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A simple and facile microwave-assisted method was developed for the synthesis of highly fluorescent silver-nanoparticles (Ag-NPs). The synthesis of silver-nanoparticles depends on a redox reaction between silver nitrate and ascorbic acid using chitosan as a stabilizing agent. The produced Ag-NPs were characterized using Zeta potential and transmission electron microscope micrograph where they are spherical in shape with smooth surface morphology and size of 26.81 ± 2.2 nm. Favipiravir (FAV) was found to cause an obvious enhancement in the fluorescence of Ag-NPs; hence, they were used for its spectrofluorimetric estimation. The fluorescence intensity was measured at 430 nm after excitation at 360 nm. Under optimum conditions, a good linear relationship was accomplished between the FAV concentration and the fluorescence intensity in a range of (5.0-200.0) ng/mL with a limit of detection of 1.59 ng/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.
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This work introduces an extremely easy method for preparing luminescent carbon dots (CDs) at ambient temperature using 1,2-naphthoquinone sulphonate and ethylenediamine as precursors via self-exothermic reaction without energy input. The as-obtained CDs have a high quantum yield (34.1 %), a production yield of 21.2 %, and a small size diameter (3.44 nm). Various techniques (NMR, TEM, EDX-mapping, XPS, XRD, FT-IR, fluorescence, and UV-visible spectroscopy) were used to characterize the prepared CDs. The CDs exhibited an excitation-independent emission with λex of 275 nm, demonstrating their homogeneity and high purity. The anticancer drug vincristine (VCR) quantitively quenched the fluorescent signal of the synthesized CDs, allowing their application as the first fluorescent nano-sensor to determine VCR. The quenching effect was linear within the range of 0.2-5.0 µg mL-1, enabling the determination of VCR in vials, plasma, and for content uniformity testing with a detection limit of 0.06 µg mL-1. Moreover, the synthesized CDs were employed as a bio-sensing platform to detect VCR in cancer cells owing to their good selectivity, excellent biocompatibility, minimal cytotoxicity, and high stability. The fabrication of CDs with excellent properties at room temperature under mild conditions paves the way for new advancements in the room temperature synthesis of CDs and offers a highly efficient alternative to traditional synthesis approaches.
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A green and simple UPLC method was developed and optimized, adopting a factorial design for simultaneous determination of oseltamivir phosphate and remdesivir with dexamethasone as a co-administered drug in human plasma and using daclatasvir dihydrochloride as an internal standard within 5 min. The separation was established on UPLC column BEH C18 1.7 µm (2.1 × 100.0 mm) connected to UPLC pre-column BEH 1.7 µm (2.1 × 5.0 mm) at 50 °C with an injection volume of 10 µL. The photodiode array detector (PDA) was set at three wavelengths of 220, 315, and 245 nm for oseltamivir phosphate, the internal standard, and both dexamethasone and remdesivir, respectively. The mobile phase consisted of methanol and ammonium acetate solution (40 mM) adjusted to pH 4 in a ratio of 61.5:38.5 (v/v) with a flow rate of 0.25 mL min-1. The calibration curves were linear over 500.0-5000.0 ng mL-1 for oseltamivir phosphate, over 10.0-500.0 ng mL-1 and 500.0-5000.0 ng mL-1 for dexamethasone, and over 20.0-500 ng mL-1 and 500.0-5000.0 ng mL-1 for remdesivir. The Gibbs free energy and Van't Hoff plots were used to investigate the effect of column oven temperatures on retention times. Fluoride-EDTA anticoagulant showed inhibition activity on the esterase enzyme in plasma. The proposed method was validated according to the M10 ICH, FDA, and EMA's bioanalytical guidelines. According to Eco-score, GAPI, and AGREE criteria, the proposed method was considered acceptable green.
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Adenosina Monofosfato , Alanina , Dexametasona , Oseltamivir , Humanos , Dexametasona/sangre , Oseltamivir/sangre , Oseltamivir/análogos & derivados , Adenosina Monofosfato/análogos & derivados , Adenosina Monofosfato/sangre , Alanina/análogos & derivados , Alanina/sangre , Cromatografía Líquida de Alta Presión/métodos , Antivirales/sangreRESUMEN
The present work reports a sensitive, affordable, and ecologically friendly spectrofluorimetric method for the assessment of two antihypertensive medications, namely minoxidil and timolol. Blue-emitting sulfur and nitrogen co-doped carbon quantum dots (S,N-CQDs) were generated by exposing soluble starch and thiourea to a 15-minute microwave treatment. The so- prepared nanodots displayed fluorescence at 276/430 nm with a quantum yield of 22 %. Inspection of the so-prepared nano-sensor verified their doping with nitrogen and sulfur, and their size was in the range of 4.5-9.03 nm. The proposed method was found to be rectilinear in the range of 0.20-5.0 and 2.0-30.0 µg/mL, with LOQs of 0.16 and 0.82 µg/mL for minoxidil and timolol, respectively. The developed method was employed to assess the concentrations of minoxidil and timolol in their pharmaceutical formulations, with %recoveries varying between 99.00 % and 101.94 %, and low RSD values (less than 2 %). The high sensitivity of the developed method allowed its use for timolol measurement in artificial aqueous humor, with % recoveries between 97.60 %.and 101.57 %. The study further examined how each analyte interacted with the prepared dots, leading to a quenching of their fluorescence. Additionally, an interference study was utilized to evaluate the specificity of the proposed approach through determining analyte levels in the existence of common additives, co-formulated drugs, and co-administered drugs. The analytical eco-scale, GAPI and AGREE assessment techniques were utilized to confirm the suggested method greenness.
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BACKGROUND: Nitroxinil has been used extensively to treat parasitic worms, mainly Fasciola, in food-producing cattle and sheep. The reported methods for nitroxinil analysis included expensive instrumentation, the need for skilled operators, and tedious procedures. Fluorimetry is one of the fastest and simplest methods widely used; hence, we aimed to develop a simple, cost-effective, and convenient fluorometric approach for the estimation of nitroxinil in various matrices. Compared with other detection methods, self-ratiometric fluorescent probes are considered a promising approach for the detection of analytes as their detection accuracy overcomes traditional fluorescence sensing probe in that it is not affected by the probe concentration, solution polarity, instrument parameters, and other factors. In this research, room temperature instantaneously synthesized carbon dots were used as a sensitive and selective self-ratiometric probe for the determination of the veterinary medicine nitroxinil in various matrices. RESULTS: A room-temperature synthesized quinone-ethanolamine carbon dots (RTQECDs) was fabricated using the instantaneous reaction of sodium 1,2-naphthoquinone-4-sulfonate (Folin's) with ethanolamine, without any energy/catalyzing reagents, for the first time. The prepared carbon dots show green-blue fluorescence at 450 nm upon exposure to UV light at 365 nm with a quantum yield of 26.6 %. Upon interaction with nitroxinil, the fluorescence intensity of RTQECDs at 450 nm is quenched and shifted to a longer wavelength at 475 nm. Meanwhile, the fluorescence of RTQECDs at 400 nm (absorbance maxima of nitroxinil) was more extremely quenched under the same conditions. Taking this in hand, a new RTQECDs self-ratiometric probe was developed for the determination of nitroxinil using the decrease in peaks at 450 nm and 400 nm and the shift of the fluorescence maxima to 475 nm as built-in reference peaks. The probe showed a quantitative increase in signal output of F475/F400 in the range of 0.10-30.0 µg/mL nitroxinil with a limit of detection of 30.0 ppb. The nitroxinil-sensing mechanism using RTQECDs is mainly ascribed to the partial secondary blue-type inner filter effect (IFE). The designed study was applied for the estimation of nitroxinil in veterinary dosage forms (recoveries; 99.78 %-100.35 %), river water (recoveries; 98.55 %-101.53 %), and food products, including meat, liver, kidney, and milk (recoveries; 97.60 %-104.25 %). SIGNIFICANCE: The novelty of our work includes the immediate synthesis of the sensing probe at room temperature, as well as its use as a self-ratiometric fluorescence probe for the determination of nitroxinil in veterinary samples, river water, and food products with excellent sensitivity down to 30.0 ppb. RTQECDs own the highest response and selectivity to nitroxinil compared with cations, anions, as well as other co-administered drugs, including cefotaxime and ivermectin.
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Carbono , Etanolamina , Leche , Puntos Cuánticos , Temperatura , Animales , Leche/química , Carbono/química , Puntos Cuánticos/química , Etanolamina/química , Etanolamina/análisis , Espectrometría de Fluorescencia , Colorantes Fluorescentes/química , Bovinos , Análisis de los Alimentos/métodos , Agua/química , Límite de Detección , Contaminación de Alimentos/análisisRESUMEN
Biocompatible and highly fluorescent phosphorus, nitrogen and sulfur carbon quantum dots (P,N,S-CQDs) were synthesized using a quick and ecologically friendly process inspired from plant sources. Garlic and red lentils were utilized as natural and inexpensive sources for efficient synthesis of the carbon-based quantum dots using green microwave-irradiation, which provides an ultrafast route for carbonization of the organic biomass and subsequent fabrication of P,N,S-CQDs within only 3 min. The formed P,N,S-CQDs showed excellent blue fluorescence at λem = 412 nm when excited at 325 nm with a quantum yield up to 26.4%. These fluorescent dots were used as a nano-sensor for the determination of the commonly used antibacterial and antiprotozoal drug, metronidazole (MTR). As MTR lacked native fluorescence and prior published techniques had several limitations, the proposed methodology became increasingly relevant. This approach affords sensitive detection with a wide linear range of 0.5-100.0 µM and LOD and LOQ values of 0.14 µM and 0.42 µM, respectively. As well as, it is cost-effective and ecologically benign. The MTT test was used to evaluate the in-vitro cytotoxicity of the fabricated P,N,S-CQDs. The findings supported a minimally cytotoxic impact and good biocompatibility, which provide a future perspective for the applicability of these CQDs in biomedical applications.
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Carbono , Colorantes Fluorescentes , Ajo , Metronidazol , Microondas , Puntos Cuánticos , Puntos Cuánticos/química , Ajo/química , Carbono/química , Colorantes Fluorescentes/química , Colorantes Fluorescentes/síntesis química , Metronidazol/análisis , Metronidazol/química , Metronidazol/farmacología , Humanos , Supervivencia Celular/efectos de los fármacosRESUMEN
Atorvastatin-an oral lipid regulating drug is a competitive inhibitor of 3-hydroxy-3-methylglutaryl coenzyme A reductase (HMG-CoA reductase), which is the rate determining enzyme for cholesterol synthesis. Adenine is a purine nucleobase that is found in deoxyribonucleic acid (DNA) and ribonucleic acid (RNA) to generate genetic information. The binding mechanism of atorvastatin and adenine was studied for the first time utilizing various techniques, including UV-visible spectrophotometry, spectrofluorimetry, synchronous fluorescence spectroscopy (SF), Fourier transform infrared (FTIR), fluorescence resonance energy transfer (FRET), and metal ion complexation. The fluorescence spectra of the complex indicated that atorvastatin is bound to adenine via hydrophobic interaction through a spontaneous binding process, and the fluorescence quenching mechanism was found to be static quenching with a binding constant of 1.4893 × 104 Lmol-1 at 298 K. Various temperature settings were used to investigate thermodynamic characteristics, such as binding forces, binding constants, and the number of binding sites. The interaction parameters, including the standard enthalpy change (ΔHο) and standard entropy change (ΔSο) were calculated using Van't Hoff's equation to be 42.82 kJmol-1 and 208.9 Jmol-1K-1, respectively. The findings demonstrated that the adenine- atorvastatin binding was endothermic. Furthermore, the results of the experiments revealed that some metal ions (K+, Ca+2, Co+2, Cu+2, and Al+3) facilitate the binding interaction between atorvastatin and adenine. Slight changes are observed in the FTIR spectra of adenine, indicating the binding interaction between adenine and atorvastatin.
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Favipiravir (FVP) is an oral antiviral drug approved in 2021 for the treatment of COVID-19. It is a pyrazine derivative that can be integrated into anti-viral RNA products to inhibit viral replication. While, adenine is a purine nucleobase that is found in deoxyribonucleic acid (DNA) and ribonucleic acid (RNA) to generate genetic information. For the first time, the binding mechanism between FVP and adenine was determined using different techniques, including UV-visible spectrophotometry, spectrofluorimetry, synchronous fluorescence (SF) spectroscopy, Fourier transform infrared (FTIR), fluorescence resonance energy transfer (FRET), and metal ion complexation. The fluorescence spectra indicated that FVP is bound to adenine via Van der Waals forces and hydrogen bonding through a spontaneous binding process (ΔGο < 0). The quenching mechanism was found to be static. Various temperature settings were used to investigate thermodynamic characteristics, such as binding forces, binding constants, and the number of binding sites. The reaction parameters, including the enthalpy change (ΔHο) and entropy change (ΔSο), were calculated using Van't Hoff's equation. The findings demonstrated that the adenine-FVP binding was endothermic. Furthermore, the results of the experiments revealed that some metal ions (K+, Ca+2, Co+2, Cu+2, and Al+3) might facilitate the binding interaction between FVP and adenine. Slight changes are observed in the FTIR spectra of adenine, indicating the binding interaction between adenine and FVP. This study may be useful in understanding the pharmacokinetic characteristics of FVP and how the drug binds to adenine to prevent any side effects.
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Nucleótidos de Adenina , Amidas , Antivirales , Pirazinas , Termodinámica , Pirazinas/química , Pirazinas/metabolismo , Amidas/química , Amidas/metabolismo , Nucleótidos de Adenina/química , Nucleótidos de Adenina/metabolismo , Antivirales/química , Antivirales/farmacología , Antivirales/metabolismo , Espectroscopía Infrarroja por Transformada de Fourier , Espectrometría de Fluorescencia , Transferencia Resonante de Energía de Fluorescencia , Espectrofotometría Ultravioleta , Sitios de Unión , Adenina/química , Adenina/metabolismoRESUMEN
Herein, we developed a rapid, one-step, and cost-effective methodology based on the fabrication of water-soluble self-nitrogen, sulfur, and phosphorus co-doped black seed carbon quantum dots (BSQDs) via microwaveirradiation in six minutes. Our synthesis approach is superior to those in the literature as they involved long-time heating (12 h) with sulfuric acid and sodium hydroxide and/or high temperatures (200 °C). A full factorial design was applied to obtain the most efficient synthesis conditions.BSQDs displayed excitation-independent emissions, demonstrating the purity of the synthesized BSQDs, with a maximum fluorescence at 425 nm after excitation at 310 nm. Eltrombopag olamine is an anti-thrombocytopenia drug that is also reported to cause toxicity in river water based on its Persistence, Bioaccumulation, and Toxicity (PBT). The synthesized BSQDs were employed as the first fluorometric sensor for environmental and bioanalysis of eltrombopag. The fluorescence of BSQDs decreased with increasing concentrations of eltrombopag, with excellent selectivity and sensitivity down to 30 ppb. BSQDs were successfully applied as sensing probes for the detection of eltrombopag in medical tablets, spiked and real human plasma samples, and river water samples, with an overall recovery of at least 97 %. The good tolerance to high levels of foreign components and co-administered drugs indicates good selectivity and versatility of the proposed methodology. Plasma pharmacokinetic parameters such as t1/2, Cmax, and t max of eltrombopag were evaluated to be 9.91 h, 16.0 µg mL-1, and 5 h, respectively. Moreover, the green character of the BSQDs as a sensor was proved by various analytical greenness scales.
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Benzoatos , Carbono , Pirazoles , Puntos Cuánticos , Puntos Cuánticos/química , Carbono/química , Pirazoles/química , Pirazoles/sangre , Benzoatos/química , Benzoatos/sangre , Humanos , Espectrometría de Fluorescencia/métodos , Animales , Nitrógeno/química , Límite de Detección , Fósforo/química , HidrazinasRESUMEN
One of the most common features of many different clinical conditions is pain; hence, there is a crucial need for eliminating or reducing it to a tolerable level to retrieve physical, psychological and social functioning. A first derivative synchronous spectrofluorimetry technique is proposed for the simultaneous determination of celecoxib and tramadol HCl, a recent coformulation authorized for treating acute pain in adults. The method includes using synchronous spectrofluorimetry at ∆λ = 80 nm where tramadol HCl was determined using first derivative technique at λ = 230.2 nm, while celecoxib was determined at λ = 288.24 nm. The proposed method was successfully applied to their co-formulated dosage forms in addition to spiked human plasma and validated in agreement with the guidelines of the International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH). The linear ranges were found to be 0.50-5.0 and 0.15-0.50, the limits of detection to be 0.088 and 0.011 and the limits of quantification to be 0.266 and 0.032 µg/ml for celecoxib and tramadol, respectively. Statistical analysis revealed no significant difference when compared with previously reported methods as evidenced by the values of the variance ratio F-test and Student t-test. The proposed method was successfully applied to commercial dosage forms and spiked human samples. Moreover, the greenness of the proposed method was investigated based on the analytical eco-scale approach, with the results showing an excellent green scale with a score of 95.
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Celecoxib , Espectrometría de Fluorescencia , Tramadol , Celecoxib/sangre , Celecoxib/análisis , Tramadol/sangre , Tramadol/análisis , Humanos , Espectrometría de Fluorescencia/métodos , ComprimidosRESUMEN
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.
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Puntos Cuánticos , Humanos , Puntos Cuánticos/química , Torasemida , Carbono/química , Nitrógeno/química , Urea , Sacarosa , Colorantes Fluorescentes/químicaRESUMEN
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.
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Antipsicóticos , Puntos Cuánticos , Colorantes Fluorescentes/química , Puntos Cuánticos/química , Fenotiazinas , Carbono/química , Nitrógeno/química , Azufre/químicaRESUMEN
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.
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Coccidiostáticos , Coccidiostáticos/análisis , Cromatografía Líquida de Alta Presión , Ionóforos/análisis , Aminoácidos , Monensina/análisisRESUMEN
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.
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Omeprazol , Comprimidos/química , Límite de Detección , Espectrometría de Fluorescencia/métodosRESUMEN
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.
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Anemia , Linfoma , Leucemia-Linfoma Linfoblástico de Células Precursoras , Adulto , Humanos , Metotrexato/efectos adversos , Egipto , Polimorfismo de Nucleótido Simple , Linfoma/tratamiento farmacológico , Genotipo , Anemia/tratamiento farmacológico , Metilenotetrahidrofolato Reductasa (NADPH2)/genética , Leucemia-Linfoma Linfoblástico de Células Precursoras/tratamiento farmacológico , Leucemia-Linfoma Linfoblástico de Células Precursoras/genéticaRESUMEN
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.
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Codeína/análogos & derivados , Guaifenesina , Espectrometría de Fluorescencia/métodos , Composición de Medicamentos , MorfolinasRESUMEN
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.
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Indoles , Salmón , Masculino , Animales , Simulación del Acoplamiento Molecular , Salmón/metabolismo , Dicroismo Circular , Espectrometría de Fluorescencia/métodos , Espectrofotometría Ultravioleta , Semen/metabolismo , ADN/química , Termodinámica , Inhibidores de Proteínas QuinasasRESUMEN
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.
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Nanopartículas , Puntos Cuánticos , Puntos Cuánticos/química , Nanotecnología , Luminiscencia , Preparaciones FarmacéuticasRESUMEN
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.
Asunto(s)
Eritrosina , Colorantes de Alimentos , Humanos , Eritrosina/química , Sunitinib , Composición de Medicamentos , Espectrometría de Fluorescencia/métodosRESUMEN
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.