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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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Nucleotídeos de Adenina , Amidas , Antivirais , Pirazinas , Termodinâmica , Pirazinas/química , Pirazinas/metabolismo , Amidas/química , Amidas/metabolismo , Nucleotídeos de Adenina/química , Nucleotídeos de Adenina/metabolismo , Antivirais/química , Antivirais/farmacologia , Antivirais/metabolismo , Espectroscopia de Infravermelho com Transformada de Fourier , Espectrometria de Fluorescência , Transferência Ressonante de Energia de Fluorescência , Espectrofotometria Ultravioleta , Sítios de Ligação , Adenina/química , Adenina/metabolismoRESUMO
The combination of Curcumin (CRN), resveratrol (RSV), and quercetin (QRN) has significant antioxidant effects and is found to be more effective than a single polyphenol. Spectrophotometric methods are considered one of the most common analytical techniques for the determination of the drugs due to their sensitivity, rapidness, low cost, and reproducibility. Therefore, the presence of new, and simple methods for the determination of such compounds will be highly valuable, specially in the presence of spectral overlap. In this research, five different facile spectrophotometric methods were investigated for the simultaneous determination of that ternary mixture for the first time, including zero order (I), first derivative (II), ratio difference double divisor (III), first derivative ratio spectra (IV), and mean centering (V) methods. The designed approaches were linear over the concentration ranges of (1.0-10.0), (0.5-8.0), and (1.0-14.0) µg/mL, respectively for curcumin, resveratrol, and quercetin. The different methods were then validated as stated by the International Council of Harmonization. The accuracy and precision have been evaluated by statistical analysis including student t-test, variance ratio F-test, and ANOVA. Moreover, the greenness and whiteness of the proposed methods were assessed to ensure the adherence to the greenness characters.
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Antioxidantes , Curcumina , Polifenóis , Quercetina , Resveratrol , Espectrofotometria , Antioxidantes/análise , Espectrofotometria/métodos , Polifenóis/análise , Resveratrol/análise , Quercetina/análise , Curcumina/análise , Química Verde/métodos , Reprodutibilidade dos Testes , Estilbenos/análise , Estilbenos/químicaRESUMO
The current study presents the first spectrofluorimetric approach for the estimation of lactoferrin, depending on the measurement of its native fluorescence at 337 nm after excitation at 230 nm, without the need for any hazardous chemicals or reagents. It was found that the fluorescence intensity versus concentration calibration plot was linear over the concentration range of 0.1-10.0 µg/mL with quantitation and detection limits of 0.082 and 0.027 µg/mL, respectively. The method was accordingly validated according to the ICH recommendations. The developed method was applied for the estimation of lactoferrin in different dosage forms, including capsules and sachets with high percent recoveries (97.84-102.53) and low %RSD values (<1.95). Lactoferrin is one of the key nutrients in milk powder and a significant nutritional fortifier. In order to assess the quality of milk powder, it is essential to rapidly and accurately quantify the lactoferrin content of the product. Therefore, the presented study was successfully applied for the selective estimation of lactoferrin in milk powder with acceptable percent recoveries (96.45-104.92) and %RSD values (≤3.607). Finally, the green profile of the method was estimated using two assessment tools: Green Analytical Procedure Index (GAPI) and Analytical GREEnness (AGREE), which demonstrated its excellent greenness.
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Química Verde , Fórmulas Infantis , Lactoferrina , Preparações Farmacêuticas , Animais , Humanos , Lactente , Fórmulas Infantis/química , Fórmulas Infantis/análise , Lactoferrina/análise , Limite de Detecção , Leite/química , Preparações Farmacêuticas/análise , Preparações Farmacêuticas/química , Espectrometria de Fluorescência/métodosRESUMO
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 , Limite de Detecção , Espectrometria de Fluorescência/métodosRESUMO
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 , Espectrometria de Fluorescência/métodos , Composição de Medicamentos , MorfolinasRESUMO
Quantitative 1H-NMR became an increasingly important issue in pharmaceutical analytical chemistry. This study used NMR spectroscopy to assay the bronchodilator drug terbutaline sulfate and its pro-drug bambuterol hydrochloride in pure form and pharmaceutical preparations. The technique proceeded using deuterium oxide (D2O) as an 1H-NMR solvent and phloroglucinol anhydrous as an internal standard (IS). Comparatively, to the phloroglucinol signal at 5.9 ppm, the resulting quantitative signals of the studied drugs were corrected. The terbutaline singlet signal at 6.3 ppm was chosen for quantification, while the bambuterol quantitative singlet signal was at 2.9 ppm. The two drugs were rectilinear over the concentration range of 1.0-16.0 mg/mL. LOD values were 0.19 and 0.21 mg/mL while LOQ values were 0.58 and 0.64 mg/mL for terbutaline and bambuterol respectively. The developed method has been validated according to the International Conference of Harmonization (ICH) regarding linearity, accuracy, precision, specificity, and robustness. A greenness profile assessment was applied, and the method proved to be green. The method enables the assay of the two drugs in pure drug and pharmaceutical preparations. The method also enables the assay of the two drugs in the presence of each other; thus, it is considered a stability-indicating method where terbutaline is an acid degradation product of bambuterol.
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Moxifloxacin and ofloxacin are two broad-spectrum quinolone antibiotics. They are among the most widely used antibiotics, at this time, applied to control the COVID-19 pandemic. Hydroxychloroquine is an FDA-approved drug for the treatment of COVID-19. This work describes a simple, green, selective, and sensitive spectrofluorimetric method for the assay of moxifloxacin and ofloxacin in the presence of hydroxychloroquine, two co-administered mixtures used in the treatment of hospital-acquired pneumonia in patients with COVID-19. Simultaneous assay of hydroxychloroquine and moxifloxacin was carried out in methanol using a direct spectrofluorimetric method (method I) at 375 and 550 nm, respectively, after excitation at 300 nm. The direct spectrofluorimetric assay was rectilinear over concentration ranges 50.0-400.0 and 300.0-2500.0 ng/ml for hydroxychloroquine and moxifloxacin, respectively, with limits of detection (LOD) of 6.4 and 33.64 ng/ml and limits of quantitation (LOQ) of 19.4 and 102.6 ng/ml, respectively, for the two drugs. The assay for hydroxychloroquine and ofloxacin was carried out by measuring the first derivative synchronous amplitude for hydroxychloroquine at the zero crossing point of ofloxacin and vice versa at Δλ = 140 nm (method II). Hydroxychloroquine was measured at 266 nm, while ofloxacin was measured at 340 nm over the concentration range 4-40 ng/ml for hydroxychloroquine and 200-2000 ng/ml for ofloxacin with LOD of 0.467 and 25.3 ng/ml and LOQ of 1.42 and 76.6 ng/ml, respectively, for the two drugs. The two methods were validated following International Conference on Harmonization guidelines and were applied to the analysis of the two drugs in plasma with good percentage recoveries (109.73-93.17%).
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COVID-19 , Ofloxacino , Humanos , Ofloxacino/análise , Moxifloxacina , Hidroxicloroquina/uso terapêutico , Espectrometria de Fluorescência/métodos , Pandemias , Tratamento Farmacológico da COVID-19 , Antibacterianos/uso terapêutico , Antibacterianos/análise , HospitaisRESUMO
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.
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Recently, the kinase receptor inhibitor drug larotrectinib has been approved as a monotherapy for the treatment of patients with solid tumors containing the neurotrophic receptor tyrosine kinase gene fusion. In this paper, a novel sensitive spectrofluorimetric method was proposed for the determination of larotrectinib based on nitrogen-doped carbon quantum dots (N-CQDs) fluorescent probes. The proposed method is the first spectroscopic method for analysis of the cited drug, which is simple to implement and involves no pre-treatment steps or complicated techniques. The N-CQDs synthesis was performed by adopting a straightforward, fast, and environmentally friendly approach. It was achieved by means of a standard domestic microwave with inexpensive and readily available starting materials: orange juice (carbon source) and urea (nitrogen source). The synthesized N-CQDs were subjected to microscopic and spectroscopic characterization procedures. They were found to be stable with a sufficiently high fluorescence quantum yield (25.3%) and a small particle size distribution (2-5 nm). The motivation for the use of N-CQDs in this study arose from their excellent fluorescence intensities at 417 nm when excited at 325 nm. Larotrectinib was found to have a quantitative and selective quenching effect on the QDs fluorescence allowing for its sensitive determination. The drug's quenching mechanism was investigated and found to be of the static type. Under optimal conditions, the proposed approach permitted the determination of larotrectinib over the concentration interval of 5.0-28.0 µg/mL. The method showed sufficient sensitivity with a detection limit of 0.19 µg/mL and a quantitation limit of 0.57 µg/mL, enabling the determination of LARO in spiked human plasma samples. The approach's recovery percentage was found to be in the range of 99.09-100.73% for pure samples and 97.35-102.59% for plasma samples. The study also successfully applied the proposed approach to the commercial oral solution form of larotrectinib (Vitrakvi®) with high selectivity. Method greenness was further evaluated by adopting two metric tools, including the complementary green analytical procedure index (ComplexGAPI) and Analytical GREENNESS metric approach (AGREE), and it was confirmed to be excellent green. The proposed method was validated in accordance with the ICHQ2 (R1) recommendations and is considered an excellent candidate for potential application in the therapeutic monitoring of larotrectinib.
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Carbono , Pontos Quânticos , Humanos , Carbono/química , Pontos Quânticos/química , Espectrometria de Fluorescência/métodos , Nitrogênio/químicaRESUMO
For the simultaneous estimation of two co-formulated antihistaminic drugs (Bilastine and Montelukast), a novel and eco-friendly reversed-phase HPLC approach with both diode array and fluorescence detection modes was designed. Rather than using the routine methodology, the Quality by Design (QbD) approach was adopted to speed up the method development and to test robustness of the method. To evaluate the effect of variable factors on chromatographic response, a full factorial design was used. The chromatographic separation was performed using isocratic elution on the C18 column. The mobile phase consists of 92% methanol, 6% acetonitrile, and 2% phosphate buffer with 0.1 (v/v) triethylamine adjusted to pH 3, it was pumped at a flow rate of 0.8 mL/min with an injection volume of 20 µL. The developed stability indicating HPLC approach was used to assess the stability of montelukast (MNT). It was subjected to a variety of stress conditions, including hydrolytic (acid-base), oxidative, thermal, and photolytic stress conditions. All of these conditions were found to have relevant degradation pathways. Under the described experimental conditions, MNT degradation followed pseudo-first-order kinetics. The kinetic parameters of its degradation (rate constant and t1/2) were calculated and a proposal for the degradation pathway was postulated.
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In this work, the binding mechanism between donepezil (DNP) and bovine serum albumin (BSA) was established using several techniques, including fluorimetry, UV- spectrophotometry, synchronous fluorimetry (SF), fourier transform infrared (FTIR), fluorescence resonance energy transfer (FRET) besides molecular docking study. The fluorescence quenching mechanism of DNP-BSA binding was a combined dynamic and static quenching. The thermodynamic parameters, binding forces, binding constant, and the number of binding sites were determined using a different range of temperature settings. Van't Hoff's equation was used to calculate the reaction parameters, including enthalpy change (ΔHο) and entropy change (ΔSο). The results pointed out that the DNP-BSA binding was endothermic. It was shown that the stability of the drug-protein system was predominantly due to the intermolecular hydrophobic forces. Additionally, the site probing method revealed that subdomain IIA (Site I) is where DNP and BSA's binding occurs. This was validated using a molecular docking study with the most stable DNP configuration. This study might help to understand DNP's pharmacokinetics profile and toxicity as well as provides crucial information for its safe use and avoiding its toxicity.
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One of the most promising drugs recently approved for the treatment of various types of cancer is dacomitinib, which belongs to the tyrosine kinase inhibitor class. The US Food and Drugs Administration (FDA) has recently approved dacomitinib as a first-line treatment for patients suffering from non-small cell lung cancer (NSCLC) with epidermal growth factor receptor (EGFR) mutations. The current study proposes the design of a novel spectrofluorimetric method for determining dacomitinib based on newly synthesized nitrogen-doped carbon quantum dots (N-CQDs) as fluorescent probes. The proposed method is simple and does not require pretreatment or preliminary procedures. Since the studied drug does not have any fluorescent properties, the importance of the current study is magnified. When excited at 325 nm, N-CQDs exhibited native fluorescence at 417 nm, which was quantitatively and selectively quenched by the increasing concentrations of dacomitinib. The developed method involved the simple and green microwave-assisted synthesis of N-CQDs, using orange juice as a carbon source and urea as a nitrogen source. The characterization of the prepared quantum dots was performed using different spectroscopic and microscopic techniques. The synthesized dots had consistently spherical shapes and a narrow size distribution and demonstrated optimal characteristics, including a high stability and a high fluorescence quantum yield (25.3%). When assessing the effectiveness of the proposed method, several optimization factors were considered. The experiments demonstrated highly linear quenching behavior across the concentration range of 1.0-20.0 µg/mL with a correlation coefficient (r) of 0.999. The recovery percentages were found to be in the range of 98.50-100.83% and the corresponding relative standard deviation (%RSD) was 0.984. The proposed method was shown to be highly sensitive with a limit of detection (LOD) as low as 0.11 µg/mL. The type of mechanism by which quenching took place was also investigated by different means and was found to be static with a complementary inner filter effect. For quality purposes, the assessment of the validation criteria adhered to the ICHQ2(R1) recommendations. Finally, the proposed method was applied to a pharmaceutical dosage form of the drug (Vizimpro® Tablets) and the obtained results were satisfactory. Considering the eco-friendly aspect of the suggested methodology, using natural materials to synthesize N-CQDs and water as a diluting solvent added to its greenness profile.
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Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Pontos Quânticos , Humanos , Pontos Quânticos/química , Espectrometria de Fluorescência/métodos , Corantes Fluorescentes/química , Carbono/química , Nitrogênio/químicaRESUMO
The current study introduces a spectrofluorimetric methodology for the assessment of palbociclib without the need for any pre-derivatization steps for the first time. This approach relied on the palbociclib quenching effect on the native fluorescence of newly synthesized nitrogen-doped carbon quantum dots (N-CQDs). An innovative, facile, and rapid microwave-assisted pyrolysis procedure was applied for the synthesis of N-CQDs using available and economic starting materials (the carbon source is orange juice and the nitrogen source is urea) in less than 10 minutes. Full characterization of the prepared QDs was carried out using various techniques. The prepared N-CQDs exhibited good fluorescence emission at 417 nm after excitation at 325 nm with stable fluorescence intensity and good quantum yield (29.3%). They showed spherical shapes and narrow size distribution with a particle size of around 2-5 nm. Different experimental variables influencing fluorescence quenching were examined and optimized. A good linear correlation was exhibited alongside the range of 1.0 to 20.0 µg mL-1 with a correlation coefficient of 0.9997 and a detection limit of 0.021 µg mL-1. The proposed methodology showed good selectivity allowing its efficient application in tablets with high percentage recoveries and low percentage RSD values. The mechanism of quenching was proved to be static by applying the Stern-Volmer equation at four different temperatures. The method was validated in accordance with ICHQ2 (R1) recommendations. Intriguingly, N-CQDs demonstrated good biocompatibility and low cytotoxicity, which permitted cellular imaging and palbociclib detection in living cancer cells. Therefore, the proposed method may have potential applications in cancer therapy and related mechanism research.
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Novel, selective, facile, and precise spectroscopic approaches were validated to determine nilotinib hydrochloride, a tyrosine kinase inhibitor used to treat patients with chronic myeloid leukemia. These approaches depend on the reaction of the tertiary amine group of nilotinib with erythrosine B in the Britton-Robinson buffer at pH 4. Method I, depends on measuring the absorbance of the formed complex at 551 nm. The absorbance concentration plot showed linearity over the concentration range of 1.0 to 9.0 µg/ml. Method II, involved the measurement of the quenching of the native fluorescence of erythrosine B by adding nilotinib in an acidic medium. The fluorescence quenching of erythrosine B was measured at 549 nm after excitation at 528 nm. This approach showed excellent linearity in the concentration range of 0.04 to 0.7 µg/ml. The limit of detection values for Method I and Method II were 0.225 and 0.008 µg/ml, respectively, while the limit of quantitation values for Method I and Method II were 0.68 and 0.026 µg/ml, respectively. To get the optimal conditions, factors that may affect the formation of the ion-pairing complex were thoroughly examined. The two approaches were carefully validated following the International Conference of Harmonization (ICH Q2R1) guidelines. Statistical assessment of the results achieved using the suggested and previously published comparison approaches showed no significant difference. The approaches were successful in determining nilotinib in a pharmaceutical dosage form as well as spiked human plasma samples. The eco-friendly properties of the methods were evaluated by three different tools.
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Eritrosina , Humanos , Pós , Espectrometria de Fluorescência/métodos , Eritrosina/química , CápsulasRESUMO
Fluorescence spectroscopy is gaining interest in the analysis and quantitative determination of different drugs. This study was carried out to investigate the fluorometric properties of the short-acting muscle relaxant mivacurium in its pure form, injection, and human plasma. It is nondepolarizing skeletal muscle relaxant for intravenous (IV) administration. Mivacurium shows a strong native fluorescence in methanol at 317 nm after excitation at 230 nm (Method I). The critical parameters that may influence the fluorescence of this drug were carefully studied. A linear response between concentration and fluorescence was constructed over the concentration range: 20.0 to 400.0 ng/mL with determination coefficient (r2) equal to 0.9998. Additionally, the correlation coefficient of the linear relationship (r) was found to be 0.9999 with a slope = 2.196 and intercept = -16.61. Limits of quantitation and detection were calculated mathematically to be 17.45 and 5.75 ng/mL respectively. Further estimation of mivacurium in spiked human plasma was performed by construction of specific calibration curve and the obtained correlation coefficient was 0.9948. Moreover, the ability to determine mivacurium in the presence of commonly co-administered drugs were investigated including propofol and thiopental. Method II includes the determination of MVC in the presence of propofol utilizing the first derivative synchronous fluorescence spectroscopy. The results of method II indicated acceptable percentage recoveries from 98.88 to 100.75 %. Statistical evaluation of the results revealed satisfactory accuracy and precision.
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Fármacos Neuromusculares não Despolarizantes , Propofol , Humanos , Mivacúrio , Espectrometria de Fluorescência , Isoquinolinas/química , Fármacos Neuromusculares não Despolarizantes/química , Preparações FarmacêuticasRESUMO
Based on their reaction with highly fluorescent carbon quantum dots (CQDts), a precise and reliable spectrofluorometric approach was developed for the determination of three calcium channel blockers. The studied drugs are: lercanidipine, nimodipine and nifedipine. (CQDts) were produced using a one-step hydrothermal method with ascorbic acid as the carbon source. The produced CQDts were capped by alcohol to create yellow emitters displaying a high fluorescence emission at 524 nm when excited at 325 nm. The fluorescence intensity of CQDts was noticeably quenched by each of the three calcium channel blockers. The relation between their concentrations and fluorescence quenching is linear over the concentration range of 0.5-20 µg/mL for each of the three drugs. A full factorial design was used to optimize the effect of variable factors. Therefore, under optimum experimental design conditions, the detection limits for lercanidipine, nimodipine, and nifedipine were 0.11 ± 1.09, 0.10 ± 0.25 and 0.12 ± 0.71 µg/mL, respectively. The LOQ was 0.33, 0.30, and 0.37 µg/mL respectively. The quenching of fluorescent CQDts occurred through the inner filter effect (IFE) for nimodipine, while it was mixed with dynamic quenching for lercanidipine and nifedipine. The proposed method was effectively used to determine the cited drugs in their pharmaceutical products and had an acceptable level of precision. The selectivity of the CQDts system towards the studied drugs was examined indicating no interference from interfering species.
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Corantes Fluorescentes , Pontos Quânticos , Bloqueadores dos Canais de Cálcio , Nimodipina , Nifedipino , Espectrometria de Fluorescência , CarbonoRESUMO
Ricinine is an important biomarker used for detecting the exposure to castor bean products. The current study describes a highly sensitive and selective spectrofluorimetric approach to determine ricinine in various edible oils. It depends on measuring the native fluorescence of ricinine at 365 nm following excitation at 307 nm over a concentration range of 50.0-1200.0 ng/mL. The method displayed high sensitivity with quantitation and detection limits down to 19.56 and 6.46 ng/mL, respectively. The significant factors affecting the fluorescence of ricinine were optimized using 22 full factorial design. The proposed approach was successfully employed for ricinine determination in three types of edible oils with high percent recoveries and low S.D. values. The most important advantage of the developed method is the reduction of sample preparation steps, analysis time, and cost. Hence, it can be better suited for routine analysis and quality control of cooking oils adulterated with castor oil.
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Alcaloides , Espectrometria de Fluorescência , Alcaloides/análise , Piridonas , Óleos de PlantasRESUMO
In the present study, a drug-like molecular hybrid structure between chalcone and sulfonamide moieties was synthesized and characterized. The structural peculiarities of the synthesized hybrid were further verified by means of single crystal X-ray crystallography. Furthermore, its biological activity as an anticancer agent was evaluated. The synthesized model of chalcone-sulfonamide hybrid 3 was found to have potent anticancer properties against the studied cancer cell lines. Hence, the in vitro binding interaction of hybrid 3 with Calf thymus DNA (CT-DNA) was studied at a simulated physiological pH to confirm its anticancer activity for the first time. This was investigated by applying different spectroscopic techniques, ionic strength measurements, viscosity measurements, thermodynamics, molecular dynamic simulation and molecular docking studies. The obtained results showed a clear binding interaction between hybrid 3 and CT-DNA with a moderate affinity via a minor groove binding mechanism. The binding constant (Kb) at 298 K calculated from the Benesi-Hildebrand equation was found to be 3.49 × 104 M-1. The entropy and enthalpy changes (ΔS0 and ΔH0) were 204.65 J mol-1 K-1 and 35.08 KJ mol-1, respectively, indicating that hydrophobic interactions constituted the major binding forces. The results obtained from molecular docking and dynamic simulation studies confirmed the minor groove binding interaction and the stability of the formed complex. This study can contribute to further understanding of the molecular mechanism of hybrid 3 as a potential antitumor agent and can also guide future clinical and pharmacological studies for rational drug design with enhanced or more selective activity and greater efficacy.[Figure: see text]Communicated by Ramaswamy H. Sarma.
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Calycosin, the major bioactive isoflavonoid inAstragali Radix and an important anti-viral drug with a variety of pharmacological actions, is being determined by five different spectroscopic methods. Two spectrophotometric methods have been investigated including measuring the absorption spectra at λmax = 270 nm and the first derivative spectra at λ = 288 nm for methods I and II, respectively. For the first time; the native fluorescence of calycosin is measured without adding any reagents. The fluorescence intensity was measured at 340 nm after excitation at 282 nm in method III. The fourth method involves the direct measuring of a first derivative spectrofluorimetric emission peak at 292 nm. In method V synchronous fluorescence spectra were recorded in methanol at Δλ = 70 nm. The linear range for the fluorescence-based methods was 0.05-1.0 µg/mL and for the UV-based methods was 0.5-10.0 µg/mL. The methods were validated per International Council of Harmonization (ICHQ2R1) guidelines. The limits of detection were found to be down to 0.11 and 0.12 µg/mL for the spectrophotometric methods, and 15.0, 18.0,16.0 ng/ mL, for the spectrofluorimetric approaches respectively, representing the high sensitivity. Accordingly, this permitted the quantitation of calycosin in spiked human plasma samples with satisfactory percentage recoveries (94.50.-102.50 %). The methods were utilized for calycosin analysis in different matrices including plasma and capsules with high precision and accuracy.