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1.
Spectrochim Acta A Mol Biomol Spectrosc ; 314: 124207, 2024 Jun 05.
Artigo em Inglês | MEDLINE | ID: mdl-38554691

RESUMO

In the current work, sulfur and nitrogen co-doped carbon dots (S,N-CDs) as simple, sensitive, and selective turn-off fluorescent nanosensors were utilized for analysis of three phenothiazine derivatives, including acetophenazine (APZ), chlorpromazine (CPH), and promethazine (PZH). S,N-CDs were synthesized through a green one-pot microwave-assisted technique using widely available precursors (thiourea and ascorbic acid). HRTEM, EDX, FTIR spectroscopy, UV-Vis absorption spectroscopy, and fluorescence spectroscopy were used to characterize the as-synthesized CDs. When excited at 330 nm, the carbon dots produced a maximum emission peak at 410 nm. The cited drugs statically quenched the S,N-CDs fluorescence as revealed by the Stern-Volmer equation. The current method represents the first spectrofluorimetric approach for the determination of the studied drugs without the need for chemical derivatization or harsh reaction conditions. The importance of the proposed work is magnified as the cited drugs do not have any fluorescent properties. The fluorescence of the developed sensor exhibited a linear response to APZ, CPH, and PZH in the concentration ranges of 5.0-100.0, 10.0-100.0, and 10.0-200.0 µM with detection limits of 1.53, 1.66, and 2.47 µM, respectively. The developed fluorescent probes have the advantages of rapidity and selectivity for APZ, CPH, and PZH analysis in tablets with acceptable % recoveries of (98.06-101.66 %). Evaluation of the method's greenness was performed using the Complementary Green Analytical Procedure Index (ComplexGAPI) and Analytical GREEnness metric (AGREE) metrics, indicating that the method is environmentally friendly. Validation of the proposed method was performed according to ICHQ2 (R1) guidelines.


Assuntos
Antipsicóticos , Pontos Quânticos , Corantes Fluorescentes/química , Pontos Quânticos/química , Fenotiazinas , Carbono/química , Nitrogênio/química , Enxofre/química
2.
Luminescence ; 39(3): e4710, 2024 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-38481364

RESUMO

A simple and facile microwave-assisted method was developed for the synthesis of highly fluorescent nitrogen-doped carbon quantum dots (N-CQDs) using sucrose and urea. The produced quantum dots exhibited a strong emission band at 376 nm after excitation at 216 nm with quantum yield of 0.57. The as-prepared N-CQDs were characterized using Fourier-transform infrared (FTIR) spectroscopy, transmission electron microscopy (TEM) images, and ultraviolet-visible (UV-visible) spectra. The average particle size was 7.7 nm. It was found that torsemide (TRS) caused an obvious quenching of the fluorescent N-CQDs; so, they were used for its spectrofluorometric estimation. An excellent linear correlation was found between the fluorescence quenching of N-CQDs and the concentration of the drug in the range of 0.10 to 1.0 µg/mL with limit of quantitation (LOQ) of 0.08 µg/mL and limit of detection (LOD) of 0.027 µg/mL. The method was successfully applied for the assay of the drug in its commercial tablets and spiked human plasma samples, and the results obtained were satisfactory. Complex GAPI was used for greenness assessment of the analytical procedures and the pre-analysis steps. Interference likely to be introduced from co-administered drugs was also studied.


Assuntos
Pontos Quânticos , Humanos , Pontos Quânticos/química , Torasemida , Carbono/química , Nitrogênio/química , Ureia , Sacarose , Corantes Fluorescentes/química
3.
Xenobiotica ; 54(2): 95-105, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38381003

RESUMO

Polymorphisms in genes coding folate-metabolising enzymes might alter the pharmacokinetics and sensitivity for methotrexate "MTX".The aim of the study aimed to investigate the influence of MTHFR C677T, DHFR19 Ins/del, GGH -401 C > T, and MTR A2756G polymorphisms on MTX toxicity and pharmacokinetics in Egyptian patients with Acute lymphoblastic leukaemia (ALL) or Non-Hodgkin lymphoma (NHL).Fifty adult Egyptian patients with ALL and NHL, treated with high dose MTX, were prospectively enrolled in the study. Clinical and biochemical data was collected objectively from medical records after each cycle of MTX. Plasma concentrations of MTX were measured after 72 h of initiation of infusion. Genotyping was done with a PCR-ARMS and PCR-RFLP assays.The MTHFR C677T T variants significantly increased the risk of leukopoenia, whereas the genotype MTHFR 677 C > T TT significantly associated with lymphocytopenia, thrombocytopenia, and anaemia. The genotype GGH-401 TT was significantly correlated with anaemia. Plasma MTX level was significantly higher in patients with MTR A2756G G variants.MTHFR polymorphism played the main role in MTX toxicities. The pharmacokinetics of MTX was affected by MTR polymorphism. GGH mutation was mainly concerned with anaemia. Pharmacogenetic testing are recommended to optimise MTX therapy.


Assuntos
Anemia , Linfoma , Leucemia-Linfoma Linfoblástico de Células Precursoras , Adulto , Humanos , Metotrexato/efeitos adversos , Egito , Polimorfismo de Nucleotídeo Único , Linfoma/tratamento farmacológico , Genótipo , Anemia/tratamento farmacológico , Metilenotetra-Hidrofolato Redutase (NADPH2)/genética , Leucemia-Linfoma Linfoblástico de Células Precursoras/tratamento farmacológico , Leucemia-Linfoma Linfoblástico de Células Precursoras/genética
4.
J Sep Sci ; 47(4): e2300761, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38403454

RESUMO

The combination of ionophoric coccidiostats and amino acids (AAs) is important in poultry feeding to enhance immunity and improve the growth and feed efficiency of birds suffering from coccidiosis. A simple, rapid, and economical high-performance liquid chromatography-ultraviolet detection (HPLC-UV) method for the simultaneous determination of three ionophoric coccidiostats, namely salinomycin (SAL), maduramicin (MAD), and monensin (MON) in addition to three AAs; L-tryptophan (L-TRP), alpha-ketoleucin (KLEU), and L-valine (L-VAL) in feed premixes was developed and validated. Chromatographic separation was achieved in less than 12 min using a phenyl hexyl column with a mobile phase consisting of acetonitrile/methanol/water (25:20:55, v/v/v) adjusted to pH 3 using phosphoric acid. Isocratic elution was performed at a flow rate of 1 mL/min with UV detection at 210 nm. The method showed good linearity in the ranges 0.50-5.0 mg/mL for MON, 0.20-2.0 mg/mL for MAD and SAL, 10.0-100.0 µg/mL for L-TRP and KLEU, and 50.0-500.0 µg/mL for VAL. The developed method was successfully applied to determine the studied analytes in feed premixes with good recoveries and precision. The good validation criteria of the proposed method allow its utilization in quality control laboratories.


Assuntos
Coccidiostáticos , Coccidiostáticos/análise , Cromatografia Líquida de Alta Pressão , Ionóforos/análise , Aminoácidos , Monensin/análise
5.
Luminescence ; 39(2): e4682, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38332466

RESUMO

A new, proven, economical spectrofluorimetric approach has been used to determine the proton pump inhibitor omeprazole (OMP). This innovative technique is based on the ability of OMP to quench the native fluorescence of the mercurochrome dye in an acidic (pH 3.6) solution. Because it was discovered that quenching is proportional to the drug concentration, this dye was used as a sensor for OMP detection. The fluorescence intensity was measured at 518/540 nm, and its linear response ranged from 0.2-10.0 µg/mL with a linear coefficient of 0.9999. The computation yielded a limit of quantification (LOQ) of 0.20 µg/mL and a limit of detection (LOD) of 0.07 µg/mL. Every circumstance and element impacting the reaction product was examined in detail. Pharmacopeial standards carried out the validation. The approved method investigated several commercial preparations and formulations, and the results were favorably compared with those provided by a reference method. According to United States Pharmacopeia (USP) rules, content consistency for two distinct formulations was evaluated.


Assuntos
Omeprazol , Comprimidos/química , Limite de Detecção , Espectrometria de Fluorescência/métodos
6.
Luminescence ; 39(1): e4660, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-38286595

RESUMO

Guaifenesin and pholcodine are frequently co-formulated in certain dosage forms. A new fast first derivative synchronous spectrofluorometric method has been used for their simultaneous analysis in mixtures. Here, first derivative synchronous spectrofluorometry enabled the successful simultaneous estimation of guaifenesin at 283 nm and pholcodine at 275 nm using a wavelength difference (Δλ) of 40 nm. The method was fully validated following International Council of Harmonization guidelines. For guaifenesin and pholcodine, linearity was determined within the corresponding ranges of 0.05-0.30 and 0.10-6.0 µg/ml. The two drugs were effectively analyzed using the developed approach in their respective formulations, and the results showed good agreement with those attained using reference methods. The method demonstrated excellent sensitivity, with detection limits down to 0.007 and 0.030 µg/ml and quantitation limits of 0.020 and 0.010 µg/ml for guaifenesin and pholcodine, respectively. Therefore, the procedure was successful in determining these drugs simultaneously in vitro in spiked plasma samples and syrup dosage form. The developed methodology also offered an environmentally friendly advantage by utilizing water as the optimal diluting solvent throughout the whole work. Different greenness approaches were investigated to ensure the method's ecofriendly properties.


Assuntos
Codeína/análogos & derivados , Guaifenesina , Espectrometria de Fluorescência/métodos , Composição de Medicamentos , Morfolinas
7.
J Biomol Struct Dyn ; 42(3): 1170-1180, 2024.
Artigo em Inglês | MEDLINE | ID: mdl-37079322

RESUMO

The study of the intermolecular binding interaction of small molecules with DNA can guide the rational drug design with greater efficacy and improved or more selective activity. In the current study, nintedanib's binding interaction with salmon sperm DNA (ssDNA) was thoroughly investigated using UV-vis spectrophotometry, spectrofluorimetry, ionic strength measurements, viscosity measurements, thermodynamics, molecular docking, and molecular dynamic simulation techniques under physiologically simulated conditions (pH 7.4). The obtained experimental results showed that nintedanib and ssDNA had an apparent binding interaction. Nintedanib's binding constant (Kb) with ssDNA, as determined using the Benesi-Hildebrand plot, was 7.9 × 104 M-1 at 298 K, indicating a moderate binding affinity. The primary binding contact forces were hydrophobic and hydrogen bonding interactions, as verified by the enthalpy and entropy changes (ΔH0 and ΔS0), which were - 16.25 kJ.mol-1 and 39.30 J mol-1 K-1, respectively. According to the results of UV-vis spectrophotometry, viscosity assays, and competitive binding interactions with ethidium bromide or rhodamine B, the binding mode of nintedanib to ssDNA was minor groove. Molecular docking and molecular dynamic simulation studies showed that nintedanib fitted into the B-DNA minor groove's AT-rich region with high stability. This study can contribute to further understanding of nintedanib's molecular mechanisms and pharmacological effects.


Assuntos
Indóis , Salmão , Masculino , Animais , Simulação de Acoplamento Molecular , Salmão/metabolismo , Dicroísmo Circular , Espectrometria de Fluorescência/métodos , Espectrofotometria Ultravioleta , Sêmen/metabolismo , DNA/química , Termodinâmica , Inibidores de Proteínas Quinases
8.
J Fluoresc ; 34(1): 119-138, 2024 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-37222883

RESUMO

Nanotechnology has emerged as one of the most potential areas for pharmaceutical analysis. The need for nanomaterials in pharmaceutical analysis is comprehended in terms of economic challenges, health and safety concerns. Quantum dots (QDs)or colloidal semiconductor nanocrystals are new groups of fluorescent nanoparticles that bind nanotechnology to drug analysis. Because of their special physicochemical characteristics and small size, QDs are thought to be promising candidates for the electrical and luminescent probes development. They were originally developed as luminescent biological labels, but are now discovering new analytical chemistry applications, where their photo-luminescent properties are used in pharmaceutical, clinical analysis, food quality control and environmental monitoring. In this review, we discuss QDs regarding properties and advantages, advances in methods of synthesis and their recent applications in drug analysis in the recent last years.


Assuntos
Nanopartículas , Pontos Quânticos , Pontos Quânticos/química , Nanotecnologia , Luminescência , Preparações Farmacêuticas
9.
J Sep Sci ; 46(22): e2300454, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-37697638

RESUMO

A method using micellar electrokinetic chromatography coupled with large-volume sample stacking for the determination of ticagrelol was developed and validated. The analysis was performed in a fused silica capillary (41.5 cm effective length, 50 µm diameter) with ultraviolet detection at 195 nm. The background electrolytes were 30 mM phosphate buffer of pH 3.0 with 120 mM sodium dodecylsulfate and 10 % (v/v) acetonitrile (120 s X 50 mbar; 20°C; -18 kV) and 30 mM borate buffer of pH 8.5 with 75 mM sodium dodecylsulfate (120 s X 50 mbar; 20°C; 25 kV); under acidic and alkaline conditions, respectively. The method was found to be reliable with respect to specificity, linearity of the calibration line (R2  > 0.99), repeatability (relative standard deviation 2.56%-3.34%), and accuracy (recovery in the range 101.21%-102.67%). The limits of detection and quantitation were 0.032, 0.071, and 0.087, 0.188 µg/mL, respectively. The method was successfully applied for the determination of ticagrelol concentrations in rat plasma and tablets with good recoveries and reproducibility. The presented method proved to be suitable for monitoring ticagrelor in rat plasma.


Assuntos
Cromatografia Capilar Eletrocinética Micelar , Ratos , Animais , Cromatografia Capilar Eletrocinética Micelar/métodos , Micelas , Reprodutibilidade dos Testes , Comprimidos , Sódio
10.
Luminescence ; 38(12): 2073-2085, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-37747151

RESUMO

Sunitinib is a tyrosine kinase inhibitor used for the treatment of renal cell carcinoma and gastrointestinal stromal tumors. In this study, two spectroscopic methods, spectrofluorometric and spectrophotometric, were utilized to quantify sunitinib in different matrices. In method I, the native fluorescence of erythrosine B was quenched by forming ion-pair complex with increasing quantities of sunitinib. This approach was utilized for measuring sunitinib in its dosage forms and spiked plasma. After excitation at 528 nm, the quenching of fluorescence is linearly related to the concentration across the range of 0.05-0.5 µg mL-1 at 550 nm in Britton-Robinson buffer (pH 4.0), with a correlation value of 0.9999 and a high level of sensitivity with detection limit down to 10 ng mL-1 . Method II relies on spectrophotometric measurements of the produced complex at 550 nm across a range of 0.5-10.0 µg mL-1 , with good correlation value of 0.9999. This method has a detection limit down to 0.16 µg mL-1 . The proposed methodologies were validated according to International Conference on Harmonization (ICH) guidelines with satisfactory results. The stoichiometry of the reaction was determined through the application of Job's method, while the mechanism of quenching was investigated by employing the Stern-Volmer plot. The designated methods were used to estimate sunitinib in its capsules and in spiked human plasma. Additionally, the statistical analysis of the data revealed no substantial differences when compared to previous reported spectroscopic method. Green assessment tools provide further details about the eco-friendly nature of the methods.


Assuntos
Eritrosina , Corantes de Alimentos , Humanos , Eritrosina/química , Sunitinibe , Composição de Medicamentos , Espectrometria de Fluorescência/métodos
11.
Methods Appl Fluoresc ; 11(4)2023 Aug 25.
Artigo em Inglês | MEDLINE | ID: mdl-37586384

RESUMO

Green, one-pot, quick, and easily synthesized nitrogen and sulfur co-doped carbon quantum dots (N,S-CDs) were obtained from cheap and readily available chemicals (sucrose, urea, and thiourea) using a microwave-assisted approach in about 4 min and utilized as a turn-off fluorescent sensor for estimation of natamycin (NAT). First, the effect of N and S doping on the microwave-synthesized CDs' quantum yield was carefully studied. CDs derived from sucrose alone failed to produce a high quantum yield; then, to increase the quantum yield, doping with heteroatoms was carried out using either urea or thiourea. A slight increase in quantum yield was observed upon using thiourea with sucrose, while an obvious enhancement of quantum yield was obtained when urea was used instead of thiourea. Surprisingly, using a combination of urea and thiourea together results in N,S-CDs with the highest quantum yield (53.5%), uniform and small particle size distribution, and extended stability. The fluorescent signal of N,S-CDs was quenched upon addition of NAT due to inner filter effect and static quenching in a manner that allowed for quantitative determination of NAT over a range of 0.5-10.0µg ml-1(LOD = 0.10µg ml-1). The N,S-CDs were applicable for determination of NAT in aqueous humor, eye drops, different environmental water samples, and bread with excellent performance. The selectivity study indicated excellent selectivity of the prepared N,S-CDs toward NAT with little interference from possibly interfering substances. In-silico toxicological evaluation of NAT was conducted to estimate its long-term toxicity and drug-drug interactions. Finally, the preparation of N,S-CDs, and analytical procedure compliance with the green chemistry principles were confirmed by two greenness assessment tools.


Assuntos
Natamicina , Pontos Quânticos , Pontos Quânticos/química , Carbono/química , Micro-Ondas , Ureia , Tioureia
12.
Luminescence ; 38(12): 1996-2006, 2023 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-37650746

RESUMO

A simple, selective, and eco-friendly synchronous fluorescence approach was introduced for the first time for the concurrent estimation of the anticancer combination therapy of bicalutamide and resveratrol. The method relies on measuring the synchronous fluorescence spectra of bicalutamide and resveratrol at 269 and 320 nm, respectively, using Δλ of 60 nm with ethanol as a green diluting solvent. The procedure was optimized, and the method was then fully validated. Excellent linearity (R2 > 0.999) with very low detection limits (0.044 and 2.001 ng/ml) were obtained for both drugs, allowing for their analysis in human plasma. The green profile of the suggested approach was evaluated using the green solvents selecting tool (GSST), spider diagram for greenness index assessment, green analytical process index (GAPI), and Analytical GREEnness (AGREE) metric tools. These assessment metrics confirmed that the developed approach met the maximum number of green requirements, recommending its application as a green substitute for the regular analysis of the concerned drugs in human plasma. The simplicity of sample measurement enables and substantially accelerates the analysis, resulting in lower costs, enhanced procedure accuracy, and lower environmental effect.


Assuntos
Anilidas , Etanol , Humanos , Resveratrol , Espectrometria de Fluorescência
13.
Methods Appl Fluoresc ; 11(4)2023 Jul 26.
Artigo em Inglês | MEDLINE | ID: mdl-37459863

RESUMO

A facile, simple, green and sensitive spectrofluorometric method was developed for determination of the calcimimetic drug cinacalcet hydrochloride. It is used for the treatment of hyperparathyroidism. The drug showed high native fluorescence intensity at 320 nm after excitation at 280 nm. The method was linear over the range of 5.0-400.0 ng ml-1with excellent correlation (R2= 0.9999). Limit of detection (LOD) and limit of quantitation (LOQ) values were 1.19 and 3.62 ng ml-1, respectively. The percentage recovery was found to be 100.42% ± 1.39 (n=8). The proposed method was successfully applied for determination of cinacalcet in spiked human plasma samples with % recoveries of (87.23 to 109.69%). Two recent greenness metrics (GAPI and Analytical Eco-Scale) were chosen to prove the eco-friendly nature of the method. Furthermore, the proposed method was successfully applied to dissolution study of commercial cinacalcet tablets. The interference likely to be introduced by some commonly co-administrated drugs such as metoprolol and itraconazole was studied; the tolerance limits were calculated.


Assuntos
Comprimidos , Humanos , Cinacalcete , Limite de Detecção
14.
Sci Rep ; 13(1): 11716, 2023 07 20.
Artigo em Inglês | MEDLINE | ID: mdl-37474596

RESUMO

Food and Drug Administration (FDA) recently approved co-formulated celecoxib and tramadol for the treatment of acute pain in adults. Three spectrophotometric methods were efficiently applied to estimate the co-formulated Celecoxib and Tramadol in their tablets; second derivative 2D-spectrophotometry technique (method I), induced dual-wavelength technique (method II) and dual-wavelength resolution technique (method III). The proposed methods were successfully validated following the International Council for Harmonisation (ICH) guidelines and statistically assessed based on the correlation coefficients, relative standard deviations as well as detection and quantitation limits. The obtained results revealed non-significant differences compared to the reported results as revealed by the variance ratio F test and Student t test. Moreover, the applied techniques were further assessed concerning their greenness based on the analytical eco-scale method revealing an excellent green scale with a final score of 95. The proposed spectrophotometric techniques could be applied for the routine analysis and quality control of the studied drugs in their dosage form.


Assuntos
Tramadol , Adulto , Humanos , Celecoxib , Espectrofotometria/métodos , Comprimidos/análise , Combinação de Medicamentos
15.
Methods Appl Fluoresc ; 11(4)2023 Jul 19.
Artigo em Inglês | MEDLINE | ID: mdl-37413998

RESUMO

The small molecular drugs pharmacodynamics and pharmacokinetics could be affected by human serum albumin (HSA) transport, so we studied the interaction between HSA and the widely used anti-ischemic agent, trimetazidine (TMZ), using different approaches. As shown by synchronous fluorescence spectroscopy, the interaction affects the microenvironment confirmation around tyrosine residues. The site-competitive experiments showed that TMZ had an affinity toward subdomain III A (site II) of HSA. The enthalpy and entropy changes (ΔH and ΔS), which were 37.75 and 0.197 K J mol-1, respectively, showed that the predominant intermolecular interactions are hydrophobic forces. According to FTIR research, the interaction between HSA and TMZ caused polypeptide carbonyl-hydrogen bonds to rearrange. The HSA esterase enzyme activity was decreased with TMZ. Docking analysis confirmed the site-competitive experiments and thermodynamic results. This study demonstrated that TMZ interacted with HSA, and the structure and function of HSA were influenced by TMZ. This study could aid in understanding the pharmacokinetics of TMZ and provide basic data for safe use.


Assuntos
Albumina Sérica Humana , Trimetazidina , Humanos , Trimetazidina/farmacologia , Sítios de Ligação , Ligação Proteica , Dicroísmo Circular , Simulação de Acoplamento Molecular
16.
Talanta ; 265: 124813, 2023 Dec 01.
Artigo em Inglês | MEDLINE | ID: mdl-37321162

RESUMO

Deep eutectic solvents (DESs) have recently sparked considerable attention in a variety of scientific and technological fields. The unique properties of DESs include biodegradability, easy preparation, low cost, and tuneability, rendering them a new and prospective alternative to hazardous solvents. Analytical chemistry is one of the most appealing fields where DESs proved to be applicable in either sample preparation or chromatographic separation. This review summarizes the new horizons dedicated to the application of DESs in microextraction and chromatographic separation. The utilization of DESs in microextraction, in chromatography as mobile phase additives, and in chromatographic material preparation processes is outlined. The enhancements in chromatographic performance achieved using DESs and any potential explanations deduced from the experimental findings were primarily discussed. An additional brief discussion on DESs preparation, characterization, and properties is addressed in this work. Finally, current challenges and future trends are also presented, supplying evidence for distinct possibilities regarding new research approaches involving DESs. This review can represent a guide and stimulate further research in this field.

17.
Spectrochim Acta A Mol Biomol Spectrosc ; 302: 123029, 2023 Dec 05.
Artigo em Inglês | MEDLINE | ID: mdl-37354857

RESUMO

In this work, resveratrol and curcumin, two natural polyphenols, were simultaneously determined in human plasma samples using a rapid, sensitive, green, and affordable synchronous fluorescence spectroscopic approach. Several factors affecting the performance of the procedure, including Δλ, pH, diluting solvent, and organized medium, were optimized. Based on the findings, the fluorescence of resveratrol and curcumin was measured at 304 and 443 nm, respectively, with Δλ of 80.0 nm and ethanol as the diluting solvent. Excellent linearity was demonstrated by the approach (r = 0.9999) over the concentration range of 5.00-1000.00 and 2.00-400.00 ng/mL for resveratrol and curcumin, respectively. The obtained detection limits for resveratrol and curcumin were 0.027 and 0.042 ng/mL, respectively, indicating the high sensitivity of the proposed method. Moreover, the method exhibited excellent precision (both inter and intra-day), with %RSD < 1 %. The "green analytical process index" and "Analytical GREEnness" metric tools were used to compare the green profiles of the proposed method to those of the published methods. These two greenness evaluation tools verified that the suggested methodology satisfied the greatest number of green criteria, proposing its usage as a green alternative for the routine analysis of the investigated natural anticancer polyphenols in human plasma.


Assuntos
Curcumina , Polifenóis , Humanos , Resveratrol , Espectrometria de Fluorescência/métodos , Solventes
18.
BMC Chem ; 17(1): 45, 2023 May 05.
Artigo em Inglês | MEDLINE | ID: mdl-37147652

RESUMO

A simple, selective, and sensitive RP-HPLC method was proposed for the simultaneous determination of two co-administered antidiabetic drugs (omarigliptin and metformin) with an anti-hyperlipidemic drug (ezetimibe) in a medicinally-recommended ratio of 2.5:50:1, respectively. The proposed procedure was optimized by adopting a quality-by-design approach. The influence of different factors on chromatographic responses was optimized by applying the two-level full factorial design (25). The optimum chromatographic separation was achieved using Hypersil BDS C18 column at 45 °C, and the mobile phase pumped isocratically composed of methanol: potassium dihydrogen phosphate buffer (6.6 mM; pH 7, 67:33% v/v) at a flow rate of 0.814 mL/min using 235 nm as a detection wavelength. The developed method was capable of separating this novel mixture in less than 8 min. The calibration plots of omarigliptin, metformin, and ezetimibe showed acceptable linearity over the ranges of 0.2-2.0, 0.5-25.0, and 0.1-2.0 µg/mL with quantitation limits of 0.06, 0.50, and 0.06 µg/mL, respectively. The proposed method was successfully applied to determine the studied drugs in their commercial tablets with high % recoveries (96.8-102.92%) and low % RSD values (less than 2%). The applicability of the method was extended to the in-vitro assay of the drugs in spiked human plasma samples with high % recoveries (94.3-105.7%). The suggested method was validated in accordance with ICH guidelines.

19.
Biomed Chromatogr ; 37(9): e5664, 2023 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-37114598

RESUMO

In this study, the development and validation of an accurate and highly sensitive LC-MS/MS method were performed for the estimation of nifedipine, bisoprolol and captopril in real human plasma. Liquid-liquid extraction using tert-butyl methyl ether was efficiently applied for extraction of the analytes from plasma samples. The chromatographic separation was carried out using an isocratic elution mode on the X-terra MS C18 column (4.6 × 50 mm, 3.5 µm). The mobile phase consisted of methanol-0.1% formic acid (95:5, v/v) for determination of nifedipine and bisoprolol and acetonitrile-0.1% formic acid (70:30, v/v) for determination of captopril with a flow rate of 0.5 ml/min. Acceptable results regarding the different validation characteristics of the analytes were obtained in accordance with US Food and Drug Administration recommendations for bioanalytical methods. The developed approach was linear over concentration ranges of 0.5-130.0, 50.0-4,500.0 and 0.3-30.0 ng/ml for nifedipine, captopril and bisoprolol, respectively. The method revealed a sufficient lower limit of quantification in the range of 0.3-50.0 ng/ml, as well as high recovery percentages, indicating high bioanalytical applicability. The proposed method was efficiently applied to a pharmacokinetic evaluation of a fixed-dose combination of the analytes in healthy male volunteers.


Assuntos
Bisoprolol , Captopril , Humanos , Masculino , Cromatografia Líquida/métodos , Nifedipino , Espectrometria de Massas em Tandem/métodos , Reprodutibilidade dos Testes
20.
Sci Rep ; 13(1): 5502, 2023 04 04.
Artigo em Inglês | MEDLINE | ID: mdl-37015951

RESUMO

In this study, highly fluorescent sulfur and nitrogen co-doped carbon quantum dots (SN-CQDs) were synthesized by a simple one-pot hydrothermal method using thiosemicarbazide and citric acid as starting materials. Various spectroscopic and microscopic techniques were applied to characterize the prepared SN-CQDs. The synthesized SN-CQDs' maximum fluorescence emission was obtained at 430 nm after excitation at 360 nm. Rifampicin (RFP), tinidazole (TNZ), ornidazole (ONZ), and metronidazole (MNZ) all quantitatively and selectively quenched the SN-CQDs' native fluorescence, which was the base-for their-spectrofluorimetric estimation without the need for any tedious pre-treatment steps or high-cost instrumentation. SN-CQDs demonstrated a "turn-off" fluorescence response to RFP, TNZ, ONZ, and MNZ over the ranges of 1.0-30.0, 10.0-200.0, 6.0-200.0, and 5.0-100.0 µM with detection limits of 0.31, 1.76, 0.57, and 0.75 µM and quantitation limits of 0.93, 5.32, 1.74, and 2.28 µM respectively. The suggested method was successfully used to determine the investigated drugs in their commercial dosage forms. The method was further extended to their determination in spiked human plasma samples, with satisfactory mean % recoveries (99.44-100.29) and low % RSD values (< 4.52). The mechanism of fluorescence quenching was studied and discussed. The suggested method was validated in accordance with ICH recommendations.


Assuntos
Corantes Fluorescentes , Pontos Quânticos , Humanos , Corantes Fluorescentes/química , Pontos Quânticos/química , Carbono/química , Nitrogênio/química , Espectrometria de Fluorescência/métodos , Enxofre/química
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