RESUMEN
Ionic microenvironment of the nasal secretions especially calcium ions play essential role in the olfactory transmission. However, there is a critical need to determine the free calcium levels in healthy people's nasal secretions in contrast to those of patients with olfactory impairment. A selective spectrofluorometric method was created to quantify nasal calcium levels utilizing its quenching ability to the fluorescence of the functionalized carbon quantum dots. The surface of carbon quantum dots was functionalized with calcium ionophore A23187 and ion association complex, calcium phosphotungstate, to improve the selectively to quantify calcium ions. The functionalized carbon quantum dots exhibited a concentration-dependent fluorescence quenching upon interaction with calcium ions. Different factors influencing the quenching process were done to provide efficient analytical process. The new method, demonstrated accurate calcium determination over the concentration range of 200-4000 ng/mL. The suggested technique was used to measure the calcium in the nasal secretions of both healthy people and patients with olfactory impairment. The findings revealed significantly higher calcium levels in the patient with olfactory dysfunction (healthy vs. patient; 735 ± 20 ng/mL vs. 2987 ± 37 ng/mL, p < 0.05).
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Calcio , Espectrometría de Fluorescencia , Humanos , Calcio/análisis , Calcio/metabolismo , Espectrometría de Fluorescencia/métodos , Puntos Cuánticos/química , Trastornos del Olfato/diagnóstico , Trastornos del Olfato/metabolismo , Mucosa Nasal/metabolismo , Mucosa Nasal/química , Masculino , Adulto , Olfato , FemeninoRESUMEN
Nasal ions environment plays a crucial role in maintaining nasal physiology and supports olfactory transmission. Addressing the limited research on nasal ion levels and their association with olfactory function, paper-based sensors were developed for determination of sodium, potassium, calcium and chloride in the nasal mucus of healthy volunteers and patients with olfactory dysfunction. Multi-walled carbon nanotubes and carbon quantum dots from beetroot were incorporated into paper substrate where sensors were designed with ion association complexes for sodium, potassium, calcium and chloride enhancing the recognition sensing capabilities. The sensors composition was optimized, including ion-exchange materials and plasticizers, to enhance sensitivity and selectivity. The performance of the sensors is evaluated based on Nernstian slope, dynamic range, detection limit and response time. Selectivity of the sensors was tested and the results demonstrated high selectivity for the target ions. The sensors were successfully determined sodium, potassium, calcium and chloride levels in nasal mucus of healthy volunteers and patients with olfactory dysfunction. The results revealed elevated calcium levels in patients with olfactory dysfunction, highlighting associated diagnostic implications. This suggests that the proposed sensors could serve as a diagnostic tool for olfactory evaluation, particularly in resource-constrained settings where access to advanced diagnostic tools is limited.
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Calcio , Papel , Humanos , Calcio/análisis , Calcio/metabolismo , Trastornos del Olfato/diagnóstico , Nanotubos de Carbono/química , Sodio/análisis , Sodio/metabolismo , Potasio/análisis , Iones/análisis , Puntos Cuánticos/química , Olfato , Cloruros/análisis , Mucosa Nasal/metabolismo , Masculino , AdultoRESUMEN
Ascorbic acid (Vitamin C) is crucial for bodily functions, including collagen synthesis, immune system support and antioxidant defense. Despite autism spectrum disorder's multifactorial nature involving genetic, environmental and neurological factors, robust evidence exploring the association between ascorbic acid and this disorder is notably lacking. This study introduces an innovative spectrofluorometric method to quantify ascorbic acid in the plasma of healthy children and those with autism spectrum disorder. The method relies on the interaction of ascorbic acid with the fluorescent dye propidium iodide. In acidic conditions, propidium iodide undergoes protonation and selectively binds to the negatively charged ascorbic acid forming an ion-pair complex. This complex alters the molecular structure of propidium iodide inducing chemical fluorescence quenching, that can be utilized for ascorbic acid quantification. The developed method undergoes rigorous validation following ICH guidelines, demonstrating a linear relationship within a concentration range of 4-40 µg/mL, with high precision and accuracy metrics. Analysis of real plasma samples from autistic and healthy children reveals clinically and statistically elevated levels of ascorbic acid in those with autism spectrum disorder.
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Ácido Ascórbico , Trastorno del Espectro Autista , Espectrometría de Fluorescencia , Ácido Ascórbico/sangre , Humanos , Trastorno del Espectro Autista/sangre , Espectrometría de Fluorescencia/métodos , Niño , Preescolar , MasculinoRESUMEN
Hypertension and hyperlipidemia are two common conditions that require effective management to reduce the risk of cardiovascular diseases. Among the medications commonly used for the treatment of these conditions, valsartan and pitavastatin have shown significant efficacy in lowering blood pressure and cholesterol levels, respectively. In this study, synchronous spectrofluorimetry coupled to chemometric analysis tools, specifically concentration residual augmented classical least squares (CRACLS) and spectral residual augmented classical least squares (SRACLS), was employed for the determination of valsartan and pitavastatin simultaneously. The developed models exhibited excellent predictive performance with relative root mean square error of prediction (RRMSEP) of 2.253 and 2.1381 for valsartan and pitavastatin, respectively. Hence, these models were successfully applied to the analysis of synthetic samples and commercial formulations as well as plasma samples with high accuracy and precision. Besides, the greenness and blueness profiles of the determined samples were also evaluated to assess their environmental impact and analytical practicability. The results demonstrated excellent greenness and blueness scores with AGREE score of 0.7 and BAGI score of 75 posing the proposed method as reliable and sensitive approach for the determination of valsartan and pitavastatin with potential applications in pharmaceutical quality control, bioanalytical studies, and therapeutic drug monitoring.
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Quinolinas , Espectrometría de Fluorescencia , Valsartán , Quinolinas/química , Quinolinas/sangre , Valsartán/química , Valsartán/sangre , Análisis de los Mínimos CuadradosRESUMEN
Attention deficit hyperactivity disorder (ADHD) is a neurological condition frequently identified in early childhood and frequently co-occurs with other neuropsychological disorders, particularly autism. Viloxazine hydrochloride, a non-stimulant medication, has recently gained approval for treating attention-deficit hyperactivity disorder. This paper describes the first spectrofluorimetric method for precisely measuring the content of viloxazine in pharmaceutical capsules and rat plasma. This method employed NBD-Cl (4-chloro-7-nitrobenzo-2-oxa-1,3-diazole) as a fluorescent probe, which transformed viloxazine in an alkaline environment into a remarkably sensitive fluorescent adduct. Upon excitation at 476 nm, this adduct becomes detectable at a wavelength of 536 nm. The method was validated using ICH criteria, revealing acceptable linearity across a concentration range of 200-2000 ng/ml and high sensitivity with LOD and LOQ values of 46.774 ng/ml and 141.741 ng/ml, respectively. This method was adeptly applied in a pharmacokinetic study of viloxazine in rat plasma following a single oral dose (10 mg/kg), yielding a mean peak plasma concentration (Cmax) of 1721 ng/ml, achieved within 1.5 h. Furthermore, the environmental impact of the technique was assessed using two greenness assessment tools, revealing a notable level of eco-friendliness and sustainability.
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Colorantes Fluorescentes , Espectrometría de Fluorescencia , Viloxazina , Animales , Ratas , Colorantes Fluorescentes/química , Viloxazina/química , Viloxazina/farmacocinética , Viloxazina/sangre , Masculino , Estructura Molecular , 4-Cloro-7-nitrobenzofurazano/química , Administración OralRESUMEN
In this study, the application of continuous wavelet transform as a signal processing technique for the spectrofluorimetric determination of rosuvastatin and losartan is investigated. Both rosuvastatin and losartan exhibited native spectrofluorometric signals with severe overlapping peaks, making their simultaneous determination challenging. To address this issue, rbio 2.4 wavelet transformation was employed to obtain zero-crossing points in the synchronous fluorescence spectra of losartan and rosuvastatin at 346 and 408 nm, respectively, making their quantification possible. The developed method was validated according to the ICH guidelines and displayed high accuracy, precision, and specificity. The method exhibited excellent linearity over concentration ranges 0.2-2.0 and 0.25-2.0 µg/mL for losartan and rosuvastatin, respectively. In addition, LOD and LOQ were 0.046 and 0.140 µg/mL for losartan and 0.036 and 0.110 µg/mL for rosuvastatin, respectively, indicating the high sensitivity of the developed method. Moreover, greenness and blueness assessments were carried, revealing a high AGREE score of 0.71 and BAGI score of 77.5 for the developed method, making it a promising greener alternative for the reported chromatographic methods. Finally, the developed method was applied to the determination of rosuvastatin and losartan in pharmaceutical formulations, posing it as a powerful greener alternative in quality control laboratories.
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Losartán , Rosuvastatina Cálcica , Espectrometría de Fluorescencia , Análisis de Ondículas , Rosuvastatina Cálcica/análisis , Losartán/análisis , Espectrometría de Fluorescencia/métodos , Límite de DetecciónRESUMEN
In this research, we focused on the production of amylose-lipid nanocomposite material (ALN) through a green synthesis technique utilizing high-speed homogenization. Our aim was to investigate this novel material's distinctive physicochemical features and its potential applications as a low-glycemic gelling and functional food ingredient. The study begins with the formulation of the amylose-lipid nanomaterial from starch and fatty acid complexes, including stearic, palmitic, and lauric acids. Structural analysis reveals the presence of ester carbonyl functionalities, solid matrix structures, partial crystallinities, and remarkable thermal stability within the ALN. Notably, the ALN exhibits a significantly low glycemic index (GI, 40%) and elevated resistance starch (RS) values. The research extends to the formulation of ALN into nanocomposite hydrogels, enabling the evaluation of its anthocyanin absorption capacity. This analysis provides valuable insights into the rheological properties and viscoelastic behavior of the resulting hydrogels. Furthermore, the study investigates anthocyanin encapsulation and retention by ALN-based hydrogels, with a particular focus on the influence of pH and physical cross-link networks on the uptake capacity presenting stearic-acid (SA) hydrogel with the best absorption capacity. In conclusion, the green-synthesized (ALN) shows remarkable functional and structural properties. The produced ALN-based hydrogels are promising materials for a variety of applications, such as medicine administration, food packaging, and other industrial purposes.
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Amilosa , Nanocompuestos , Amilosa/química , Hidrogeles/química , Antocianinas , Almidón/química , Nanocompuestos/química , NanogelesRESUMEN
Hypertension and hyperlipidemia frequently coexist and are correlated with elevated cardiovascular adverse outcomes. Fixed dose combination tablets containing antihypertensive and antihyperlipidemic drugs have the potential to improve patient compliance. Telmisartan and rosuvastatin fixed dose combination tablet has been recently formulated. This study provided the first fluorescence spectroscopic method for simultaneously quantifying telmisartan and rosuvastatin in tablet dosage form and plasma. The native fluorescence spectra of telmisartan and rosuvastatin completely overlapped, making direct measurement unachievable. However, through the implementation of synchronous fluorescence measurements of telmisartan and rosuvastatin at a Δλ = 60, distinct narrow bands were observed at 358 nm and 375 nm, respectively. Regrettably, the challenge of overlapping remained unresolved. Nevertheless, by converting these synchronous spectra into first-order spectra, the problem of overlapping was completely resolved. This conversion also allowed for the selective quantification of telmisartan and rosuvastatin at 374 nm and 358 nm, respectively. The validity of this method was confirmed in accordance with ICH guidelines, yielding satisfactory results in terms of the validation characteristics. The method demonstrated linear relationships between the response and the studied drugs concentrations in working range of 50-1000 ng/mL for telmisartan and 100-2000 ng/mL for rosuvastatin. The described methodology was applied for the pharmacokinetic study of telmisartan and rosuvastatin in rat plasma after a single oral dose of 4 mg/kg telmisartan and 50 mg/kg rosuvastatin. Pharmacokinetic analyses revealed a moderate drug-drug interaction between the two drugs, which was not considered to be clinically significant. Moreover, the described method was assessed in terms of sensitivity and environmental sustainability against three previously documented methods. The comparison effectively underscores the supremacy of the proposed technique over the documented techniques.
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Antihipertensivos , Humanos , Animales , Ratas , Rosuvastatina Cálcica , Telmisartán/efectos adversos , Fluorescencia , Comprimidos , Espectrometría de FluorescenciaRESUMEN
Velpatasvir and simeprevir are two direct acting antivirals that are often used in combination with sofosbuvir to treat HCV infections. Herein, an environmentally benign spectrofluorimetric method was developed for simultaneous quantification of velpatasvir and simeprevir in pharmaceutical and plasma samples. To address the issue of overlapping fluorescence spectra presented by these compounds, this method integrates synchronous fluorescence and second-derivative spectroscopy. By employing the second derivative of the synchronous fluorescence spectra measured at Δλ of 140 nm, the accurate determination of velpatasvir at 400 nm and simeprevir at 426 nm was achieved without any interference. Different experimental parameters affecting the synchronous fluorescence of the studied drugs were carefully optimized. The plots of second-derivative amplitudes against concentrations showed linearity in the range of 5-400 ng/mL for velpatasvir and 80-800 ng/mL for simeprevir. The method was very sensitive, with lower detection limits of 1.11 ng/mL and 25.40 ng/mL, and quantification limits of 3.36 ng/mL and 76.96 ng/mL for velpatasvir and simeprevir, respectively.The method was effectively used to determine velpatasvir and simeprevir simultaneously in their pure forms, pharmaceutical dosage forms, and human plasma with no interference. The suggested technique was additionally evaluated for its eco-friendliness through the utilization of the Analytical GREEnness (AGREE) and Green Analytical Procedure Index (GAPI) evaluation metrics, revealing that the method is indeed sustainable.
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Atomoxetine is a psychostimulant drug used for the treatment of attention-deficit/hyperactivity disorder (ADHD) symptoms in people with autism. Herein, eco-friendly fluorescent carbon quantum dots (CQDs) were synthesized using black-eyed pea beans and characterized for the purpose of quantifying atomoxetine in pharmaceutical capsules and human plasma. The selectivity of these CQDs towards atomoxetine was improved by functionalizing their surface with an atomoxetine-tetraphenylborate ion complex. The quantification of atomoxetine is based on measuring the fluorescence quenching of the functionalized CQDs in response to varying concentrations of atomoxetine. The Stern-Volmer plot was employed to investigate the mechanism through which atomoxetine quenches the fluorescence intensity of the CQDs. The outcomes indicated a dynamic quenching mechanism. The applied method was optimized and validated in compliance with ICH requirements, resulting in excellent linearity across the concentration range of 50-800 ng/mL. The developed method was successfully used to quantify atomoxetine in pharmaceutical dosage form and human plasma with acceptable accuracy and precision outcomes. In addition, the method was applied for clinical pharmacokinetic study of atomoxetine in the plasma of children diagnosed with both autism and ADHD. Atomoxetine was rapidly absorbed after a single oral dose of 10 mg, reaching maximum concentration within two hours and having a half-life (t1/2) of 3.11 h. Moreover, the method demonstrates a notable degree of eco-friendliness, as evidenced by two greenness evaluation metrics; Green Analytical Procedure Index (GAPI) and Analytical GREEnness (AGREE).
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Clorhidrato de Atomoxetina , Colorantes Fluorescentes , Puntos Cuánticos , Espectrometría de Fluorescencia , Clorhidrato de Atomoxetina/farmacocinética , Clorhidrato de Atomoxetina/sangre , Humanos , Puntos Cuánticos/química , Colorantes Fluorescentes/química , Colorantes Fluorescentes/farmacocinética , Espectrometría de Fluorescencia/métodos , Trastorno por Déficit de Atención con Hiperactividad/tratamiento farmacológico , Trastorno por Déficit de Atención con Hiperactividad/sangre , Niño , Masculino , Trastorno Autístico/tratamiento farmacológico , Reproducibilidad de los Resultados , Límite de DetecciónRESUMEN
This research investigates the effects of the immunotherapeutic agent nivolumab on the metabolism of lung cancer cells (NCI-H1975) using GC-MS metabolomic profiling. Multivariate analysis such as unsupervised PCA and supervised OPLS-DA along with univariate analysis and pathway analysis were employed to explore the metabolomic data and identify altered metabolic pathways induced by nivolumab treatment. The study revealed distinct metabolic alterations in cancer cells, linked to proliferative and survival advantages, such as enhanced glycolysis, increased glutaminolysis, and modified amino acid metabolism. Key findings indicate elevated levels of glycolysis-related metabolites (glycine, alanine, pyruvate, and lactate) and TCA cycle intermediates (succinate, fumarate, malate) in cancer cells, with a significant decrease following nivolumab treatment. Additionally, lower levels of aspartic acid and citrate in cancer cells imply altered nucleotide synthesis and fatty acid production essential for tumor growth. Treatment with nivolumab also reduced oleic acid levels, indicative of its effect on disrupted lipid metabolism. Our research shows nivolumab's potential to modify metabolic pathways involved in lung cancer progression, suggesting its dual role in cancer therapy: as an immune response modulator and a metabolic pathway disruptor.
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Carcinoma de Pulmón de Células no Pequeñas , Cromatografía de Gases y Espectrometría de Masas , Neoplasias Pulmonares , Redes y Vías Metabólicas , Metabolómica , Nivolumab , Humanos , Carcinoma de Pulmón de Células no Pequeñas/tratamiento farmacológico , Carcinoma de Pulmón de Células no Pequeñas/metabolismo , Cromatografía de Gases y Espectrometría de Masas/métodos , Nivolumab/uso terapéutico , Nivolumab/farmacología , Neoplasias Pulmonares/tratamiento farmacológico , Neoplasias Pulmonares/metabolismo , Metabolómica/métodos , Línea Celular Tumoral , Análisis Multivariante , Redes y Vías Metabólicas/efectos de los fármacos , Metaboloma/efectos de los fármacosRESUMEN
BACKGROUND: Diabetes mellitus is a complex metabolic disorder with systemic implications, necessitating the search for reliable biomarkers and therapeutic strategies. This study investigates the metabolomics profile alterations in diabetic rats, with a focus on the therapeutic effects of Dapagliflozin, a drug known to inhibit renal glucose reabsorption, using Gas Chromatography-Mass Spectrometry analysis. METHODS: A GC-MS based metabolomics approach combined with multivariate and univariate statistical analyses was utilized to study serum samples from a diabetic model of Wistar rats, treated with dapagliflozin. Metabolomics pathways analysis was also performed to identify the altered metabolic pathways associated with the disease and the intervention. RESULTS: Dapagliflozin treatment in diabetic rats resulted in normalized levels of metabolites associated with insulin resistance, notably branched-chain and aromatic amino acids. Improvements in glycine metabolism were observed, suggesting a modulatory role of the drug. Additionally, reduced palmitic acid levels indicated an alleviation of lipotoxic effects. The metabolic changes indicate a restorative effect of dapagliflozin on diabetes-induced metabolic perturbations. CONCLUSIONS: The comprehensive metabolomics analysis demonstrated the potential of GC-MS in revealing significant metabolic pathway alterations due to dapagliflozin treatment in diabetic model rats. The therapy induced normalization of key metabolic disturbances, providing insights that could advance personalized diabetes mellitus management and therapeutic monitoring, highlighting the utility of metabolomics in understanding drug mechanisms and effects.
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Compuestos de Bencidrilo , Diabetes Mellitus Experimental , Glucósidos , Ratas , Animales , Cromatografía de Gases y Espectrometría de Masas/métodos , Diabetes Mellitus Experimental/tratamiento farmacológico , Ratas Wistar , Metabolómica/métodos , Análisis MultivarianteRESUMEN
Simeprevir and daclatasvir represent a cornerstone in the management of Hepatitis C Virus infection, a global health concern that affects millions of people worldwide. In this study, we propose a synergistic approach combining synchronous spectrofluorimetry and chemometric modeling i.e. Partial Least Squares (PLS-1) for the analysis of simeprevir and daclatasvir in different matrices. Moreover, the study employs firefly algorithms to further optimize the chemometric models via selecting the most informative features thus improving the accuracy and robustness of the calibration models. The firefly algorithm was able to reduce the number of selected wavelengths to 47-44% for simeprevir and daclatasvir, respectively offering a fast and sensitive technique for the determination of simeprevir and daclatasvir. Validation results underscore the models' effectiveness, as evidenced by recovery rates close to 100% with relative root mean square error of prediction (RRMSEP) of 2.253 and 2.1381 for simeprevir and daclatasvir, respectively. Moreover, the proposed models have been applied to determine the pharmacokinetics of simeprevir and daclatasvir, providing valuable insights into their distribution and elimination patterns. Overall, the study demonstrates the effectiveness of synchronous spectrofluorimetry coupled with multivariate calibration optimized by firefly algorithms in accurately determining and quantifying simeprevir and daclatasvir in HCV antiviral treatment, offering potential applications in pharmaceutical formulation analysis and pharmacokinetic studies for these drugs.
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Carbamatos , Imidazoles , Pirrolidinas , Simeprevir , Espectrometría de Fluorescencia , Valina , Valina/análogos & derivados , Imidazoles/farmacocinética , Imidazoles/química , Valina/farmacocinética , Simeprevir/farmacocinética , Simeprevir/análisis , Pirrolidinas/química , Carbamatos/farmacocinética , Análisis de los Mínimos Cuadrados , Espectrometría de Fluorescencia/métodos , Algoritmos , Antivirales/farmacocinética , Reproducibilidad de los ResultadosRESUMEN
This study presents the development of an eco-friendly and highly selective mitrogen-doped carbon quantum dot based sensor (N-CQDs) for the detection of gabapentin - a commonly misused drug. A detailed characterization of N-CQDs spectral features and their interaction with gabapentin is provided. The optimal conditions for sensing, including pH value, buffer volume, N-CQDs concentration, and incubation time, were established. The results showed excellent fluorescence quenching at 475 nm (λex = 380 nm) due to the dynamic quenching mechanism, and the sensor demonstrated excellent linearity in the 0.5-8.0 µg mL-1 concentration range with correlation coefficients of more than 0.999, a limit of detection (LOD) of 0.160 and limit of quantification (LOQ) of 0.480 µg mL-1. The accuracy of the proposed sensor was acceptable with a mean accuracy of 99.91 for gabapentin detection. In addition, precision values were within the acceptable range, with RSD% below 2% indicating good repeatability and reproducibility of the sensor. Selectivity was validated using common excipients and pooled plasma samples. The proposed sensor accurately estimated gabapentin concentration in commercial pharmaceutical formulations and spiked plasma samples, exhibiting excellent comparability with previously published methods. The 'greenness' of the sensing system was evaluated using the Analytical GREEnness calculator, revealing low environmental impact and strong alignment with green chemistry principles with a greenness score of 0.76. Thus, the developed N-CQDs-based sensor offers a promising, eco-friendly, and effective tool for gabapentin detection in various situations, ranging from clinical therapeutics to forensic science.
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Celecoxib and tramadol have been combined in a novel FDA-approved medication to address acute pain disorders requiring opioid treatment when other analgesics proved either intolerable or ineffective. The absorbance spectra of celecoxib and tramadol exhibit significant overlap, posing challenges for their individual quantification. This study introduces a spectrophotometric quantification approach for celecoxib and tramadol using a principle component regression assistive model to assist resolving the overlapped spectra and quantifying both drugs in their binary mixture. The model was constructed by establishing calibration and validation sets for the celecoxib and tramadol mixture, employing a five-level, two-factor experimental design, resulting in 25 samples. Spectral data from these mixtures were measured and preprocessed to eliminate noise in the 200-210 nm range and zero absorbance values in the 290-400 nm range. Consequently, the dataset was streamlined to 81 variables. The predicted concentrations were compared with the known concentrations of celecoxib and tramadol, and the errors in the predictions were evidenced calculating root mean square error of cross-validation and root mean square error of prediction. Validation results demonstrate the efficacy of the models in predicting outcomes; recovery rates approaching 100 % are demonstrated with relative root mean square error of prediction (RRMSEP) values of 0.052 and 0.164 for tramadol and celecoxib, respectively. The selectivity was further evaluated by quantifying celecoxib and tramadol in the presence of potentially interfering drugs. The model demonstrated success in quantifying celecoxib and tramadol in laboratory-prepared tablets, producing metrics consistent with those reported in previously established spectrophotometric methods.
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Celecoxib , Análisis de Componente Principal , Espectrofotometría , Tramadol , Celecoxib/análisis , Celecoxib/química , Tramadol/análisis , Espectrofotometría/métodos , Calibración , Reproducibilidad de los Resultados , Formas de Dosificación , Analgésicos Opioides/análisisRESUMEN
Herein, two different sustainable and green signal processing spectrophotometric approaches, namely, derivative spectroscopy and wavelet transform, have been utilized for effective measurement of the antiretroviral therapy abacavir and lamivudine in their pharmaceutical formulations. These methods were used to enhance the spectral data and differentiate between the absorption bands of abacavir and lamivudine in order to accurately measure their concentrations. For determining abacavir and lamivudine, the first derivative spectrophotometric method has been applied to the zero-order and ratio spectra of both drugs. The same approach has been tested using the continuous wavelet transform method where a second order 2.4 of rbio and bior wavelet families were found to be optimum for measuring both drugs. Validation of the proposed methods affirmed their reliability in terms of linearity over the concentration range 1.5-30 µg/mL and 1.5-36 µg/mL for abacavir and lamivudine, respectively, precision (RSD < 2 %), and accuracy with mean recoveries ranging between 98 % and 102 %. Additionally, these spectrophotometric methodologies were applied to real pharmaceutical preparations and yielded results congruent with a prior chromatographic method. Most prominently, the proposed methods stood out for their greenness and sustainability with 97 points as evaluated by the analytical eco-scale method and a score value of 0.79 as analyzed by AGREE method, thereby making them suitable for resource-limited settings and highlighting the potential for broader application of green analytical methods in pharmaceutical analysis.
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Ciclopropanos , Didesoxiadenosina/análogos & derivados , Lamivudine , Análisis de Ondículas , Humanos , Lamivudine/química , Reproducibilidad de los Resultados , Espectrofotometría , Preparaciones FarmacéuticasRESUMEN
Vitamin D is one of the most essential nutrients for brain development, and deficiencies during pregnancy and early childhood development might be associated with autism. Regular monitoring of serum 25-hydroxyvitamin D3 level could help in early diagnosis and therapy. Analytical measurement of serum 25-hydroxyvitamin D3 level using the traditional matrix-matched calibration technique yields inaccurate results due to absence of serum matrix free from 25-hydroxyvitamin D3. The aim of this work was to develop a validated spectrofluorimetric methodology based on the standard addition approach for quantifying 25-hydroxyvitamin D3 levels in real serum samples of autistic children. The spectrofluorimetric methodology utilizes functionalized graphene quantum dots as a fluorescent probe for selective quantification of 25-hydroxyvitamin D3 level, which is based on measuring the quenching properties of 25-hydroxyvitamin D3 on a fluorescent probe. The standard addition approach exhibits a minimal matrix interference since it identically utilizes the same matrix of each study sample for creating its own calibration curve. The method was validated using the guidelines outlined in ICH M10 draft for endogenous compounds quantification. The method was successfully applied for quantifying the serum 25-hydroxyvitamin D3 levels in autistic and healthy children, and autistic children had significantly lower serum 25-hydroxyvitamin D3 levels (with a mean ± SD of 23.80 ± 17.19) when compared to healthy children (with a mean ± SD of 50.13 ± 18.74, P < 0.001). These results suggested an association between vitamin D deficiency and autism.
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Trastorno Autístico , Grafito , Puntos Cuánticos , Niño , Humanos , Preescolar , Vitamina D , Calcifediol , Colorantes Fluorescentes , Espectrometría de Fluorescencia , VitaminasRESUMEN
This study investigates the potential of graphene quantum dots (GQDs) as fluorescent probes for the determination of the antipsychotic drug lumateperone. The spectral characteristics and sensing mechanism of the fluorescent probes were examined, revealing a static quenching mechanism as indicated by the Stern-Volmer analysis. Different factors affecting the quenching process, such as pH, concentration of QDs, and incubation time, were carefully tuned. The developed method was validated according to ICH guidelines, demonstrating excellent linearity in the range of 0.5-2.5 µg/mL, limits of detection and quantification of 0.1226 µg/mL and 0.3714 µg/mL, respectively, and high accuracy, precision, robustness and selectivity. Furthermore, the greenness and blueness of the proposed method were assessed using GAPI, AGREE, and BAGI tools, yielding an AGREE score of 0.78 and a BAGI score of 75 confirming its environmentally benign nature as well as analytical practicality. The method was successfully applied to determine lumateperone in a pharmaceutical formulation, highlighting its potential for routine quality control analysis. This study demonstrates the promising analytical capabilities of GQDs for the sensitive and selective detection of antipsychotic drug lumateperone, offering a simple, rapid, and green alternative to existing analytical techniques.
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Anastrazole (ASZ) is an effective aromatase inhibitor that is used for breast cancer treatment. Nevertheless, ASZ's effectiveness is diminished due to its low water solubility, unregulated release, absence of targeting, and inadequate patient compliance. The goal of the research was to create a hydrogel formulation of ASZ-loaded invasomes (ALI) to enhance the solubility, permeability, targeting, and efficacy of ASZ while also sustaining its release for treatment of breast cancer. The optimized ALI formulation was determined to be 3%w/v phospholipid, 0.15%w/v cholesterol, 3%v/v ethanol, and 1 %v/v cineole based on the results of the pre-formulation study. After conducting in vitro characterization of the optimum formulation, it was combined with carbopol for in vivo examination of its anti-tumor efficacy in a rat model of 7, 12-dimethylbenzanthracene. Compared to free ASZ, ALI hydrogel increased its penetration by 10.67 times and prolonged its release by 64.02%. Compared to the control positive group, ALI hydrogel reduced tumor volume by 99.19% and mortality by 10.93%. The anti-tumor effect of the ALI hydrogel was demonstrated by its ability to accumulate more ASZ in tumors and reduce hypercellular tumors. Overall, transdermal ALI hydrogel shows potential as a promising approach for treating breast cancer.
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Anastrozol , Neoplasias de la Mama , Hidrogeles , Animales , Femenino , Hidrogeles/química , Neoplasias de la Mama/tratamiento farmacológico , Neoplasias de la Mama/patología , Anastrozol/administración & dosificación , Humanos , Ratas , 9,10-Dimetil-1,2-benzantraceno , Solubilidad , Liberación de Fármacos , Nitrilos/química , Línea Celular Tumoral , Triazoles/química , Triazoles/administración & dosificación , Triazoles/farmacocinética , Triazoles/farmacología , Células MCF-7 , Inhibidores de la Aromatasa/administración & dosificación , Inhibidores de la Aromatasa/química , Inhibidores de la Aromatasa/farmacología , Inhibidores de la Aromatasa/farmacocinética , Sistemas de Liberación de Medicamentos/métodosRESUMEN
Futibatinib is a powerful inhibitor of fibroblast growth factor receptors that impedes its phosphorylation and subsequently leading to a reduction in in cell viability across various cell lines. Futibatinib was approved for initial use as an effective treatment for several diseases, including non-small cell lung cancer and breast cancer. Herein, a novel selective fluorescence probe was created for futibatinib quantification in various matrices, including pharmaceutical formulation and human plasma. The technique primarily depends on futibatinib's chemical conversion into a fluorescent product through a reaction with trimethylamine and bromoacetyl bromide. The created fluorescent probe exhibits maximum emission peak at 338 nm upon excitation at 248 nm. The method provided a low detection limit of 0.120 ng/mL and maintained a linear concentration-dependent relationship across the range of 1-200 ng/mL. High sensitivity, accuracy and precision were demonstrated for futibatinib quantification in pharmaceutical formulation and spiked plasma matrix by the method, which was validated in accordance with ICH requirements.