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Assessing medication adherence through the determination of antihypertensive drugs in biological matrices holds significant importance. Amlodipine (AP), a potent antihypertensive medication extensively prescribed for hypertensive patients, is particularly noteworthy in this context. This article aims to introduce a rapid, simple, improved sensitivity, and reproducibility in detecting AP in its pure form, tablet formulation, and spiked human plasma than the other reported methods. The proposed method utilizes a fluorescence approach, relying on the inhibition of the intramolecular photoinduced electron transfer (PET) effect of the lone pair of the N-atom in the primary amino moiety of AP. This inhibition is achieved by acidifying the surrounding medium using 0.2 M acetic acid. By blocking PET, the target AP drug is sensitively detected, at [Formula: see text] 423 nm over a concentration range 25-500 ng mL- 1 showcasing an exceptionally low quantitation limit of 1.41 ng mL- 1. Notably, this innovative technique was successfully applied to detect AP in its solid dosage form and spiked human plasma. Remarkably, matrix interference was found to be insignificant, underscoring the robustness and applicability of the established approach. The combination of speed, sensitivity, and reproducibility makes this method particularly suitable for assessing medication adherence in patients prescribed AP for hypertension.
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Olopatadine (OLP) is widely utilized as an effective antihistaminic drug for alleviating ocular itching associated with allergic conjunctivitis. With its frequent usage in pharmacies, there arises a pressing need for a cost-effective, easily implementable, environmentally sustainable detection method with high sensitivity. This study presents a novel signal-on fluorimetric method for detecting OLP in both its pure form and aqueous humor. The proposed approach depends on enhancing the weak intrinsic fluorescence emission of OLP, achieving a remarkable increase of up to 680% compared to its intrinsic fluorescence. This enhancement is achieved by forming micelles around protonated OLP using an acetate buffer (pH 3.6) and incorporating a solution of sodium dodecyl sulfate (SDS) surfactant. A strong correlation (R = 0.9996) is observed between the concentration of OLP and fluorescence intensities ranging from 1.0 to 100.0 ng mL-1 with a limit of detection of 0.22 ng mL-1. This described method is successfully employed for quantifying OLP in both its powder form and pharmaceutical eye drops. Furthermore, it demonstrates robust performance in determining OLP in artificial aqueous humor with a percentage recovery of 99.05 ± 1.51, with minimal interference from matrix interferents. Moreover, the greenness of the described method was evaluated.
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Humor Acuoso , Fluorometría , Clorhidrato de Olopatadina , Clorhidrato de Olopatadina/análisis , Humor Acuoso/química , Tecnología Química Verde , Espectrometría de Fluorescencia , Límite de DetecciónRESUMEN
9-Mesityl-10-methylacridinium ion (Acr+-Mes) is a donor-acceptor molecule with a much longer lifetime and a higher energy electron transfer excited state than natural photosynthetic reaction centers. Unlike lucigenin with a coplanar geometry, Acr+-Mes has an orthogonal geometry. There is no π conjugation between Acr+ and Mes. Due to its special electron donor-acceptor structure, it does not rely on strong alkalinity to generate an electron transfer state like lucigenin, which makes it possible to achieve chemiluminescence (CL) under weakly alkaline or neutral conditions. In this study, we report Acr+-Mes CL for the first time. Acr+-Mes generates about 400 times stronger CL intensity than lucigenin under neutral conditions (pH = 7) using KHSO5 as the coreactant. Moreover, Co2+ can enhance Acr+-Mes/KHSO5 CL remarkably. Acr+-Mes/KHSO5 CL enables Co2+ detection with a linear range of 0.5-500 nM and a limit of detection of 28 pM (S/N = 3). This method was tested for the detection of Co2+ in lake water, and the standard recovery rate of 96.8-107% was achieved. This study provides a new way to develop efficient CL systems in neutral solutions.
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The ability to estimate and quantify biothiols in biological fluids is very significant for attaining a detailed understanding of biothiols-related pathological diseases. Most of the developed methods for biothiols detection are not suitable for this purpose owing to their low sensitivity, poor selectivity, and long experimental procedures. In this study, a novel and simple structure electrochemical probe has been synthesized for the first time for the selective determination of biothiols. The developed probe is based on using 2,4-dinitrobenzenesulfonyl moiety (DNBS) as a selective recognition moiety for biothiols. The electrochemical probe was successfully fabricated through a facile one-step reaction between 2,4-dinitrobenzenesulfonyl chloride (DNBS-Cl) and p-aminophenol. The successful synthesis of the probe was confirmed by using different characterization techniques such as an NMR spectroscopy, Fourier-transform infrared (FT-IR) spectroscopy, and mass spectrometry. Biothiols can selectively cleave the DNBS moiety through an aromatic nucleophilic substitution (ANS) reaction within 10 min to release p-aminophenol, which is a highly electrochemical active molecule that can be selectively detected easily by cyclic voltammetry at low potential. The probe has been employed for the quantification of cysteine, glutathione, and homocysteine with a LOD of 1.50, 3.48, and 4.67 µM, respectively. Excellent recoveries have been achieved in the range of 95.44-98.71% for the determination of the total biothiols in the human plasma sample.
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Cisteína , Colorantes Fluorescentes , Cisteína/química , Colorantes Fluorescentes/química , Glutatión/análisis , Homocisteína , Humanos , Espectrometría de Fluorescencia , Espectroscopía Infrarroja por Transformada de Fourier , Compuestos de Sulfhidrilo/análisisRESUMEN
A new fluorimetric procedure is described for analysis of milnacipran in its bulk, tablet dosage forms, as well as in biological human samples such as plasma and urine. The suggested method relies on the construction of a derivative with strong fluorescence called dihydropyridine derivative. This derivative resulted from the interaction of the primary amino group in the studied drug and acetylacetone/formaldehyde in McIlvaine buffer (pH 5). The fluorescent dihydropyridine derivative was measured at 470 nm. Influences of experimental variables namely pH, reagent concentration and temperature were examined and optimized. The calibration curve showed linearity over the range of 0.15-1.25 µg ml-1 of milnacipran with an R2 value of 0.9998. The detection limit was 0.02 µg ml-1 and the determination limit was 0.07 µg ml-1 . The developed procedure was successfully used in the assay of the studied drug in Avermilan® tablets with excellent selectivity. In addition, the reaction was applied to estimate the drug in spiked human plasma and urine with mean percentage recoveries of 100.04 ± 1.61 and 99.78 ± 0.81% for urine and plasma, respectively.
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Fibromialgia , Fibromialgia/tratamiento farmacológico , Formaldehído , Humanos , Milnaciprán , Espectrometría de Fluorescencia , ComprimidosRESUMEN
Herein, we report luminol-silicotungstic acid (STA) chemiluminescence (CL) for the first time. The luminol-STA system resulted in remarkable CL enhancement (65 times) compared with the known classical luminol-H2O2 system because of the generation of the strong oxidizing agent tungsten trioxide from STA. Based on the quenching effect of uric acid, the new CL system is applied for the sensitive and selective assay of uric acid in its pure state (LOD 0.75 nM) and in real human urine with excellent recoveries in the range of 99.6-102.3%. Furthermore, this system permits the efficient detection of STA (LOD, 0.24 µM).
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Mediciones Luminiscentes/métodos , Luminol/química , Silicatos/química , Compuestos de Tungsteno/química , Ácido Úrico/orina , Humanos , Peróxido de Hidrógeno/química , Concentración de Iones de Hidrógeno , Límite de Detección , Oxidación-Reducción , Óxidos/química , Tungsteno/químicaRESUMEN
One of the most commonly used drugs in treatment of schizophrenia is flupentixol dihydrochloride, therefore it is important to develop a simple, low cost and sensitive spectrofluorimetric method for the estimation of flupentixol dihydrochloride. The yellow fluorescent product that is generated from the nucleophilic substitution reaction of the free lone pair of the alcoholic hydroxyl group of the drug and 4-chloro-7-nitrobenzofurazan (NBD-Cl) in Mcllvaine buffer pH 7.0 was estimated at 510 nm (λex 460 nm). The variables that affect the development of the reaction product were explored and optimized. The linear range of this method was 0.5-2.5 µg ml-1 with a limit of quantitation equal to 0.29 µg ml-1 . Our method was successfully applied for the assurance of flupentixol in tablet form with average percentage recovery of 99.08 ± 1.01% without obstruction from the basic excipients exhibits. Furthermore, our strategy was extended to study the content uniformity testing of flupentixol in Fluaxnol® tablets.
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Benzoxazoles/química , Colorantes Fluorescentes/química , Flupentixol/análisis , Ácido Clorhídrico/análisis , Estructura Molecular , Espectrometría de FluorescenciaRESUMEN
A simple and sensitive spectrofluorimetric method has been developed and validated for determination of oseltamivir phosphate (OSP). The proposed method is based on condensation reaction of the primary amino group of OSP with ninhydrin and phenylacetaldehyde in buffered medium (pH 6.5). The formed yellow fluorescent product exhibits excitation and emission maxima at 390 and 460 nm, respectively. The selectivity improvement of our proposed method is based on the water insolubility of the oseltamivir carboxylic acid (OSC) the active metabolite of OSP, which contains the same primary amino group as OSP but cannot, condensed with ninhydrin and phenylacetaldehyde reagents. The different experimental parameters affecting the formation and stability of the reaction product were carefully studied and optimized. The fluorescence intensity concentration plot is rectilinear in the range of 2-15 µg ml-1 with detection and quantitation limits of 0.32 and 0.98 µg ml-1, respectively. The proposed method was successfully applied for determination of OSP in commercial capsules, suspension and spiked human plasma with good percentage recovery. In addition, the developed procedure was extended to study the stability of OSP under different stress conditions; including acid and alkali hydrolysis, oxidation, photolysis, and thermal degradation. Furthermore, the kinetic of alkaline and acidic degradation of the cited drug were investigated. The apparent first order degradation rate constants were 0.258 and 0.318 K h-1 with half times of 2.68 and 2.17 h, for acidic and alkaline degradation, respectively.
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Antivirales/sangre , Cápsulas/análisis , Oseltamivir/sangre , Fosfatos/sangre , Espectrometría de Fluorescencia/métodos , Fluorescencia , Humanos , Oxidación-ReducciónRESUMEN
The ability to determine antihistaminic drugs in biological matrices is critical for the medication adherence assessment. Among these antihistaminic medications, cyproheptadine (CPD); that is acting as a potent first-generation antihistaminic drug that has been extensively prescribed for allergic patients. Most of the established approaches for CPD detection are not appropriate for this purpose owing to their weak sensitivity, lack of rapidity, and complicated experimental procedures. Herein, we present a very fast, highly sensitive, and reproducible approach for the detection of CPD in its pure form, tablet formulation, and spiked human plasma. The photoluminescence approach depends on hindering the intramolecular photoinduced electron transfer (PET) effect of the lone pair of the N-atom present on the piperidine ring of CPD by making the surrounding medium acidic using 1.0 M acetic acid. Based on blocking PET, the target CPD drug has been sensitively detected from 5.0 to 500 ng mL-1 with a very low detection and quantitation limit of 7.01 and 21.25 ng mL-1, respectively. Moreover, the established approach was used for checking the tablet content uniformity testing for each tablet and spiked human plasma, and noteworthy, the matrices interference was insignificant.
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Ciproheptadina , Electrones , Humanos , Espectrometría de Fluorescencia/métodos , ComprimidosRESUMEN
A green, rapid and sensitive fluorimetric method to quantify levodropropizine (LVP) in human plasma was exploited for the first time. The proposed method adopts LVP's intrinsic fluorescence in distilled water at a detecting emission of 345 nm following excitation at 240 nm. LVP displayed linearity across concentrations ranging from 50 to 1000 ng mL-1, with a detection limit of 0.77 ng mL-1 and a quantification limit of 2.33 ng mL-1. Thorough validation confirmed its reliability, successfully determining LVP in tablets with an average recovery of 98.64 ± 1.07 %. Furthermore, the method's applicability extended to estimate the studied drug in spiked human plasma with excellent obtained percentage recoveries (98.68 ± 1.28-100.14 ± 1.23).
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Plasma , Glicoles de Propileno , Humanos , Espectrometría de Fluorescencia/métodos , Reproducibilidad de los Resultados , Fluorometría , ComprimidosRESUMEN
This study aims to develop a novel and selective method for the detection of natamycin (E235) in yoghurt. The suggested method adopts an application of Hantzsch reaction to turn on the fluorescence behavior of natamycin (blue fluorescence), allowing its sensitive and selective determination in yoghurt samples without any overlapping at 485 nm. The originality of the research lies in the fact that this application takes place for the first time, also the detection (LOD) and quantification (LOQ) limits were very low (0.02 and 0.06µg mL-1, respectively) with a linear concentration range of 0.1-1.0 µgmL-1. Moreover, the developed method was employed for the detection of E235 in yoghurt sample with a good recoveries (98.80 ± 1.20-99.20 ± 1.15 (%), over a concentration range of 0.5-1.0 µgmL-1, (LOD = 0.04 and LOQ = 0.12 µgmL-1). Furthermore, the specificity and convenient application of our intended method is an attempt to determine E235 in milk anddairy products with easily followable steps.
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Límite de Detección , Natamicina , Espectrometría de Fluorescencia , Yogur , Yogur/análisis , Natamicina/análisis , Espectrometría de Fluorescencia/métodos , Leche/química , Reproducibilidad de los Resultados , Contaminación de Alimentos/análisisRESUMEN
Pathogenic bacteria and viruses are the main causes of infectious diseases all over the world. Early diagnosis of such infectious diseases is a critical step in management of their spread and treatment of the infection in its early stages. Therefore, the innovation of smart sensing platforms for point-of-care diagnosis of life-threatening infectious diseases such as COVID-19 is a prerequisite to isolate the patients and provide them with suitable treatment strategies. The developed diagnostic sensors should be highly sensitive, specific, ultrafast, portable, cheap, label-free, and selective. In recent years, different nanosensors have been developed for the detection of bacterial and viral pathogens. We focus here on label-free miniaturized nanosensing platforms that were efficiently applied for pathogenic detection in biological matrices. Such devices include nanopore sensors and nanostructure-integrated lab-on-a-chip sensors that are characterized by portability, simplicity, cost-effectiveness, and ultrafast analysis because they avoid the time-consuming sample preparation steps. Furthermore, nanopore-based sensors could afford single-molecule counting of viruses in biological specimens, yielding high-sensitivity and high-accuracy detection. Moreover, non-invasive nanosensors that are capable of detecting volatile organic compounds emitted from the diseased organ to the skin, urine, or exhaled breath were also reviewed. The merits and applications of all these nanosensors for analysis of pathogenic bacteria and viruses in biological matrices will be discussed in detail, emphasizing the importance of artificial intelligence in advancing specific nanosensors.
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COVID-19 , Enfermedades Transmisibles , Nanoporos , Virus , Humanos , Inteligencia Artificial , COVID-19/diagnóstico , BacteriasRESUMEN
Potentiometric sensors based on ion-selective membrane electrodes have continued to get great attention from the scientific community. These sensors have been employed in several applications including medicine, forensic analysis, environmental assessment, industry, agriculture, and pharmaceutical drug analysis. Indeed, these sensors possess several advantages, for example, simple design, fabrication, and manipulation, rapid response time, good selectivity, applicability to colored and turbid solutions, and possible interfacing with automated and computerized systems. On the other hand, therapeutic drug monitoring and the detection of pharmaceutical drugs in their pharmaceutical formulations and biological matrices are highly significant from a medical point of view, especially for drugs with a narrow therapeutic index, such as anticancer drugs, which can cause fatal side effects for patients. Interestingly, potentiometric sensors have been broadly employed as one of the most important electrochemical approaches for pharmaceutical drug analysis. Moreover, the breakthroughs in potentiometric sensors based on ion-selective electrodes (ISEs) make them superior to the other reported methods for pharmaceutical drug analysis in terms of many performance parameters, such as sensitivity, selectivity, low detection limit, and low cost. In this review, we try to offer a summary prologue to the applicability and merits of potentiometric sensors that have been employed for pharmaceutical drug analysis while emphasizing their application for the assay of pharmaceutical drugs in their dosage forms and the in-vivo assay of pharmaceutical drugs in different biological samples such as milk, water, plasma, and urine.
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Electrodos de Iones Selectos , Agua , Humanos , Preparaciones Farmacéuticas , PotenciometríaRESUMEN
Developing new, cheap, sensitive and selective chemiluminescence (CL) systems with multiple detection properties is still a big challenge for biological and environmental applications. Here, we report a new CL system having multiple detection applications (environmental and biological). The developed lucigenin-pyrogallol system gave an enhancement (190 times) over the conventional lucigenin-H2O2 CL system. Cobalt ion and tyrosinase can inhibit lucigenin-PG CL intensity. Based on these phenomena, we have developed new CL methods for the detection of pyrogallol (LOD = 0.94 µM), lucigenin (LOD = 0.42 µM), cobalt (LOD = 68 nM), and tyrosinase (LOD = 1.8 µg/mL). Furthermore, the developed system gave excellent recoveries in real samples within the range of 93.59-103.12% for the assay of pyrogallol, Co2+ and tyrosinase in coffee, lake water, and human plasma, respectively.
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Luminiscencia , Pirogalol , Acridinas , Cobalto , Humanos , Peróxido de Hidrógeno , Mediciones Luminiscentes/métodos , Monofenol MonooxigenasaRESUMEN
In this work, a glutathione (GSH) sensing nano-platform using lucigenin as a fluorescent probe in the presence of MnO2 nanosheets was reported for the first time. Unlike the earlier fluorescent detection systems based on MnO2 nanosheets, which depend on Förster resonance energy transfer (FRET) or the dynamic quenching effect (DQE), the mechanism of the quenching process of MnO2 nanosheets on lucigenin fluorescence was attributed mainly to a static quenching effect (SQE) with a minor contribution of the inner filter effect (IFE). A double exponential fluorescence decay of lucigenin was obtained in various MnO2 nanosheet concentrations as a result of their SQE and IFE. Based on this phenomenon and taking advantage of the redox reaction between GSH and MnO2 nanosheets, we have developed a switch-on sensitive fluorescent method for GSH via the recovery of the MnO2 nanosheet-quenched fluorescence of lucigenin. A good linearity range of 1.0-150.0 µM with a low limit of detection (S/N = 3) of 180.0 nM was achieved, revealing the higher sensitivity for GSH determination in comparison with the previously reported MnO2 nanosheet-based turn-on fluorescent methods. The developed fluorescent nano-platform exhibits excellent selectivity with successful application for GSH detection in human serum plasma, indicating its good practicability for GSH sensing in biological and clinical applications.
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Acridinas/química , Colorantes Fluorescentes/química , Glutatión/sangre , Compuestos de Manganeso/química , Nanopartículas/química , Óxidos/química , Humanos , Compuestos de Manganeso/síntesis química , Estructura Molecular , Óxidos/síntesis química , Tamaño de la Partícula , Propiedades de SuperficieRESUMEN
Women are the most ones who susceptible to a common syndrome called fibromyalgia syndrome, up to 90% of all people with fibromyalgia are women. It affects mainly muscles and soft tissue and cause for them muscle pain, sleep problems and painful tender points. Milnacipran is acting as a serotonin-norepinephrine reuptake inhibitor (SNRI) therefore, it is recommended for the treatment of this syndrome. The widespread use of this compound in our market requires the development and validation of a simple, sensitive, cheap, fast and reproducible spectrofluorimetric method for the assay of milnacipran hydrochloride in its pure state, pharmaceutical tablets and spiked human urine and plasma. In the current work ninhydrin and phenylacetaldehyde in Teorell and Stenhagen buffer (pHâ¯7) reacts with the amino moiety of milnacipran through a sensitive condensation reaction resulting in formation of a fluorescent product, which exhibits its fluorescence emission intensity at 465â¯nm after excitation at 390â¯nm. It is observed that, in the concentration range 0.5 to 3.0⯵gmL-1, the constructed calibration curve was linear with a good correlation coefficient (0.9998). The condensation reaction was successfully applied for the assay of the studied drug in Avermilan® tablets, spiked human urine and plasma without interference from the components of the sample matrix with average percentage recoveries of 101.73⯱â¯0.56 and 100.55⯱â¯0.64 for urine and plasma, respectively.
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Milnaciprán/sangre , Milnaciprán/orina , Ninhidrina/química , Espectrometría de Fluorescencia/métodos , Humanos , Límite de Detección , Modelos Lineales , Reproducibilidad de los Resultados , Inhibidores Selectivos de la Recaptación de Serotonina/sangre , Inhibidores Selectivos de la Recaptación de Serotonina/orina , ComprimidosRESUMEN
Our article presents the development and validation of two simple, very sensitive, and low-cost spectroscopic methods for the assay of milnacipran hydrochloride in bulk form, pharmaceutical tablets and spiked human urine and plasma. Spectroscopic methods (spectrophotometric and spectrofluorimetric techniques) were dependent on the chromogenic and fluorogenic properties of the 4-chloro-7 nitrobenzofurazan (NBD-Cl) reagent. The reaction product, resulting from the interaction between NBD-Cl and milnacipran in the presence of borate buffer pH 8.5, was measured spectrophotometrically at 465 nm and spectrofluorimetrically at 510 nm after excitation at 465 nm. The absorbance-concentration plot was rectilinear over the range of 1.5-12 µg mL-1 with a limit of quantitation 1.09 µg mL-1, while the fluorescence-concentration plot was rectilinear over the range of 0.03-0.5 µg mL-1 with a limit of quantitation 0.02 µg mL-1. Influential parameters affecting the development and stability of the reaction product were studied and optimized. Assurance of the cited drug in its tablets by our proposed methods was successfully completed without obstruction from the presence of the basic excipients with average percentage recoveries of 99.27 ± 1.18 and 99.44 ± 0.69 for the spectrophotometric and spectrofluorimetric methods, respectively. The spectrofluorimetric method was additionally adopted as a preliminary in vitro study for the assay of the cited drug in spiked human urine and plasma with average percentage recoveries of 101.52 ± 1.01 and 100.38 ± 1.57 for spiked urine and plasma, respectively.
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A simple and sensitive spectrofluorimetric method has been development for the assurance of quetiapine fumarate (QTF). The proposed method was utilized for measuring the fluorescence intensity of the yellow fluorescent product at 510nm (λex 470nm). The fluorescent product has resulted from the nucleophilic substitution reaction of QTF with 4-chloro-7-nitrobenzofurazane (NBD-Cl) in Mcllvaine buffer (pH7.0). The diverse variables influencing the development of the reaction product were deliberately changed and optimized. The linear concentration range of the proposed method was of 0.2-2.0µgml-1.The limits of detection and quantitation were 0.05 and 0.17µgml-1, respectively. The proposed method was applied for the assurance of QTF in its tablets without interference from basic excipients. In addition, the proposed method was used for in vitro analysis of the QTF in spiked human plasma, the percent mean recovery was (n=3) 98.82±1.484%.