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1.
Luminescence ; 39(10): e4911, 2024 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-39350509

RESUMEN

As a gamma amino butyric acid-ergic agonist, Baclofen is often prescribed to adults and children for the treatment of severe spasticity that originates in the brain or spinal cord. Even after reviewing the literature extensively, no one has documented a method for estimating baclofen using microwave-assisted stability-indicating spectrofluorimetric techniques, despite the abundance of options for baclofen stability, assay, and bioanalysis. Organic solvents, which are typically necessary for current procedures but may be costly and toxic, have a severe effect on aquatic life and the environment. Using green solvents and 4-chloro-7-nitrobezofuran as a fluorescent probe, this work conducted a stability-indicating spectrofluorimetric estimate of baclofen. Through the use of a design-of-experiments technique, a reliable microwave-aided spectrofluorimetric method was developed, with little solvent consumption and time for sample analysis. Prior to conducting response surface analysis and optimizing important variables and responses, a fractional factorial design was used to screen method variables and responses. A central composite design was then employed for these purposes. This flexible spectrofluorimetric technique was used to assess baclofen concentrations in forced degraded samples and marketed formulations. For baclofen determination, the suggested spectrofluorimetric approach was found to be green, quick, easy to use, economical, and user-friendly.


Asunto(s)
Baclofeno , Microondas , Espectrometría de Fluorescencia , Baclofeno/química , Baclofeno/análisis , Tecnología Química Verde , Color , Solventes/química
2.
Spectrochim Acta A Mol Biomol Spectrosc ; 326: 125168, 2024 Sep 21.
Artículo en Inglés | MEDLINE | ID: mdl-39340944

RESUMEN

Designing new verified methods for the determination of pharmaceutical compounds in their specified formulation without prior separation and with high sensitivity taking in consideration analytical performance and simplicity has become a major concern of pharmaceutical quality control units. In the present work, a new simple and eco-friendly spectrofluorimetric method was developed and validated for the determination of Naproxen (NAP) and Domperidone (DOM) in their binary mixture, pharmaceutical formulation in addition to human plasma without prior separation. The proposed method is based on measuring the second derivative fluorescence intensity for NAP at 345 nm and for DOM at 292 after excitation at 235 nm without any interference from each other. All the variables affecting fluorescence intensity were studied and optimized. The proposed method showed excellent sensitivity with limit of detection (LOD) 12.286 ng/mL and 3.240 ng/mL for NAP and DOM respectively. In compliance with the ICH requirements, the optimized method was validated and was successfully utilized for the determination of both drugs in their pharmaceutical formulation and human plasma. Finally, the greenness of the proposed method was assessed using different assessment tools.

3.
BMC Chem ; 18(1): 164, 2024 Sep 09.
Artículo en Inglés | MEDLINE | ID: mdl-39252071

RESUMEN

Recently, phytochemicals play an important role in cancer management. Curcumin (CUR), a natural phytochemical, has been co-administered with widespread chemotherapeutic agents such as doxorubicin (DOX) due to its excellent antitumor activity and the ability to lower the adverse reactions and drug resistance cells associated with DOX use. The present study aims to determine DOX and CUR utilizing a label-free, selective, sensitive, and precise synchronous spectrofluorimetric method. The obvious overlap between the emission spectra of DOX and CUR prevents simultaneous estimation of both analytes by conventional spectrofluorimetry. To solve such a problem, synchronous spectrofluorimetric measurements were recorded at Δλ = 20 nm, utilizing ethanol as a diluting solvent. Curcumin was recorded at 442.5 nm, whereas DOX was estimated at 571.5 nm, each at the zero-crossing point of the other one. The developed method exhibited linearity over a concentration range of 0.04-0.40 µg/mL for CUR and 0.05-0.50 µg/mL for DOX, respectively. The values of limit of detection (LOD) were 0.009 and 0.012 µg/mL, while the values of limit of quantitation (LOQ) were 0.028 and 0.037 µg/mL for CUR and DOX, respectively. The adopted approach was carefully validated according to the guidelines of ICH Q2R1. The method was utilized to estimate CUR and DOX in laboratory-prepared mixtures and human biological matrices. It showed a high percentage of recoveries with minimal RSD values. Additionally, three different tools were utilized to evaluate the greenness of the proposed approach.

4.
Anal Chim Acta ; 1320: 343016, 2024 Sep 01.
Artículo en Inglés | MEDLINE | ID: mdl-39142787

RESUMEN

BACKGROUND: Direct detection of the notorious explosive triacetone triperoxide (TATP) is very difficult because it lacks facile ionization and UV absorbance or fluorescence. Besides, the current indirect methods are time-consuming and need a pre-step for TATP cleavage to hydrogen peroxide. Moreover, they commonly show significant false-positive results in the presence of some camouflage which limits their field applications. Herein, for the first time, a novel label-free field-applicable spectrofluorimetric nanobiosensor was developed for direct TATP detection using a novel activated-protein protected gold nanocluster (ABSA-AuNCs; QY = 28.3 %) synthesized by a combined protein-assisted-ultrasonication procedure. RESULTS: The ABSA-AuNCs revealed a fluorescence spectrum centered at 330.0 nm which was significantly quenched by TATP (binding constant = 154.06 M-1; ΔG = -12.5 kJ mol-1; E(%) = 88.5 %). This phenomenon was used as a basis for direct TATP quantification, providing a working range of 0.01-40.0 mg L-1 and a detection limit of 6.7 µg L-1 which is the lowest LOD provided for TATP detection up to now. A %RSD of 0.9 % and 1.56 % was obtained for repeatability and inter-day reproducibility, respectively. The selectivity was checked against a variety of camouflages, revealing ultra-selectivity. Several synthetic samples prepared by several camouflages and real samples (clay soil and real water media) were analyzed, revealing quantitative recoveries of TATP. SIGNIFICANCE: During the production of the notorious explosive TATP, it can be discharged into water and soil. This novel method eliminated the false-positive results of traditional methods and is applicable for direct quantitative detection of camouflaged TATP and its residues in real soil and water samples in a highly short response time (2 min). The camouflaged TATP analysis is important for tracking the terrorist attacks in field conditions and analysis of soil and water can provide a first indication of the location of the production site.


Asunto(s)
Sustancias Explosivas , Oro , Compuestos Heterocíclicos con 1 Anillo , Nanopartículas del Metal , Peróxidos , Espectrometría de Fluorescencia , Espectrometría de Fluorescencia/métodos , Sustancias Explosivas/análisis , Compuestos Heterocíclicos con 1 Anillo/química , Nanopartículas del Metal/química , Peróxidos/análisis , Peróxidos/química , Oro/química , Límite de Detección , Técnicas Biosensibles/métodos
5.
Luminescence ; 39(8): e4837, 2024 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-39113185

RESUMEN

During the pandemic, Favipiravir (FVP) and Molnupiravir (MPV) have been widely used for COVID-19 treatment, leading to their presence in the environment. A green synchronous spectrofluorimetric method was developed to simultaneously detect them in environmental water, human plasma, and binary mixtures. Maximum fluorescence intensity was achieved at pH 8, with MPV exhibiting two peaks at 300 and 430 nm, and FVP showing one peak at 430 nm. A fluorescence subtraction method effectively removed interference, enabling direct determination of MPV at 300 nm and FVP at 430 nm. The method showed linearity within 2-13 ng/mL for FVP and 50-600 ng/mL for MPV, with recoveries of 100.35% and 100.12%, respectively. Limits of detection and quantification were 0.19 and 0.57 ng/mL for FVP and 10.52 and 31.88 ng/mL for MPV. Validation according to ICH and FDA guidelines yielded acceptable results. The method demonstrated good recoveries of FVP and MPV in pharmaceuticals, tap water and Nile water (99.62% ± 0.96% and 99.69% ± 0.64%) as per ICH guidelines and spiked human plasma (94.87% ± 2.111% and 94.79% ± 1.605%) following FDA guidelines, respectively. Its environmental friendliness was assessed using Green Analytical Procedure Index (GAPI) and the Analytical Greenness Metric (AGREE) tools.


Asunto(s)
Amidas , Antivirales , Pirazinas , Espectrometría de Fluorescencia , Pirazinas/análisis , Pirazinas/sangre , Pirazinas/química , Amidas/análisis , Amidas/química , Amidas/sangre , Espectrometría de Fluorescencia/métodos , Humanos , Antivirales/análisis , Antivirales/sangre , Uridina/análisis , Uridina/sangre , Límite de Detección , Citidina/análisis , Citidina/sangre , Citidina/análogos & derivados , Tratamiento Farmacológico de COVID-19 , Mercaptopurina/sangre , Mercaptopurina/análisis , SARS-CoV-2 , Hidroxilaminas
6.
Luminescence ; 39(8): e4861, 2024 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-39109462

RESUMEN

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.


Asunto(s)
Piperazinas , Espectrometría de Fluorescencia , Piperazinas/química , Piperazinas/análisis , Tecnología Química Verde , Antipsicóticos/química , Estructura Molecular , Límite de Detección
7.
Spectrochim Acta A Mol Biomol Spectrosc ; 322: 124811, 2024 Dec 05.
Artículo en Inglés | MEDLINE | ID: mdl-39008930

RESUMEN

A novel spectrofluorimetric method with high selectivity and sensitivity was created to determine Pregabalin (PG) in pharmaceutical form, human serum, and urine. This method relies on detecting quenching in the intensity of luminescence of the europium acetylacetone complex (Eu3+-ACAC) at emission wavelength λem = 616 nm, which results from interaction with various concentrations of PG after excitation at λex = 395 nm and pH 6.5 in dimethylformamide (DMF). The calibration curve was generated using concentrations ranging from 7.6 × 10-8 to 6.3 × 10-6 mol/L. The plot showed a high correlation coefficient (r2) of 0.994 with a detection limit (LOD) of 2.81 × 10-8 mol/L and a quantification limit (LOQ) of 8.5 × 10-8 mol/L. The remarkable luminescence intensity quenching of the Eu3+-ACAC by ranged concentrations of PG was effectively employed as a photo probe to determine PG in marketable form and different body fluids. Spectroscopic characterization, such as absorption and emission spectra, confirmed the obtained sensor. The improved method is verified using a range of characteristics, such as accuracy, precision, selectivity, linearity, and robustness.


Asunto(s)
Europio , Límite de Detección , Pregabalina , Espectrometría de Fluorescencia , Espectrometría de Fluorescencia/métodos , Europio/química , Pregabalina/sangre , Pregabalina/análisis , Humanos , Pentanonas/química , Reproducibilidad de los Resultados , Acetamidas/química , Acetamidas/análisis
8.
R Soc Open Sci ; 11(7): 240268, 2024 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-39050722

RESUMEN

A sensitive, rapid and green synchronous spectrofluorimetric method was developed to simultaneously analyze a binary mixture of diosmin (DSM) and hesperidin (HSP). The RSFI of both medications was measured in methanol at Δλ of 100 nm. The results indicated that specific experimental factors had an impact on these intensities. The optimization and thorough examination of these parameters were conducted. The plots of synchronous fluorescence intensity-concentration for DSM and HSP were found to be linear within the concentration ranges of 0.5-5.0 µg ml-1 and 0.2-3.0 µg ml-1, respectively. The detection limits for DSM and HSP were 0.107 µg ml-1 and 0.048 µg ml-1, respectively. The limits of quantification were 0.323 µg ml-1 and 0.144 µg ml-1 for DSM and HSP, respectively. The method outlined in this study was successfully used to determine the quantities of both drugs present in commercially available mixed tablets. The results obtained using this method were subsequently compared to those of a comparison method. Greenness assessment of the suggested procedure was accomplished by applying the GAPI method. Consequently, the recommended method can be used in the routine quality control analysis of the two cited drugs with minimum harmful effect on the environment as well as the individuals.

9.
Luminescence ; 39(7): e4812, 2024 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-38965972

RESUMEN

Attention deficit hyperactivity disorder (ADHD) is a neurological condition frequently identified in early childhood and frequently co-occurs with other neuropsychological disorders, particularly autism. Viloxazine hydrochloride, a non-stimulant medication, has recently gained approval for treating attention-deficit hyperactivity disorder. This paper describes the first spectrofluorimetric method for precisely measuring the content of viloxazine in pharmaceutical capsules and rat plasma. This method employed NBD-Cl (4-chloro-7-nitrobenzo-2-oxa-1,3-diazole) as a fluorescent probe, which transformed viloxazine in an alkaline environment into a remarkably sensitive fluorescent adduct. Upon excitation at 476 nm, this adduct becomes detectable at a wavelength of 536 nm. The method was validated using ICH criteria, revealing acceptable linearity across a concentration range of 200-2000 ng/ml and high sensitivity with LOD and LOQ values of 46.774 ng/ml and 141.741 ng/ml, respectively. This method was adeptly applied in a pharmacokinetic study of viloxazine in rat plasma following a single oral dose (10 mg/kg), yielding a mean peak plasma concentration (Cmax) of 1721 ng/ml, achieved within 1.5 h. Furthermore, the environmental impact of the technique was assessed using two greenness assessment tools, revealing a notable level of eco-friendliness and sustainability.


Asunto(s)
Colorantes Fluorescentes , Espectrometría de Fluorescencia , Viloxazina , Animales , Ratas , Colorantes Fluorescentes/química , Viloxazina/química , Viloxazina/farmacocinética , Viloxazina/sangre , Masculino , Estructura Molecular , 4-Cloro-7-nitrobenzofurazano/química , Administración Oral
10.
Luminescence ; 39(7): e4824, 2024 Jul.
Artículo en Inglés | MEDLINE | ID: mdl-39004773

RESUMEN

Dabigatran (DBG), marketed as Pradaxa, is an anticoagulant medication prescribed for the treatment and mitigation of blood clots and to lower the risk of stroke in individuals with the heart condition known as atrial fibrillation. This medication is specifically indicated for preventing blood clots post hip or knee replacement surgeries and in patients with a prior history of clots. Compared to warfarin, dabigatran serves as a viable alternative that does not necessitate routine blood monitoring tests. The complimentary benefits associated with SALL (salting-out assisted liquid-liquid extraction) and the fluorogenic capabilities of benzofurazan. These methods were combined to provide an affordable and sensitive DBG assaying method. The spectral strength of the yellow luminous product was examined at 533.8 nm and by adjustment of a wavelength of 474.7 nm for excitation. To assess its linearity, the calibration chart was tested across a DBG concentration range of 30-500 ng/ml. Via accurate computation based on ICH, the detection limit (LD) was determined to be 9.5 ng/ml, and the strategy can quantify the DBG to a limit of 28 ng/ml. To ensure success, various crucial parameters for method implementation have been extensively studied and adapted. The validation of the strategy adhered to the policies outlined by ICH, affirming its precision in quantifying DBG in capsules. Furthermore, the inclusion of SALLE steps facilitated accurate monitoring of DBG in plasma samples, introducing a unique and advanced methodology for analyzing this compound in biological samples.


Asunto(s)
Anticoagulantes , Cápsulas , Dabigatrán , Dabigatrán/sangre , Dabigatrán/química , Dabigatrán/farmacología , Humanos , Anticoagulantes/química , Anticoagulantes/sangre , Anticoagulantes/farmacología , Colorantes Fluorescentes/química , Extracción Líquido-Líquido , Espectrometría de Fluorescencia , Límite de Detección , 4-Cloro-7-nitrobenzofurazano
11.
Sci Rep ; 14(1): 16460, 2024 07 16.
Artículo en Inglés | MEDLINE | ID: mdl-39013989

RESUMEN

A novel, highly sensitive and eco-friendly micellar-mediated spectrofluorimetric method was developed and validated for the determination of the novel antiparkinsonian drug safinamide mesylate in the presence of its related precursor impurity, 4-hydroxybenzaldehyde. The proposed approach relies on increasing the inherent fluorescence emission at 296 nm of safinamide, by forming hydrogen bonds between the mentioned drug and sodium dodecyl sulfate in the micellar system using 0.1 N HCl as a solvent, following excitation at 226 nm. A thorough investigation was conducted into the experimental factors affecting spectrofluorimetric behavior of the studied drug. A linearity plot of safinamide over the concentration range of 10.0-1000.0 ng/mL against the relative fluorescence intensities was established. The proposed method demonstrated excellent sensitivity down to the nano-gram level with detection and quantitation limits of 1.91 and 5.79 ng/mL, respectively. The studied drug was effectively determined in Parkimedine® Tablets. Furthermore, the proposed method allows for ultrasensitive quantification of safinamide in spiked human plasma, with satisfactory percentage recovery (98.97-102.28%). Additionally, the greenness assessment using the advanced green certificate classification approach, the complementary green analytical procedure index (Complex-GAPI), and the analytical GREEness metric approach (AGREE), along with the practicality check using the Blue Applicability Grade Index in addition to the all-inclusive overall whiteness evaluation using the RGB-12 model were carried out. The outcomes demonstrated the effectiveness and whiteness of the proposed technique. Clearly, the suggested approach has the advantages of being simple, requiring no pretreatment steps, and relying solely on direct measuring procedures.


Asunto(s)
Alanina , Antiparkinsonianos , Bencilaminas , Micelas , Espectrometría de Fluorescencia , Humanos , Espectrometría de Fluorescencia/métodos , Alanina/análogos & derivados , Alanina/sangre , Antiparkinsonianos/sangre , Antiparkinsonianos/análisis , Antiparkinsonianos/uso terapéutico , Bencilaminas/sangre , Bencilaminas/análisis , Bencilaminas/química , Comprimidos , Límite de Detección , Reproducibilidad de los Resultados
12.
Spectrochim Acta A Mol Biomol Spectrosc ; 321: 124731, 2024 Nov 15.
Artículo en Inglés | MEDLINE | ID: mdl-38955074

RESUMEN

Ibrutinib, an antineoplastic agent tackling chronic lymphocytic leukemia, mantle cell lymphoma, and Waldenstrom's Macroglobulinemia, falls under the category of BCS class II drugs, characterized by a puzzling combination of low solubility and high permeability. Its oral bioavailability remains a perplexing challenge, merely reaching 2.9 % due to formidable first-pass metabolism hurdles. In a bid to surmount this obstacle, researchers embarked on a journey to develop ibrutinib-loaded NLCs (Nanostructured Lipid Carriers) using a methodology steeped in complexity: a Design of Experiments (DoE)-based hot melted ultrasonication approach. Despite a plethora of methods for analyzing ibrutinib in various matrices, the absence of a spectrofluorimetric method for assessing it in rat plasma added to the enigma. Thus emerged a spectrofluorimetric method, embodying principles of white analytical chemistry and analytical quality by design, employing a Placket-Burman design for initial method exploration and a central composite design for subsequent refinement. This method underwent rigorous validation in accordance with ICH guidelines, paving the way for its application in scrutinizing the in-vivo pharmacokinetics of ibrutinib-loaded NLCs, juxtaposed against commercially available formulations. Surprisingly, the optimized NLCs exhibited a striking 1.82-fold boost in oral bioavailability, shedding light on their potential efficacy. The environmental impact of this method was scrutinized using analytical greenness tools, affirming its eco-friendly attributes. In essence, the culmination of these efforts has not only propelled advancements in drug bioavailability but also heralded the dawn of a streamlined and environmentally conscious analytical paradigm.


Asunto(s)
Adenina , Lípidos , Piperidinas , Pirimidinas , Espectrometría de Fluorescencia , Animales , Adenina/análogos & derivados , Adenina/farmacocinética , Adenina/química , Adenina/sangre , Piperidinas/farmacocinética , Piperidinas/química , Piperidinas/sangre , Lípidos/química , Masculino , Espectrometría de Fluorescencia/métodos , Ratas , Pirimidinas/farmacocinética , Pirimidinas/química , Pirimidinas/sangre , Portadores de Fármacos/química , Nanoestructuras/química , Pirazoles/farmacocinética , Pirazoles/química , Pirazoles/sangre , Pirazoles/administración & dosificación , Reproducibilidad de los Resultados , Ratas Wistar
13.
Luminescence ; 39(6): e4813, 2024 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-38922756

RESUMEN

Pemigatinib (PGT) is a recently FDA-approved small molecule kinase inhibitor used for the treatment of relapsed or refractory myeloid/lymphoid neoplasms in adults. This study introduces the development of a first microwell spectrofluorimetric method (MW-SFM) for quantifying PGT in FDA-approved tablets and plasma samples. The method utilized the enhancement of PGT's weak native fluorescence by blocking photoinduced electron transfer (PET) and micellization with sodium lauryl sulfate (SLS). The MW-SFM was performed in 96-microwell plates, and fluorescence signals were measured using a fluorescence microplate reader with excitation at 290 nm and emission at 350 nm. The method exhibited a linear range of 2-250 ng mL-1, and a limit of quantitation was 6.5 ng mL-1. The accuracy and precision of the method were confirmed with recovery rates ranging from 96.5% to 102.8% and relative standard deviations of 1.52% to 3.51%. The MW-SFM successfully analyzed Pemazyre® tablets, assessed content uniformity, and analyzed PGT-spiked human plasma samples. The greenness of the MW-SFM was verified using three different metric tools. In conclusion, the proposed MW-SFM is a valuable tool in supporting quality assessment of dosage forms, conducting pharmacokinetic studies, and monitoring therapeutic outcomes.


Asunto(s)
Espectrometría de Fluorescencia , Comprimidos , Humanos , Fluorescencia , Transporte de Electrón , Micelas , Pirimidinas/sangre , Pirimidinas/química , Dodecil Sulfato de Sodio/química , Estructura Molecular , Procesos Fotoquímicos
14.
J Fluoresc ; 2024 Jun 12.
Artículo en Inglés | MEDLINE | ID: mdl-38865063

RESUMEN

Pemetrexed is a chemotherapeutic medicine, under the trade name Alimta. Malignant pleural mesothelioma patients. Its application in lung cancer has been studied. Here in, a second spectrofluorimetric method was advanced for quantifying of Pemetrexed in pharmaceutical formulation and spiked human plasma. That method depends on fluorescence derivatization of Pemetrexed with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) at 75 °C in a (pH 9) of borate buffer to produce a fluorescent derivative which can be detected at 520 nm afterwards excitation at 460 nm. The method has been validated using ICH criteria, and it demonstrated linearity in a range of 2-120 ngmL-1. The proposed method was applied precisely and accurately for quantifying Pemetrexed within pharmaceutical formulation and spiking human plasma without any interferences. Moreover, the method's sustainability was evaluated and compared to the published method using two greenness assessment tools termed analytical eco-scale and Analytical GREENness (AGREE). That findings suggest that the method is more sustainable than the published method.

15.
Spectrochim Acta A Mol Biomol Spectrosc ; 320: 124596, 2024 Nov 05.
Artículo en Inglés | MEDLINE | ID: mdl-38850823

RESUMEN

People frequently administer Tizanidine (TIZ) to treat spasticity resulting from diseases like multiple sclerosis or spinal cord injuries. It also helps prevent muscle spasms. It helps to relax and release tense and stiff muscles by inhibiting specific nerve signals in the brain and spinal cord. The technique employed in this study made use of the unique ability of benzofurazan to confer fluorescent character when reacted with TIZ at specific conditions. This fluorogenic property was harnessed to evolve a remarkably sensitive, affordable, and selective method to quantify TIZ. The resulting yellow fluorescent product was observedat a wavelength beam of 532.9 nm, and an excitation wavelength beam of 474.9 nm was applied. By looking at the response across the TIZ concentration, the calibration chart's linearity was assessed in the range of 40-500 ng/mL. By computation, the approach's detection level (LOD) was determined to be 11.9 ng/mL, while the quantitation level was approximated to be 36 ng/mL. All pertinent factors impacting the strategy's efficacy were thoroughly inspected and adjusted accordingly. The proposed strategy was validated following the guidelines outlined by the ICH. The outcomes confirmed the method's capability for the accurate quantifying of TIZ in tablets, spiked plasma, and pharmaceutical assessing content uniformity.


Asunto(s)
Benzoxazoles , Clonidina , Límite de Detección , Espectrometría de Fluorescencia , Comprimidos , Clonidina/análogos & derivados , Clonidina/análisis , Clonidina/sangre , Espectrometría de Fluorescencia/métodos , Humanos , Benzoxazoles/química , Colorantes Fluorescentes/química , Reproducibilidad de los Resultados , Calibración , Concentración de Iones de Hidrógeno
16.
Spectrochim Acta A Mol Biomol Spectrosc ; 319: 124521, 2024 Oct 15.
Artículo en Inglés | MEDLINE | ID: mdl-38830329

RESUMEN

The USFDA recently approved mirabegron, a novel once-daily ß-3 adrenoceptor agonist for oral administration, as a transformative treatment for overactive bladder. Despite the existence of numerous analytical methods for the assay and bioanalysis of mirabegron, it's perplexing that none have explored the domain of microwave-assisted sensitive spectrofluorimetric method for mirabegron estimation, even after extensive literature review. Adding to the enigma is the insistence of current analytical methods on using expensive and harmful organic solvents, posing a threat to marine life and the broader environment. Recently, the white analytical chemistry approach has been introduced to develop analytical methods that are cost-effective, environmentally friendly, and user-friendly. Consequently, a white analytical chemistry-based, sensitive, and eco-friendly spectrofluorimetric estimation of mirabegron has been initiated, using 4-Chloro-7-nitrobenzofurazan as a fluorescent biosensing probe. The development of this robust method involved a series of experiments designed to minimize solvent and time wastage. Through a combination of fractional factorial and Box-Behnken designs, researchers identified the critical variables and optimized the method to perfection. This method was validated according to the stringent ICH Q2 (R2) and USFDA guidelines, ensuring its reliability and accuracy. Once approved, this sensitive spectrofluorimetric method was tested, accurately estimating mirabegron levels in commercial formulations and rat plasma samples. To further enrich the study, a comprehensive evaluation of existing analytical methods was conducted alongside the proposed spectrofluorimetric method, using advanced tools like the AGREE calculator, GAPI software, and RGB model to assess their eco-friendliness and effectiveness in mirabegron estimation.


Asunto(s)
Acetanilidas , Colorantes Fluorescentes , Microondas , Espectrometría de Fluorescencia , Tiazoles , Tiazoles/química , Tiazoles/sangre , Tiazoles/análisis , Acetanilidas/análisis , Acetanilidas/sangre , Acetanilidas/química , Animales , Colorantes Fluorescentes/química , Espectrometría de Fluorescencia/métodos , Técnicas Biosensibles/métodos , Tecnología Química Verde/métodos , Reproducibilidad de los Resultados , Ratas , Límite de Detección , Masculino
17.
Luminescence ; 39(5): e4777, 2024 May.
Artículo en Inglés | MEDLINE | ID: mdl-38785072

RESUMEN

This study introduces a practical and cost-effective method for tracking diltiazem (DLZ) analytically. It utilizes a fluorimetric approach that relies on the modulation of fluorescence intensity of a dye called erythrosine B. Through a one-pot experiment performed in an acidic environment, a complex is rapidly formed between DLZ and erythrosine B. By observing the decrease in erythrosine B emission, a linear calibration plot is established, enabling the detection and quantification of DLZ concentrations ranging from 40 to 850 ng/ml. The estimated limits of detection and quantitation were 10.5 and 32.1 ng/ml, respectively. The variables affecting the DLZ-dye complex system were carefully adjusted. The validity of the approach was confirmed through a thorough evaluation based on the criteria set by ICH guidelines. The accuracy and precision of the methodology were evaluated, and the standard deviation and relative standard deviation were below 2. The strategy was successfully employed to analyze DLZ in tablets and capsules, and no significant variation between the proposed and reported methods as the values of the estimated t-test and F-test at five determinations were below 2.306 and 6.338, respectively. Notably, the method adheres to the principle of green chemistry by utilizing distilled water as the dispersing medium.


Asunto(s)
Diltiazem , Eritrosina , Diltiazem/análisis , Diltiazem/química , Eritrosina/química , Eritrosina/análisis , Espectrometría de Fluorescencia , Comprimidos/análisis , Concentración de Iones de Hidrógeno , Límite de Detección , Cápsulas/química , Colorantes Fluorescentes/química , Formas de Dosificación
18.
J Fluoresc ; 2024 Apr 16.
Artículo en Inglés | MEDLINE | ID: mdl-38625571

RESUMEN

For the first time, clemastine was estimated in this work utilizing two validated resonance Rayleigh scattering (RRS) and fluorimetric methods. The methods relied on forming an association complex in an acidic medium between eosin Y reagent and clemastine. In the spectrofluorimetric approach, the investigated drug was quantified by quenching the fluorescence-emission intensity of eosin Y at 543.5 nm. The RRS method relied on enhancing the RRS spectrum at 331.8 nm, which is produced when eosin Y interacts with clemastine. Suitable conditions were established for the reaction to achieve maximum sensitivity. The linear values obtained from the spectrofluorimetric approach and the RRS method fall into the ranges of 0.2-1.5 µg mL- 1 and 0.25-2.0 µg mL- 1, respectively. It was established that the detection limits for these methods were 0.045 µg mL- 1 and 0.059 µg mL- 1, respectively. The developed methodologies yielded acceptable recoveries when used to estimate the quantity of clemastine in its pharmaceutical tablet dosage form. Regarding the use of greener solvents that were chosen, the suggested and reported methods were compared with the help of the Green Solvents Selecting (GSST) tool for assessing hazardous solvents to achieve sustainability. Furthermore, analytical Eco scale and comprehensive assessments of whiteness, blueness, and greenness were carried out utilizing Modified NEMI, ComplexGAPI, and AGREE evaluation tools. Additionally, recently developed tools such as BAGI and RGB 12 were applied to assess the blueness and the whiteness of the suggested methods.

19.
Luminescence ; 39(3): e4704, 2024 Mar.
Artículo en Inglés | MEDLINE | ID: mdl-38433336

RESUMEN

Darolutamide is an oral nonsteroidal androgen receptor antagonist used to delay the process of prostate cancer to metastatic disease and to increase the quality of life for people with advanced prostate cancer. Here, a second spectrofluorimetric method was advanced for quantifying Darolutamide in pharmaceutical formulation and spiked human plasma. This method depends on the fluorescence derivatization of Darolutamide with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) at 75°C in a (pH 9) of borate buffer to produce a fluorescent derivative that can be detected at 520 nm after excitation at 460 nm. The method has been validated using ICH criteria, and it demonstrated linearity in the range 5-200 ng ml-1 . The limit of detection (LOD) and limit of quantitation (LOQ) were 1.15 and 3.84 nm, respectively. The proposed method was applied precisely and accurately for quantifying Darolutamide within the pharmaceutical formulation and spiking human plasma without any interferences. Moreover, the method's sustainability was evaluated and compared with the published method using two greenness assessment tools termed analytical eco-scale and Analytical GREEnness (AGREE). These findings suggest that the method is more sustainable than the published method.


Asunto(s)
4-Cloro-7-nitrobenzofurazano , Antineoplásicos , Neoplasias de la Próstata , Pirazoles , Masculino , Humanos , Composición de Medicamentos , Calidad de Vida , Espectrometría de Fluorescencia
20.
Spectrochim Acta A Mol Biomol Spectrosc ; 313: 124168, 2024 May 15.
Artículo en Inglés | MEDLINE | ID: mdl-38513420

RESUMEN

A typical drug used to treat Parkinson's disease is called rasagiline. It belongs to an assortment of drugs known as monoamine oxidase inhibitors, which function by raising dopamine levels in the brain. This work created a unique spectrofluorimetric method for the analytical assay of rasagiline for the first time. The approach utilized the synergistic utility of the fluorogenic properties of benzofurazan and salting-out assisted liquid-liquid extraction. By combining these techniques an ultrasensitive, and highly selective methodology for the assay of rasagiline was established. Measurements were made of the resultant yellow fluorescent product at 533 nm by applying an excitation wavelength of 475.3 nm. The calibration graph was examined to assess its linearity across a range of 30-600 ng/ml. Through estimation, the limit of detection was discovered to be 8.9 ng/ml, while the quantitation limit was estimated to be 27 ng/ml. All relevant parameters influencing the fulfillment of the developed method were thoroughly examined and tuned. Following the directives set by the (ICH) the suggested approach was confirmed and demonstrated its capability for the accurate determination of rasagiline in tablets, as well as for testing content uniformity. The incorporation of salting-out assisted liquid-liquid extraction technology enables effective tracking of rasagiline in plasma samples, providing a novel and innovative approach for its analysis in biological matrices.


Asunto(s)
4-Cloro-7-nitrobenzofurazano , Inhibidores de la Monoaminooxidasa , Cloruro de Sodio , Inhibidores de la Monoaminooxidasa/farmacología , Inhibidores de la Monoaminooxidasa/uso terapéutico , Indanos , Extracción Líquido-Líquido/métodos
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