Commercial Tablets Research Articles

Validated Spectrofluorometric Assay for Folic Acid Determination in Pure and Pharmaceutical Forms via Basic Fuchsin Fluorescence Quenching.

A simple, specific, sensitive, rapid, and cost-effective spectrofluorometric method for quantifying folic acid has been developed using basic fuchsin as a fluorescence quenching agent. This method relies on the quenching effect of folic acid on the inherent fluorescence of basic fuchsin, facilitated by their interaction in Britton-Robinson buffer solution at pH 9, leading to the formation of an ion-associated complex. The decrease in fluorescence intensity of basic fuchsin was measured at 730 nm, with excitation at 365 nm. The method demonstrated a linear relationship (R2 = 0.9977) between the quenching fluorescence intensity (ΔF) and folic acid concentration over the range of 4-20 μg/mL, with a detection limit of 0.17 μg/mL. The method showed no significant interference from common excipients found in pharmaceutical tablets. The results obtained were in good agreement with those from high-performance liquid chromatography, with no significant differences in precision or accuracy. This spectrofluorimetric method was successfully applied to determine the folic acid content in various commercial pharmaceutical tablets.

Development and Validation of an optimized HPLC-UV analytical method for the quantification of 5-Methyltetrahydrofolate (Active Folate) in dietary Supplements: Application to commercial tablets and capsules

5-MTHF is the active form of folic acid, and it is provided as a dietary supplement in the market. Therefore, in this study we provide a new, simple and economic HPLC-UV analysis method to quantify 5-MTHF in dietary supplement. A new HPLC-UV method was developed and validated for the quantification of 5-methyltetrahydrofolate in dietary supplements. The method was optimized in terms of chromatographic conditions, including the mobile phase composition, chromatographic column, and the sample preparation diluent using ascorbic acid. A combination of ammonium acetate buffer with methanol (90:10) was the optimal mobile phase, achieving a retention time of approximately 11.4 min on C18 column with good column performance (N = 6786, Asymmetry = 1.03). The method was validated for selectivity, linearity, precision, accuracy, and robustness. The calibration curve was linear (r2 > 0.999) over the concentration range of 1.20 to 4.80 µg/mL. Precision was demonstrated with RSD% values ranging from 1.38 % to 2.90 % for intra-day precision and 0.96 % to 2.61 % for inter-day precision. Accuracy was confirmed with recovery values between 96.5 % and 110.6 % for spiked samples. To demonstrate the method’s applicability, ten brands of 5-MTHF dietary supplements were collected from local pharmacies. Assay results showed significant variability, with four brands having contents below the acceptable range (90–110 % of labeled contents) and two brands exceeding this range. The stability of 5-MTHF in these products appeared to be formula-dependent, emphasizing the need for regulatory revisions to mandate stability testing for dietary supplements.

Concurrent Estimation of Pregabalin and Etoricoxib by New Stability-Indicating RP-UPLC Approach - Application in Assay of Commercial Tablets

Background: The study emphasizes establishing a stability-indicating RP-UPLC method for concurrent estimation of pregabalin and etoricoxib in combined pharmaceutical formulations, confirming effective separation, sensitivity, and repeatability, validated according to ICH guidelines. Objective: The present research study aims to establish a new stability-indicating RP-UPLC method for concurrently estimating pregabalin and etoricoxib in blended powder and their combined tablet formulation with less run time, high sensitivity, and specificity. Methods: The effective separation of pregabalin and etoricoxib was achieved with HSS column C18 (150x2.1mm,1.8μm), 0.1% orthophosphoric acid:acetonitrile (65:35 v/v) at a flow rate of 0.3mL/min, and isocratic elution at 228nm. The elution of PRB and ETB was noticed at 1.56 and 2.01 minutes, with good resolution and system suitability with the developed approach. Results: Pregabalin and etoricoxib have shown linear responses from 18.75 to 112.5μg/mL and 15 to 90μg/mL, respectively. The range of the % RSD for intraday and inter-day precision was 0.33 to 0.81. The LOD and LOQ of pregabalin and etoricoxib were computed to be 0.07 μg/mL and 0.21 μg/mL, and 0.01μg/mL and 0.04 μg/mL, respectively, by standard deviation method. The validation method was carried out using ICH standards. The stability-indicating feature of the method was confirmed by the forced degradation studies where degradants generated by stress testing were clearly distinguished from the peaks of analytes. Conclusion: The shorter elution period and superior sensitivity of both analytes with this method have been found to be appropriate for regular analysis of pregabalin and etoricoxib.

Evaluation of Mucoadhesive Nano-Bilosomal In Situ Gels Containing Anti-Psychotic Clozapine for Treatment of Schizophrenia: In Vitro and In Vivo Studies

Background/Objectives: Patients with schizophrenia have significant challenges in adhering to and complying with oral medicines, resulting in adverse consequences such as symptom worsening and psychotic relapse. Methods: This study aimed to develop clove oil-based bilosomes using definitive screening design (DSD) to maximize the anti-schizophrenic action of clozapine and promote its nose-to-brain delivery. The target was to optimize the physicochemical properties of bilosomes and incorporate them into mucoadhesive intranasal in situ gels, searching for augmented ex vivo and in vivo clozapine delivery. Results: The bilosomes’ particle size was decreased by increasing the span, SDC, and clove oil amounts. In addition to using a high lipid amount, the aforementioned components also helped increase the entrapment efficiency values. Increased zeta potential was only observed by increasing surfactant amount and reducing clozapine concentration. After incorporation of optimized liquid clove oil-based bilosomes, which had a spherical nano-sized vesicular shape, into P 407-dependent gels, an HPMC (2% w/w)/P 407 (20% w/w)-containing formulation (G6) was selected as an optimized gel owing to its acceptable gelation time (13.28 s), gel strength (27.72 s), viscosity (12,766.67 cP), and mucoadhesive strength (4273.93 dyne/cm2). The optimized G6 exhibited higher Jss (50.86 μg/cm2·h−1) through the nasal mucosa compared to the control gel (23.03 μg/cm2·h−1). Compared to the control gel, G6 displayed higher relative bioavailability (491.37%) than a commercial tablet (264.46%). Following ELISA analysis, dopamine and serotonin were significantly reduced, while BDNF was remarkably increased after administration of optimized G6 into schizophrenic rats. Conclusions: Our study indicates the potential of intranasal bilosomal gels in upgrading the anti-schizophrenic and neuroprotective activity of clozapine.

Utility of Microwave-Synthesized Silver Nano Particles as Spectrofluorimetric Sensors for the Determination of Nano Concentrations of Favipravir: Application to Dosage Forms and Spiked Human Plasma.

A simple and facile microwave-assisted method was developed for the synthesis of highly fluorescent silver-nanoparticles (Ag-NPs). The synthesis of silver-nanoparticles depends on a redox reaction between silver nitrate and ascorbic acid using chitosan as a stabilizing agent. The produced Ag-NPs were characterized using Zeta potential and transmission electron microscope micrograph where they are spherical in shape with smooth surface morphology and size of 26.81 ± 2.2nm. Favipiravir (FAV) was found to cause an obvious enhancement in the fluorescence of Ag-NPs; hence, they were used for its spectrofluorimetric estimation. The fluorescence intensity was measured at 430nm after excitation at 360nm. Under optimum conditions, a good linear relationship was accomplished between the FAV concentration and the fluorescence intensity in a range of (5.0-200.0) ng/mL with a limit of detection of 1.59 ng/mL. The method was successfully applied for the assay of the drug in its commercial tablets and spiked human plasma samples, and the results obtained were satisfactory.

Novel Fimasartan Fluidized Solid Dispersion and Its Tablet: Preparation, Crystallinity, Solubility, Dissolution, and Pharmacokinetics in Beagle Dogs.

Fimasartan, an angiotensin II receptor antagonist, exhibits low bioavailability due to its poor solubility; consequently, using solubilization technologies is essential to improve its bioavailability. In this study, novel fimasartan fluidized solid dispersion (FFSD) was developed using a fluid bed granulator to enhance the drug solubility andoral bioavailability. An appropriate FFSD was prepared in 50% ethanol using a fluid bed granulator, and its drug dissolution, morphology, and crystallinity were evaluated in comparison to the powdered drug. Moreover, the dissolution in various pH conditions and pharmacokinetics of the FFSD tablet in beagle dogs were investigated compared to the commercial fimasartan tablet. Among the hydrophilic polymers tested, hydroxypropyl methylcellulose (HPMC)showed the highest solubility. The FFSD, composed of fimasartan, HPMC, and microcrystalline cellulose at the weight ratio of 20:10:25, gave a granular aggregation of several particles with a smooth surface. The drug in this FFSD existed as an amorphous state, leading to a greatly increased drug dissolution. The FFSD tablet was prepared by compressing a mixture of FFSD, mannitol, croscarmellose sodium, and magnesium stearate at the weight ratio of 55:40:5:1. The FFSD tablet gave significantly higher drug dissolution, plasma concentrations, maximum plasma concentration (Cmax) andarea under the whole blood concentration-time curve (AUC) values than did the commercial fimasartan tablet. In the beagle dogs, the FFSD tablet (140.39±27.40ng·h/ml) had about a 1.7-fold higher AUC than the commercial fimasartan tablet (80.58±22.18 ng·h/ml), indicating an enhancement in thebioavailability. This novel FFSD tablet could be a potential oral pharmaceutical product with the improved oral bioavailability of fimasartan.

Copper-decorated covalent organic framework covalently modified 3D-printed nanocarbon electrodes for the determination of methotrexate

3D printing has emerged as a popular topic in electrochemistry due to its high flexibility in production. In this work, we used graphene/polylactic acid materials for the fabrication of 3D printed electrodes (3DEs) via fused deposition modeling (FDM). Subsequently, the synthesized novel copper-decorated covalent organic framework (Cu(II)@S-COF) was covalently bound on the 3DE by the Au-S bonding to construct the Cu(II)@S-COF@Au@3DE sensor. Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and contact angle experiments were used to characterize the prepared 3DEs. Cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) were used to investigate the electrochemical performance of the prepared 3DEs. The sensor exhibited good electrocatalytic performance for detecting methotrexate (MTX). It was capable of accurately determining MTX in the range from 0.5 to 100 μM with a limit of detection (LOD) of 0.07 μM and a sensitivity of 0.1489 μA μM−1 cm−2. In addition, the sensor has recoveries from 97.33% to 101.09% for the detection of MTX in commercial tablets and urine samples, so it can be used to detect MTX in real samples successfully. This work opens a novel avenue for using metal-decorated COF materials in the field of electrochemistry.

Streamlined turn-off fluorescence sensing of Donepezil: Enhancing evaluation in pharmaceutical formulations, quality control labs, and biological fluids at nano levels

Donepezil (DPZ) is used to treat Alzheimer’s disease by increasing acetylcholine in the brain, necessitating precise analytical methods for its evaluation. This study aims to develop and validate a new turn-off fluorescence sensing method for quantifying DPZ, enhancing its evaluation in pharmaceutical formulations, quality control laboratories, and biological fluids. By leveraging the fluorescence-quenching interplay between DPZ and tetrabromofluorescein, the assay parameters were fine-tuned to enhance the development of an ion-associated complex. The developed method demonstrated a measurement range from 40 to 800 ng/mL, with detection and quantification limits of 12.6 ng/mL and 38 ng/mL, respectively. However, the successful application of the method to commercial DPZ tablets and plasma samples confirmed its effectiveness for both quality control labs and clinical research settings. It ensured accurate content uniformity and high precision, making it ideal for routine DPZ monitoring. In contrast to previous methods, this approach emphasizes environmental sustainability, evaluated using advanced tools like the Eco score scale, AGREE, RGB12, and BAGI. These tools facilitated a thorough assessment of the method’s ecological impact and sustainability, underscoring its advantage over traditional methods in terms of environmental responsibility.

Optimization and characterization of a dose-controllable orodispersible dexamethasone film for personalized medicine

Decadron® tablets are commercially available in 0.5 and 4 mg formulations, often requiring the use of multiple tablets or fractional doses when the required dosage is unavailable. This practice can lead to inaccuracies and handling difficulties associated with tablet splitting and crushing tablets into powder. This study aimed to develop an orodispersible dexamethasone film that would allow precise dose control and overcome these challenges. The film formulation was optimized by dissolving varying amounts of hypromellose, glycerol, and dexamethasone in ethanolic solutions. These solutions were cast and dried at different thicknesses. Statistical optimization using the design of experiments was used to determine the ideal film composition. The optimized films met pharmaceutical standards, with a mass variation ≦ 2 %, thickness variation ≦ 2.5 %, and disintegration time ≦ 20 s. The uniform distribution of dexamethasone within the film enabled easy content control based on the film area. Dissolution testing indicated that the dissolution behavior of the film formulation behaved similarly to commercial tablets for up to 90 min. In conclusion, the developed orodispersible film offers precise dexamethasone dose control and addresses the limitations of tablet splitting, positioning it as a promising candidate for personalized medicine applications.

Preparation, Swelling, and Drug Release Studies of Chitosan-based Hydrogels for Controlled Delivery of Buspirone Hydrochloride.

Buspirone is used for the management of depression and anxiety disorders. Due to its short half-life and low bioavailability, it requires multiple daily doses and is associated with some side effects. This study aimed to develop chitosan-based hydrogels as drug-controlled release carriers. The objective of this study is to prepare chitosan-based hydrogels as controlled release carriers in order to overcome the side effects of buspirone HCl and improve patients' compliance and their life quality. Polymer chitosan was polymerized with two monomers, acrylic acid and itaconic acid, to synthesize pH-sensitive hydrogel. The Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) analysis were performed to confirm the structure formation and thermal stability. Water penetration capability and loading of the drug were performed by porosity and drug loading studies. The swelling and dissolution tests were performed to analyze the pH-sensitive nature of the developed hydrogels. FTIR, TGA, and DSC demonstrated that the chitosan-based hydrogels were successfully prepared. An increase in water penetration and drug loading into the hydrogel network was seen with the high incorporation of chitosan, acrylic acid, and itaconic acid. The swelling and dissolution studies revealed that prepared hydrogel offered the greatest swelling and drug release at a high pH of 7.4. The swelling and drug release from the hydrogel were affected by the concentrations of the incorporated contents. A controlled release of the drug was achieved by using chitosan-based hydrogel as a delivery carrier compared to commercial tablets of buspirone. The results showed that the developed chitosan-based hydrogel can be considered one of the most suitable drug carrier systems for the controlled delivery of buspirone.

Oral Gels as an Alternative to Liquid Pediatric Suspensions Compounded from Commercial Tablets.

The aim of the study was to propose pharmacy-compounded oral gels as a new and alternative dosage form that is attractive to children as having a better masking taste than syrups and reducing the risk of spilling. The application and physical properties of the gels prepared with cellulose derivatives (hydroxyethylcellulose and carmellose sodium) or carbomers were evaluated. The results of the study showed the most suitable consistency, viscosity, and organoleptic properties for gels prepared with carbomer and cellulose derivatives at concentrations of 0.75% and 2.0%, respectively. The microbial stability of the gels was guaranteed by the use of methylparaben and potassium sorbate. VAL (valsartan) and CC (candesartan cilexetil) tablets, often used off-label in children, were pulverized and suspended in the hydrogel bases, resulting in final drug concentrations of 4 mg/g and 1 mg/g, respectively. There was no significant change in viscosity and consistency parameters when the pulverized tablets were added, and only small changes in viscosity and consistency were observed during 35 days of storage, especially in the gels with sodium carmellose and candesartan. On the basis of the drug assay, an expiry date of 25 °C was recommended: 35 days for valsartan and 14 days for candesartan preparations.

Formulation and <i>in vitro</i> Evaluation of Liquisolid Compact of Celecoxib

<i>Introduction</i>: The liquisolid technique presents a promising avenue for enhancing the dissolution rate and bioavailability of poorly water-soluble drugs like celecoxib. This study investigated the formulation and evaluation of celecoxib tablets using this technique. <i>Aim</i>: To formulate and evaluate celecoxib tablets using the liquisolid technique, with the objective of enhancing its dissolution rate and bioavailability. <i>Methods</i>: Celecoxib tablets were prepared using the liquid-solid technique by incorporating a non-volatile liquid medication carrier and a suitable solid carrier. Various formulations were developed by altering the ratios of drug, carrier, and coating materials. The prepared tablets were characterized for their physical properties, drug content uniformity, <i>in vitro</i> dissolution behavior, and compatibility using Fourier-transform infrared (FTIR) spectroscopy. <i>Results</i>: The solubility profile showed that the maximum rate of solubility was recorded in PEG-400 (11.03 ± 0.01) when compared to other non-volatile solvents. The angle of slide, indicated that the excipients used were within the acceptable limit of 33°. The FTIR spectroscopy showed compatibility of the drug and excipients. The results of the SEM showed that spherically-shaped vesicles were formed. Evaluation of the pre-compression parameters indicated that the drug content was highest in batch F-11 hence its optimization (96.1 ± 0.90). The post compression evaluation indicated that the official tests were within the acceptable range for disintegration time (2.25 ± 0.35). The results of the <i>in vitro</i> release studies of the optimized formulation, conventional tablet and reference commercial tablet showed that the amount of drug released increased steadily with time over the 1-hour period. <i>Conclusion</i>: Our findings underscore its viability as a strategy to enhance the therapeutic efficacy of poorly water-soluble drugs, offering promising prospects for pharmaceutical formulation.

Formulation and Evaluation of Solid Dispersion of Phenytoin by Solvent Evaporation Technique

The aim of the present study is Formulation and Evaluation of Phenytoin by making solid dispersion with polyvinyl alcohol and inclusion complexation with HPβ Cyclodextrin, β Cyclodextrin. Solid dispersion of Phenytoin is prepared with Solvent Evaporation method. Phenytoin belongs to BCS class II drug which is characterized by high membrane permeability, slow dissolution rate due to low aqueous solubility. It is an anti-epileptic or anti- convulsant is used to treat wide variety of Seizures. The Phenytoin solid dispersions were prepared by solvent evaporation method at 1:0.25, 1:0.5, 1:0.75, 1:1, 1:1.25, 1:1.5 ratios of Phenytoin to HP β CD, β CD and PVA. The prepared dispersions were evaluated by solubility studies, in-vitro dissolution studies, melting point determination, drug content uniformity, entrapment efficiency and FT-IR studies. Finally comparing all the formulations (P:HPβ F1-P:HPβ F6) (P: βF1-P βF6) and (P:PF1-P:PF6) formulation P:PF4 containing Phenytoin: Polyvinyl alcohol (1:1) shows better result at the end of 90 min with drug release 93.99%, hence it was selected as the best formulation. By release kinetic studies of best formulation of Phenytoin with zero order and first order we can say that the best formulation follows first order kinetics studies having r2 value 0.945 where as zero order release kinetics studies having r2 value 0.849. The results indicated as formulated solid dispersion tablets displayed better dissolution profiles as compared to existing commercial tablets.

Amorphous Solid Dispersion Formation for Enhanced Release Performance of Racemic and Enantiopure Praziquantel.

Praziquantel (PZQ) is the treatment of choice for schistosomiasis, which affects more than 250 million people globally. Commercial tablets contain the crystalline racemic compound (RS-PZQ) which limits drug dissolution and oral bioavailability and can lead to unwanted side effects and poor patient compliance due to the presence of the S-enantiomer. While many approaches have been explored for improving PZQ's dissolution and oral bioavailability, studies focusing on investigating its release from amorphous solid dispersions (ASDs) have been limited. In this work, nucleation induction time experiments were performed to identify suitable polymers for preparing ASDs using RS-PZQ and R-PZQ, the therapeutically active enantiomer. Cellulose-based polymers, hydroxypropyl methylcellulose acetate succinate (HPMCAS, MF grade) and hydroxypropyl methylcellulose (HPMC, E5 LV grade), were the best crystallization inhibitors for RS-PZQ in aqueous media and were selected for ASD preparation using solvent evaporation (SE) and hot-melt extrusion (HME). ASDs prepared experimentally were subjected to X-ray powder diffraction to verify their amorphous nature and a selected number of ASDs were monitored and found to remain physically stable following several months of storage under accelerated-stability testing conditions. SE HPMCAS-MF ASDs of RS-PZQ and R-PZQ showed faster release than HPMC E5 LV ASDs and maintained good performance with an increase in drug loading (DL). HME ASDs of RS-PZQ formulated using HPMCAS-MF exhibited slightly enhanced release compared to that of SE ASDs. SE HPMCAS-MF ASDs showed a maximum release increase of the order of 6 times compared to generic and branded (Biltricide) PZQ tablets. More importantly, SE R-PZQ ASDs with HPMCAS-MF released the drug as effectively as RS-PZQ or better, depending on the DL used. These findings have significant implications for the development of commercial PZQ formulations comprised solely of the R-enantiomer, which can result in mitigation of the biopharmaceutical and compliance issues associated with current commercial tablets.

Multivariate approaches for assessing dissolution behaviour of spironolactone. Dissolution-driven determination of polymorphic purity limits

Spironolactone (SPN) is an aldosterone antagonist effective for preventing and controlling cardiovascular diseases. Form I and Form II exhibit different behaviour in their dissolution properties, which can compromise the quality of the pharmaceutical formulation. Hence, in the present work, we propose the combination of two multivariate approaches to estimate the polymorphic purity of SPN in commercial tablets and predict the dissolution behaviour of these formulations considering their polymorphic composition. Multiple linear regression (MLR) approach was applied to model the dissolution behaviour of formulations depending on their polymorphic composition, showing excellent agreement among actual vs. predicted dissolution curves. This model was applied to establish a design space were the risks of dissolution failure due to the polymorphic purity was avoided. Next, to evaluate the purity of Form II of SPN in formulated products, two quantitative partial least squares (PLS) models were developed based on near (NIR) and mid (MIR) infrared spectroscopies. Training (n = 14) and validation (n = 8) sets were prepared by mixing both polymorphs and the excipient matrix to simulate commercial tablets. Methodologies showed recoveries non-statistical different from 100 %, but MIR-PLS model showed a higher dispersion (100.1 ± 1.82 % and 99.5 ± 6.94 % for NIR and MIR, respectively). Similar values of Form II content (1.02 ± 0.01 w/w with NIR and 1.03 ± 0.03 w/w with MIR) were obtained during the analysis of commercial and spiked SPN tablets. Finally, NIR-PLS was coupled to MLR model for the prediction of dissolution in entire tablets based on polymorphic composition to act as Quality by Design (QbD) tool. The full coincidence among actual and NIR-MLR predicted curves validated the final purpose of this approach.

Enhanced Oral Bioavailability and Stability Studies of Loratadine Tablets Based on Solid Dispersion of Modified Ziziphus spina-christi Gum

Background: Solid dispersion is a common technique used for solubility enhancement of poorly soluble drugs. Objective: In this study, loratadine (LOR), a class II biopharmaceutical classification system (BCS), was formulated as solid dispersion tablets using modified Ziziphus spina-christi gum (MZG) as a carrier. Methods: The solvent evaporation method was used for LOR-MZG solid dispersion (SD) preparation. A variety of tests were conducted to characterize and optimize the formulation. Solubility, Fourier transform infrared (FTIR) analysis, Differential Scanning Calorimetry (DSC), X-Ray Diffraction (X-RD), and Scanning Electron Micrograph (SEM) of solid dispersions were carried out. Accelerated stability testing and pharmacokinetic studies of formulated tablets were also performed using albino Wistar rats. Results: Solid dispersion improved the solubility of LOR by 51 folds. FTIR spectra excluded drugpolymer interactions, and results obtained by DSC, X-RD, and SEM proved the transition from the crystalline to the amorphous state. The stability of LOR-MZG solid dispersion tablets was found to be better when the Alu-Alu package was used. The pharmacokinetics of LOR-MZG compared to MZG-free loratadine tablets (LOR pure) and commercial loratadine tablets (LOR-TM) following oral administration revealed that about 6 folds and 10 folds bioavailability were achieved with LOR-MZG compared to LOR pure and LOR-TM, respectively. Conclusion: Such promising results encourage more studies on MZG to be used for improving the aqueous solubility and bioavailability of a wide range of poorly soluble drugs.

One-pot derivatization spectrofluorimetric method for detection of aspartame in sweetener commercial tablets and soft drinks: Greenness assessments of the methodology.

Aspartame is an artificial sweetener used in drinks and many foods. International Agency for Research on Cancer classified aspartame as possibly carcinogenic to humans (IARC Group 2B). In this study, a sensitive and selective spectrofluorimetric method was developed to detect aspartame. The method is based on switching on the fluorescence activity of aspartame upon its condensation with O-phthalaldehyde (Roth's reaction) in the presence of 2-mercaptoethanol. The reaction product was detected fluorometrically at λem of 438 nm after λex of 340 nm. All reaction conditions required to yield the optimal fluorescence intensity were observed and investigated. Furthermore, the approach was validated according to ICH guidelines. Upon plotting the concentrations of aspartame against their associated fluorescence intensity values, the relationship between the two variables was linear within the range of 0.5-3.0μg/mL. Furthermore, the method was employed to analyze the quantity of aspartame in commercial packages and soft drinks with an acceptable level of recovery. In addition, the Green Solvents Selecting Tool, Complementary Green Analytical Procedure Index, and the Analytical Greenness Metric tool were used to evaluate the sustainability and the greenness of the developed methodology.

Self-Microemulsifying Drug Delivery System to Enhance Oral Bioavailability of Berberine Hydrochloride in Rats.

Berberine hydrochloride (BH) is a versatile bioactive compound derived from the plants of the Berberis genus, known for its various pharmacological effects. However, its oral bioavailability is low due to its high hydrophilicity and limited permeability. To enhance its clinical efficacy and oral bioavailability, this study designed and prepared a BH-loaded self-microemulsifying drug delivery system (BH-SMEDDS), and characterized its in vitro and in vivo properties. Firstly, the optimal formulation of BH-SMEDDS was selected using solubility evaluations, pseudo-ternary phase diagrams, and particle size analysis. The formulation containing 55% Capmul MCM, 22.5% Kolliphor RH 40, and 22.5% 1,2-propanediol was developed. BH-SMEDDS exhibited stable physicochemical properties, with an average particle size of 47.2 ± 0.10 nm and a self-emulsification time of 26.02 ± 0.24 s. Moreover, in vitro dissolution studies showed significant improvements in BH release in simulated intestinal fluid, achieving 93.1 ± 2.3% release within 300 min. Meanwhile, BH-SMEDDS did not exhibit cytotoxic effects on the Caco-2 cells. Additionally, BH-SMEDDS achieved a 1.63-fold increase in oral bioavailability compared to commercial BH tablets. Therefore, SMEDDS presents a promising strategy for delivering BH with enhanced oral bioavailability, demonstrating significant potential for clinical application.

GREEN HPLC DETERMINATION OF PHENYTOIN AND METHOD VALIDATION

Objective: In this study, the chromatographic behavior of the antiepileptic drug phenytoin was determined by the green HPLC method. The optimization of the developed method was based on the capacity factor values of phenytoin in varying water-ethanol binary mixtures and the ethanol concentration in the mobile phase where the compound was analyzed. Material and Method: Ethanol-water binary mixtures containing 35%, 40%, and 45% (v/v) ethanol were used in the optimization for the determination performed by the RPLC method. Retention times of the compound were determined with the Zorbax SB-CN (150x4.6 mm, 3.5 µm ID) column. Analyzes were performed at a constant flow rate (0.3 ml/min) and column temperature (37°C). The optimum condition for quantitative analysis was determined as an ethanol-water binary mixture containing 40% (v/v) ethanol with a pH of 6.5. Result and Discussion: In this study, the hydrophobicity of phenytoin was calculated using the logk-φ relationship. The optimum condition was determined using the obtained chromatographic data, and the quantitative determination of phenytoin in the commercial tablet formulation was made by the internal standard method. Under these conditions, excellent linearity (r>0.99) was obtained in the concentration range of 0.8-2.8 μg/ml. The detection limit of the developed method is 0.021 μg/ml; the limit of quantitation was calculated as 0.064 μg/ml. The recovery value of the method was determined as 99.61%. It was concluded that the parameters of precision, accuracy, and method robustness were appropriate for the validation procedures.

Electrochemical Detection of Melatonin at Nano-Sized Highly Boron-Doped Diamond Electrode

This work investigates the electrochemical oxidation of melatonin at boron-doped diamond electrodes and demonstrates the significant enhancement in the detection of melatonin using highly boron-doped diamond nanopowder (h-BDD). Employing differential pulse voltammetry, Tween-coated h-BDD modified screen-printed electrodes (Tween/h-BDD/SPE) showed two linear response ranges for melatonin: 0.057–10 and 10–200 μM, with sensitivities of 390 ± 36 and 72.2 ± 3.4 μA mM–1, respectively, and a detection limit (3Sb/m) of 0.017 μM. The Tween/h-BDD/SPE demonstrated good selectivity against common interferences such as tryptophan, serotonin, lactate, cytidine, cytosine, and urea. The analytical utility of Tween/h-BDD/SPE was validated by quantifying melatonin in commercial pharmaceutical tablets, achieving close to 100% recoveries.