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1.
Luminescence ; 39(4): e4748, 2024 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-38644515

RESUMO

In an acidic buffered solution, erythrosine B can react with amiodarone to form an association complex, which not only generates great enhancement in resonance Rayleigh scattering (RRS) spectrum of erythrosine B at 346.5 nm but also results in quenching of fluorescence spectra of erythrosine B at λemission = 550.4 nm/λexcitation = 528.5 nm. In addition, the formed erythrosine B-amiodarone complex produces a new absorbance peak at 555 nm. The spectral characteristics of the RRS, absorbance, and fluorescence spectra, as well as the optimum analytical conditions, were studied and investigated. As a result, new spectroscopic methods were developed to determine amiodarone by utilizing erythrosine B as a probe. Moreover, the ICH guidelines were used to validate the developed RRS, photometric, and fluorimetric methods. The enhancements in the absorbance and the RRS intensity and the decrease in the fluorescence intensity of the used probe were proportional to the concentration of amiodarone in ranges of 2.5-20.0, 0.2-2.5, and 0.25-1.75 µg/mL, respectively. Furthermore, limit of detection values were 0.52 ng/mL for the spectrophotometric method, 0.051 µg/mL for the RRS method, and 0.075 µg/mL for the fluorimetric method. Moreover, with good recoveries, the developed spectroscopic procedures were applied to analyze amiodarone in its commercial tablets.


Assuntos
Amiodarona , Eritrosina , Espectrometria de Fluorescência , Amiodarona/análise , Amiodarona/química , Eritrosina/química , Eritrosina/análise , Antiarrítmicos/análise , Antiarrítmicos/química , Estrutura Molecular
2.
J Fluoresc ; 2024 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-38625571

RESUMO

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.

3.
Luminescence ; 2023 Dec 11.
Artigo em Inglês | MEDLINE | ID: mdl-38081623

RESUMO

In this study, netilmicin (NTM) was selectively assessed in its dosage forms after a facile derivatization reaction. The proposed approach was based on the interaction between NTM and o-phthalaldehyde/2-mercaptoethanol (Roth's reagent). The reaction product was fluorometrically measured at λemission of 434 nm after λexcitation of 338 nm. All reaction conditions for achieving the optimum fluorescence switch-on activity were visualized and monitored. Moreover, the method was validated under ICH guidelines, and was linear over the range 30-210 ng/ml after plotting netilmicin concentrations against the corresponding fluorescence intensity values. In addition, the selectivity of the developed method was investigated against either the co-formulated drug (dexamethasone) or a common ophthalmic drop excipient (benzalkonium chloride) without interference from either of them. Furthermore, the developed method was applied to assay netilmicin in various samples of pharmaceutical eye drops with good recovery. Finally, multicriteria greenness and whiteness metrics were used to evaluate the sustainability, greenness, and whiteness of the approach. The applied tools were the AGREE algorithm, the RGB 12 algorithm, and HEXAGON.

4.
Int J Nanomedicine ; 18: 5831-5869, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-37869062

RESUMO

Purpose: Immunomodulatory and broad-spectrum antiviral activities have motivated the evaluation of curcumin for Coronavirus infection 2019 (COVID-19) management. Inadequate bioavailability is the main impediment to the therapeutic effects of oral Cur. This study aimed to develop an optimal curcumin transferosome-loaded thermosensitive in situ gel to improve its delivery to the lungs. Methods: Transferosomes were developed by using 33 screening layouts. The phospholipid concentration as well as the concentration and type of surfactant were considered independent variables. The entrapment efficiency (EE%), size, surface charge, and polydispersity index (PDI) were regarded as dependent factors. A cold technique was employed to develop thermosensitive in-situ gels. Optimized transferosomes were loaded onto the selected gels. The produced gel was assessed based on shape attributes, ex vivo permeability enhancement, and the safety of the nasal mucosa. The in vitro cytotoxicity, antiviral cytopathic effect, and plaque assay (CV/CPE/Plaque activity), and in vivo performance were evaluated after intranasal administration in experimental rabbits. Results: The optimized preparation displayed a particle size of 664.3 ± 69.3 nm, EE% of 82.8 ± 0.02%, ZP of -11.23 ± 2.5 mV, and PDI of 0.6 ± 0.03. The in vitro curcumin release from the optimized transferosomal gel was markedly improved compared with that of the free drug-loaded gel. An ex vivo permeation study revealed a significant improvement (2.58-fold) in drug permeability across nasal tissues of sheep. Histopathological screening confirmed the safety of these preparations. This formulation showed high antiviral activity against SARS-CoV-2 at reduced concentrations. High relative bioavailability (226.45%) was attained after the formula intranasally administered to rabbits compared to the free drug in-situ gel. The curcumin transferosome gel displayed a relatively high lung accumulation after intranasal administration. Conclusion: This study provides a promising formulation for the antiviral treatment of COVID-19 patients, which can be evaluated further in preclinical and clinical studies.


Assuntos
COVID-19 , Curcumina , Humanos , Animais , Coelhos , Ovinos , Lipossomos , Administração Intranasal , Curcumina/farmacologia , SARS-CoV-2 , Portadores de Fármacos , Géis , Antivirais/farmacologia , Tamanho da Partícula
5.
Luminescence ; 38(10): 1836-1843, 2023 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-37555794

RESUMO

Naftidrofuryl is a vasodilator medication used for treating cerebral and peripheral vascular diseases. In this study, two spectroscopical techniques, spectrofluorimetric and resonance Rayleigh scattering (RRS), were utilized to quantify naftidrofuryl in its pharmaceutical samples. The developed methodologies in this study rely on a facile process of forming an association complex between erythrosine B reagent and naftidrofuryl under acidic conditions. The fluorimetric assay is based on the ability of naftidrofuryl to quench and decrease the native fluorescence intensity of the reagent when measured at λ emis . = 550 nm ( λ excit . = 526 nm). Under similar reaction conditions, the RRS method relies on the observed amplification in the RRS spectrum of the reagent at a wavelength of 577 nm following its interaction with naftidrofuryl. The methods exhibited linearity within the ranges 0.2-1.6 µg/ml (r2  = 0.999) and 0.1-1.4 µg/ml (r2  = 0.9994), with limit of quantitation values of 0.146 and 0.099 µg/ml, and limit of detection values of 0.048 and 0.032 µg/ml, for the fluorometric and the RRS methods, respectively. Moreover, the quenching between the dye and naftidrofuryl was studied using Stern-Volmer analysis, and the methodologies were experimentally optimized and validated. Additionally, acceptable recoveries were achieved when the procedures were applied to determine naftidrofuryl in pharmaceutical samples.


Assuntos
Eritrosina , Nafronil , Nafronil/análise , Espectrometria de Fluorescência/métodos , Espalhamento de Radiação , Preparações Farmacêuticas
6.
Spectrochim Acta A Mol Biomol Spectrosc ; 299: 122839, 2023 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-37201330

RESUMO

Netilmicin is an aminoglycoside antibiotic used to treat infections caused by a broad spectrum of Gram-negative and Gram-positive bacteria and is pharmaceutically formulated in ophthalmic dosage forms. In this study, two spectrofluorimetric approaches were designed and developed to switch-on the fluorescence activity of NTC. The first method, or Hantzsch (HNZ) method, was relied on measuring the generated fluorescence intensity upon the condensation of NTC with acetylacetone and formaldehyde (Hantzsch reaction) at λemis=483 nm/λexcit=425.5 nm. While the second fluorometric method (NHD method) was relied on measuring the generated fluorescence intensity upon the condensation of NTC with ninhydrin/phenylacetaldehyde at λemis=482.2 nm/λexcit=385.8 nm. The reaction conditions for the two approaches were well investigated and optimized. The selectivity study for the methods was investigated by determining NTC in the presence of the co-formulated drug (dexamethasone) and pharmaceutical excipients. The validation for two approaches was performed based on ICH guidelines, and ranges of linearity were 0.1-1.2 and 1.5-6.0 µg/mL, while LOD values were 0.039 and 0.207 µg/mL for the HNZ method and the NHD method, respectively. Finally, NTC has been determined in different ophthalmic preparations by the proposed approaches with adequate recovery values.


Assuntos
Netilmicina , Ninidrina , Indicadores e Reagentes , Espectrometria de Fluorescência/métodos , Formaldeído
7.
Spectrochim Acta A Mol Biomol Spectrosc ; 295: 122616, 2023 Jul 05.
Artigo em Inglês | MEDLINE | ID: mdl-36947938

RESUMO

Principles of Green Analytical Chemistry recommended preferring using reagents from renewable sources and eliminating toxic reagents. Vachellia nilotica is a widespread plant throughout different parts of the world. In this study, using microwave energy, fluorescent carbon dots were synthesized for the first time from Vachellia nilotica pods. The morphology of the prepared carbon dots was characterized by SEM and TEM techniques, and the spectroscopic character exhibit green emission at 480 nm at λex = 386.5 nm. This fluorescence can be effectively quenched by adding Fe (III) ions (Method I). Furthermore, Vachellia nilotica pods were extracted by different solvents, including methanol, deionized water, absolute ethanol, acetone, acetonitrile, and DMF. The acetonitrile extract of Vachellia nilotica exhibited a strong red fluorescence emission at 673.9 at λex = 410 nm. Among various types of salt metals, only Fe (III) can effectively quench the fluorescence intensity of the acetonitrile extract (method II). Moreover, the bright yellow color of the aqueous extract can be changed into violet color. The absorbance of the resulted color can be spectrophotometrically measured at λ max = 530 nm (method III). The best analytical factors were optimized for the developed methods. The developed methods were applied to determine Fe (III) in different water samples.

8.
Luminescence ; 38(4): 477-486, 2023 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-36880484

RESUMO

A sensitive and selective phenothiazine-based sensor (PTZ) has been successfully synthesized. The sensor PTZ displayed specific identification of CN- 'turn-off' fluorescence responses with a quick reaction and strong reversibility in an acetonitrile:water (90:10, V/V) solution. The sensor PTZ for detecting CN- exhibits the marked advantages of quenching the fluorescence intensity, fast response time (60 s), and low value of the detection limit. The concentration that is authorized for drinking water by the WHO (1.9 µM) is far higher than the detection limit, which was found to be 9.11 × 10-9 . The sensor displays distinct colorimetric and spectrofluorometric detection for CN- anion due to the addition of CN- anion to the electron-deficient vinyl group of PTZ, which reduces intramolecular charge transfer efficiencies. The 1:2 binding mechanism of PTZ with CN- was validated by fluorescence titration, Job's plot, HRMS, 1 H NMR, FTIR analysis, and density functional theory (DFT) investigations, among other methods. Additionally, the PTZ sensor was successfully used to precisely and accurately detect cyanide anions in actual water samples.


Assuntos
Cianetos , Água Potável , Cianetos/química , Ânions/química , Água Potável/análise , Espectrofotometria , Colorimetria/métodos
9.
Luminescence ; 38(2): 92-98, 2023 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-36427249

RESUMO

Indigo Carmine is a hazardous dye and produces an allergic action for humans despite the excessive use of the dye in several industrial fields. A sensitive and simple fluorescent assay for determining Indigo Carmine relying on quenching of the fluorescent europium-doped carbon dots by the action of inner filter effect was developed. This sensing platform involved the preparation of europium-doped carbon dots from the hydrothermal carbonization of tannic acid and europium chloride, which was used as fluorescent reagent with a distinctive excitation/emission wavelength at 307/340 nm. Both excitation and emission fluorescence of prepared carbon dots can be successfully quenched by adding Indigo Carmine dye. The developed spectrofluorimetric method exhibits good linearity with the concentration of Indigo Carmine dye in the range of 1.5 to 10.0 µg/ml and provided a limit of detection (LOD) value of 0.40 µg/ml. Furthermore, the prepared carbon nanoparticles were identified and characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier-transform infrared (FTIR), and ultraviolet (UV)-spectrophotometer techniques. In addition, the developed detecting approach was applied to determine Indigo Carmine in juice samples with acceptable recovery.


Assuntos
Índigo Carmim , Pontos Quânticos , Humanos , Carbono , Carmim , Európio , Corantes , Taninos , Corantes Fluorescentes
10.
Spectrochim Acta A Mol Biomol Spectrosc ; 287(Pt 1): 122124, 2023 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-36427404

RESUMO

Turmeric, a spice known for its therapeutic benefits, is a major source of curcumin which is a polyphenol with anti-inflammatory properties. It aids in treating arthritis, anxiety, metabolic syndrome, liver disease, hyperlipidemia, and inflammatory diseases. In this study, a novel fluorescence probe was designed to detect the adulteration of curcumin by metanil yellow (a harmful artificial dye). The probe was synthesized from the carbonization and conversion of the Tannic acid-Eu3+ complex to bright fluorescence Eu-carbon dots in the presence of orthophosphoric acid. The size, morphological, and optical features of the formed Eu-carbon dots were characterized by UV, SEM, TEM, and FTIR techniques. Furthermore, the formed Eu-carbon dots possess unique fluorescence excitation and emission features at 307.5 nm and 340.6 nm, respectively. These fluorescence features can be successfully quenched upon the addition of metanil yellow dye. The value of quenching in the fluorescence intensity of the Eu-C-dots was directly proportional to the dye's concentration. The LOD value for the proposed method was 0.390 µg/mL with a linear range of 1.0-15.0 µg/mL. Furthermore, the methodology exhibited good recovery values for determining the studied dye without any interference from the presence of curcumin.


Assuntos
Curcuma , Curcumina , Pós , Fluorescência , Európio , Carbono
11.
J Pharm Biomed Anal ; 219: 114941, 2022 Sep 20.
Artigo em Inglês | MEDLINE | ID: mdl-35905532

RESUMO

Nitazoxanide is an antimicrobial compound that was originally developed as an antiprotozoal drug. Recently nitazoxanide has been identified as broad-spectrum antiviral agent and redirected for the remediation of some respiratory tract viral infections. In this study, the spectrofluorimetric technique has been applied to determine Nitazoxanide (NTX) in tablets or its metabolite, tizoxanide (TZD), in human urine samples. The developed methodology is based on oxidizing NTX (non-fluorescence) into a highly fluorescent product by sodium hypochlorite. The fluorescence emission intensity was measured at 436.5 nm after fluorescence excitation at 362.5 nm. After optimizing all conditions, the analytical procedures and bio-analytical steps were evaluated and validated using ICH and FDA criteria, respectively. The method linearity, LOQ, and LOD values of NTX were 1.0-5.0 µg/mL, 0.434, and 0.143 µg/mL, respectively. The other novelty side of the presented work is the application of cobalt ferrite (CoFe2O4) nanoparticles (NPs) as a magnetic solid-phase for the pre-concentration and extraction process. The synthesized magnetic nanoparticles were characterized by scanning electron microscope and zeta sizer techniques. Finally, the utilized magnetic nanoparticles exhibited good recovery results for pre-concentration and extraction of NTX or its metabolite from spiked and real human urine samples, respectively.


Assuntos
Ácido Hipocloroso , Nanopartículas , Cobalto , Compostos Férricos , Corantes Fluorescentes , Humanos , Nitrocompostos , Oxirredução , Tiazóis
12.
Luminescence ; 37(6): 1001-1008, 2022 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-35412020

RESUMO

Selective fluorometric detection and determination of uranium ions is provided here using a novel fluorescent reagent, namely (E)-4-([4-hydroxynaphthalen-1-yl]diazenyl)-N-(5-methyleisoxazol-3-yl) benzenesulfonamide (UVI reagent). The UVI reagent offers a selective fluorescence enhancement behaviour at emission wavelength = 557 nm. The parameters affecting fluorometric detection of uranium ions, such as the pH, solvent type, ligand concentration, interaction time, and interfering ions, were investigated and adjusted. The proposed UVI reagent can detect and determine uranium ions even at low concentrations, for which the obtained limit of detection was 0.1 ppm. Additionally, this proposed determination protocol was successfully used to detect, monitor, and determine uranium ions in actual water samples.


Assuntos
Urânio , Íons , Espectrometria de Fluorescência , Sulfonamidas , Água
13.
Sci Rep ; 12(1): 6953, 2022 04 28.
Artigo em Inglês | MEDLINE | ID: mdl-35484380

RESUMO

Polyvinylpyrrolidone stabilized silver nanoparticles (PV-AgNPs) were synthesized from AgNO3/trisodium citrate and with the assistance of microwave energy. The synthesized PV-AgNPs were found to own an actual peroxidase mimicking activity. This catalytic activity can oxidize the non-fluorescence reagent (o-phenylenediamine) to a high fluorescence reaction product (2,3-diaminophenazine). The reaction product exhibited a fluorescence emission at 563 nm upon the excitation at 420. Among many metals, only mercury (II) ions can inhibit the catalytic activity of PV-AgNPs nanozyme. Accordingly, the fluorescence intensity of the reaction product has been successfully quenched. This quenching effect in the fluorescence intensity was directly proportional to the concentration of mercury (II). Depending on this finding, a simple, cost-effective, and selective spectrofluorimetric approach has been designed for mercury (II) detection in water samples. The linear relationship between the inhibition in fluorescence intensity and mercury (II) concentration was found in 20-2000 nM with a detection limit of 8.9 nM.


Assuntos
Mercúrio , Nanopartículas Metálicas , Peróxido de Hidrogênio , Íons , Peroxidases , Fenilenodiaminas , Prata
14.
Luminescence ; 37(3): 448-454, 2022 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-35023289

RESUMO

In this study, a fluorescence azothiazol-benzenesulfonamide derivative (M-sensor) was prepared for the determination of Mg2+ ions in different samples. The utilized M-sensor exhibited an emission fluorescence activity at 587 nm upon excitation at 537 nm. The developed method was based on the quenching effect of Mg2+ ions on the fluorescence intensity of the M-sensor with the above-mentioned fluorescence features. Furthermore, the utilized M-sensor was complexed with Mg2+ ions in the molar ratio of 1:1 (Mg2+ to M-sensor) and the selectivity of M-sensor toward Mg2+ against other metals ions, and the reversibility and reusability of the sensor were studied and verified. After optimization of the fluorometric detection, the quenching effect was directly proportional to the increase in the concentration of Mg2+ in the linear range 100-600 ng ml-1 with a limit of detection value of 18 ng ml-1 . The fluorescence sensor was successfully applied with good recovery for the determination of Mg2+ in water samples and different pharmaceutical samples (ampoules and suspension) without any interference from aluminium.


Assuntos
Magnésio , Água , Íons , Espectrometria de Fluorescência/métodos , Sulfonamidas
15.
Spectrochim Acta A Mol Biomol Spectrosc ; 264: 120258, 2022 Jan 05.
Artigo em Inglês | MEDLINE | ID: mdl-34384994

RESUMO

In this study, a facile nanoparticle catalytic sensor for resonance Rayleigh scattering quantification of mercury (II) ion was developed. The developed approach is relied on the selective inhibition of the peroxidase-like activity of polyvinylpyrrolidone-stabilized silver nanoparticles (PVP-Ag-NPs) by mercury (II) ions. The synthesized PVP-Ag-NPs oxidize the aqueous solution of O-Phenylenediamine (colorless) to 2,3-phenazinediamine (bright yellow) and their resonance Rayleigh scattering (RRS) activity was completely suppressed. When mercury (II) was introduced, the RRS activity of PVP-Ag-NPs was turned on combined with a reduction of the intensity of the yellow color. The enhancement in the RRS intensity was related to the concentration of mercury (II) in the linear range of 10-2000 nM. The smaller size (4.5 nm), the large surface area and the uniform size (PDI = 0.379) of the synthesized PVP-Ag-NPs offered a higher chance for interaction between mercury (II) and PVP-Ag-NPs with the advantages of high sensitivity (LOD = 4 nM) and excellent selectivity for mercury (II) detection over several metals and anions.


Assuntos
Mercúrio , Nanopartículas Metálicas , Fenilenodiaminas , Prata , Água
16.
Luminescence ; 36(6): 1544-1552, 2021 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-34080773

RESUMO

In this study, rapid resonance Rayleigh scattering (RRS), spectrophotometric, and spectrofluorimetric methods were performed for facile quantitation of daclatasvir dihydrochloride without interference from sofosbuvir (a co-formulated anti-hepatitis C virus drug). The proposed approaches were based on forming a binary complex between daclatasvir dihydrochloride and merbromin reagent at pH 4.1. The binary complex was measured spectrophotometrically at λmax = 544 nm. The spectrofluorimetric approach relied on the quenching effect of daclatasvir dihydrochloride on the fluorescence strength of merbromin at λEmission = 545 nm. The RRS approach depended on augmentation in the merbromin RRS spectrum at 363 nm upon addition of daclatasvir dihydrochloride. The presented methodologies were linear over the concentration ranges 2.5-15.0, 0.2-1.6 and 0.15-3.0 µg ml-1 with detection limits of 0.45, 0.046, and 0.036 µg ml-1 for the spectrophotometric approach, the spectrofluorometric approach, and RRS approach, respectively. Current approaches were validated in compliance with International Council for Harmonisation guidelines and utilized practically to estimate daclatasvir dihydrochloride either in binary mixtures with sofosbuvir or in its commercial tablet dosage form with good results. Moreover, the test for content uniformity was applied successfully on commercial tablets using the current spectroscopic approaches.


Assuntos
Merbromina , Sofosbuvir , Carbamatos , Imidazóis , Pirrolidinas , Espectrometria de Fluorescência , Comprimidos , Valina/análogos & derivados
17.
Spectrochim Acta A Mol Biomol Spectrosc ; 258: 119806, 2021 Sep 05.
Artigo em Inglês | MEDLINE | ID: mdl-33933938

RESUMO

α-Difluoromethylornithine or Eflornithine is an FDA-approved drug used for the treatment of Sleeping Sickness (as vials dosage form) and also used for diminishing the unwanted excess facial hair in the hirsutism (as creams dosage form). The proposed work is based on the condensation interaction between the amino moiety of Eflornithine and O-phthalaldehyde/2-mercaptoethanol to form a highly fluorescent isoindole derivative. The fluorescence and the Resonance Rayleigh Scattering (RRS) intensities of the reaction product were greatly augmented upon the addition of hexadecyl-trimethyl ammonium bromide by 153% and 250%, respectively. After optimization of the reaction conditions, the formed isoindole derivative was measured fluorometrically at λemission= 429 nm after λexcitation= 337 nm. Moreover, the significant augmentation in the RRS intensity of the formed product was measured at λmax= 422 nm. In regards to accuracy, sensitivity, robustness and precision, the proposed methods were validated according to ICH guidelines. Furthermore, the proposed methods were successfully applied for the assay of Eflornithine in various commercial brands of the pharmaceutical cream samples with good recovery. In addition to the current fluorometric method was confirmed to be effective in the assaying of Eflornithine in spiked plasma and urine specimens with good recovery.


Assuntos
Eflornitina , Micelas , Hirsutismo , Humanos , Isoindóis , Espectrometria de Fluorescência
18.
R Soc Open Sci ; 8(5): 210366, 2021 May 12.
Artigo em Inglês | MEDLINE | ID: mdl-34040792

RESUMO

Eflornithine (EFN) is an anti-Trypanosoma brucei agent for the medication of sleeping sickness and widely distributed for the treatment of hirsutism (unwanted facial hair in women). The presented work demonstrates a comprehensive analytical approach for the spectrofluorometric determination of EFN in commercial cream samples and various biological samples. The proposed method is based on the formation of a highly yellow-green fluorescence dihydropyridine derivative after the interaction between EFN and acetylacetone/formaldehyde reagent in a slightly acidic medium. Furthermore, the optimal variables such as reagent volumes, pH of the medium, heating time, buffer volume, heating temperature and diluting solvent were carefully selected to achieve the maximum fluorescence activity. The fluorescence activity for the formed derivative was measured at λ emission = 477 nm after λ excitation = 418 nm. Concerning linearity, accuracy, sensitivity, precision and robustness, the presented method was validated and verified according to ICH guidelines. Moreover, the proposed work offered a selective determination for EFN in various brands of pharmaceutical cream without any interference from excipients. Eventually, the current approach was assured to be successful in the estimation of EFN in urine and plasma samples with acceptable recovery results.

19.
J Chromatogr Sci ; 59(7): 634-641, 2021 Jun 21.
Artigo em Inglês | MEDLINE | ID: mdl-33634316

RESUMO

An innovative thin-layer chromatography method coupled with the fluorescence detection was developed for a specific estimation of ledipasvir. The separation was achieved on plates of silica gel 60 F254 using ethylacetate: hexane: acetonitrile: triethylamine; (6: 3.5: 1.5: 0.5, $\mathrm{v}/\mathrm{v}/\mathrm{v}/\mathrm{v}$) as a mobile phase system. The method involved the exposure of the developed thin-layer chromatography plate of ledipasvir to strong ultraviolet irradiation, resulting in a great enhancement in the fluorescence properties of ledipasvir. The irradiated plates were scanned after the excitation at 315 $\mathrm{nm}$. The method provided a sufficient separation of ledipasvir from sofosbuvir with ${R}_F$values of 0.28 and 0.36 for ledipasvir and sofosbuvir, respectively. The developed procedures were validated based on guidelines from the International Conference on Harmonization and Food and Drug Administration guidelines. The calibration curve was linear over the range of 5-50 $\mathrm{ng}/\mathrm{band}$. The excellent analytical features of the proposed method allow to the specific determination of ledipasvir in pharmaceutical tablets without interference from sofosbuvir or excipients. As the main elimination route for ledipasvir is via the fecal excretion (86%), the method was applied for the estimation of ledipasvir in fecal specimens with adequate recovery. In addition, the proposed method was applied for testing the content uniformity of ledipasvir in the pharmaceutical tablets.


Assuntos
Benzimidazóis/análise , Cromatografia em Camada Delgada/métodos , Fezes/química , Fluorenos/análise , Animais , Benzimidazóis/química , Benzimidazóis/efeitos da radiação , Fluorenos/química , Fluorenos/efeitos da radiação , Limite de Detecção , Modelos Lineares , Masculino , Ratos , Reprodutibilidade dos Testes , Espectrometria de Fluorescência , Comprimidos , Fatores de Tempo , Raios Ultravioleta
20.
R Soc Open Sci ; 8(1): 201545, 2021 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-33614086

RESUMO

Terbinafine hydrochloride is a potent antifungal drug indicated for oral and topical treatment of mycoses. A resonance Rayleigh scattering (RRS) method was developed for the determination of terbinafine hydrochloride through a feasible complexation reaction with erythrosine B. In a weakly acidic medium (acetate buffer, pH 5.0), terbinafine hydrochloride can react with erythrosine B through the electrostatic attraction and virtue of hydrophobic force to form an ion-association complex. The reaction resulted in the appearance of a new RRS peak at 369 nm. The RRS peak was increased by increasing the concentration of terbinafine hydrochloride in the linear range of 0.1-1.5 µg ml-1. All the reaction conditions (erythrosine B concentration, buffer volume, diluting solvent and pH) were optimized. The detection limit was 0.029 µg ml-1 while the quantitation limit was 0.089 µg ml-1. The suggested method after its validation was successfully applied for the determination of terbinafine hydrochloride in different pharmaceutical formulations (tablets and cream) with sufficient recovery.

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