDs manifest blue emission using λex/em of 340/418 nm. The synthesized nanosensor was characterized using UV Spectroscopy, transmission electron microscopy (TEM), and Fourier-transform infrared spectrometry (FTIR). Sensor II was the acriflavine reagent (AV) that exhibits native fluorescence using λex/em of 265/505 nm. Both sensors displayed quantitative turning off in their native fluorescence by increasing concentrations of NXL (1.0–10.0 and 0.5–8.0 µg mL−1) with correlation coefficients r = 0.9998 and 0.9999 for sensors I and II, respectively. The two probes achieved satisfactory percentage recoveries and standard deviation (SD < 4) for NXL assessing in complex matrices of diverse food samples (bovine muscle, kidney, and fat) and Fasciolar® veterinary formulation. Additionally, they have been successfully used to detect the investigated drug in river ecosystems with a mean %recovery of 100.10 ± 1.70, and 99.95 ± 1.31 for sensors I and II, respectively. The two constructed sensors’ specificity has been confirmed for all tested matrices reflecting their feasibility as promising platforms in therapeutic drug monitoring, livestock ecosystems, food safety assurance, quality control of drugs, and environmental pollution monitoring. Quenching mechanisms for both methodologies were studied and the reaction stoichiometry for NXL − AV complex was calculated in two ways. Lastly, a comprehensive comparison was performed between the suggested methodologies and published fluorimetric works. The greenness feature was assessed by the Analytical Eco-scale (AES), Green Analytical Procedure Index (GAPI), and Analytical GREEnness Metric Approach (AGREE). In addition, white analytical chemistry principles were checked to assess sustainability criteria using the RGB 12 algorithm. The recently launched Blue Applicability Grade Index (BAGI) metric tool was also employed to assess the practicality (Blueness) character.

Analysis of phosphodiesterase type 5 inhibitors and analogues as adulterants in herbal dietary food supplements in Saudi market using green UPLC-MS/MS method: Assessment of the greenness and whiteness profiles

Herbal dietary supplements are popular alternatives to oral phosphodiesterase type 5 inhibitors (PDE5Is) for treating Erectile Dysfunction (ED), yet concerns arise regarding their adulteration with undeclared synthetic PDE5Is or analogues, posing health risks. The aim of this study was to develop and validate a green UPLC-MS/MS method for sensitive and rapid detection of PDE5Is and analogues in sexual enhancement herbal dietary supplements marketed in Saudi Arabia. Method validation revealed good linearity with determination coefficients (r2) ≥ 0.9990, and LODs and LOQs in the range of 0.4 – 32 ng g−1 and 1––96 ng g−1, respectively. The accuracy ranged from 80.8 % to 103.4 % while inter-day precision was ≤ 8.6 % and intra-day precision was ≤ 8.4 %. The method was successfully utilized to analyze 32 herbal dietary supplements. The results revealed that 18 samples (56.3 %) tested positive for at least one of the target analytes. Sildenafil emerged as the most frequently detected analyte, found in 15 samples (20.1 µg g−1 to 37,492 µg g−1). Tadalafil was detected in 7 samples, with concentrations ranging from 4.46 µg g−1 to 19,986 µg g−1. Yohimbine was detected in only 4 samples, while icariin was detected at lower concentrations in 3 samples. Furthermore, the method greenness and whiteness profiles were evaluated using four metrics including the Analytical Eco-Scale, Green Analytical Procedure Index (GAPI), Analytical GREEnness (AGREE) metric, and Red-Green-Blue 12 (RGB 12) metric.This study provides foundational data on the adulteration of dietary supplements in Saudi Arabia and offers insights for future interventions to promote consumer safety and awareness regarding herbal dietary supplement consumption.