A highly sensitive and green electroanalytical method for the determination of favipiravir in pharmaceutical and biological fluids.

BACKGROUND: Favipiravir is currently used for the treatment of coronavirus disease-2019 (COVID-19). OBJECTIVE: A highly sensitive and eco-friendly electroanalytical method was developed to quantify favipiravir. METHOD: The voltammetric method optimized a sensor composed of reduced graphene oxide / modified carbon paste electrode in the presence of an anionic surfactant, improving the favipiravir detection limit. The investigation reveals that favipiravir-oxidation is a diffusion-controlled irreversible process. The effects of various pH and scan rates on oxidation anodic peak current were investigated. RESULTS: The developed method offers a wide linear dynamic range of 1.5-420 ng/mL alongside a higher sensitivity with a limit of detection in the nanogram range (0.44 ng/mL) and a limit of quantification in the low nanogram range (1.34 ng/mL). CONCLUSION: The proposed method was applied for the determination of favipiravir in the dosage form, human plasma and urine samples. The developed method exhibited good selectivity in the presence of two potential electroactive biological interferants, uric acid which increases during favipiravir therapy and the recommended co-administered vitamin C. The organic solvent-free method greenness was evaluated via the Green Analytical Procedure Index, The present work offers a simple, sensitive and environment-friendly method fulfilling green chemistry concepts.

Green Spectrophotometric Platforms for Resolving Overlapped Spectral Signals of Recently Approved Antiparkinsonian Drug (Safinamide) in the Presence of Its Synthetic Precursor (4-Hydroxybenzaldehyde): Applying Ecological Appraisal and Comparative Statistical Studies.

BACKGROUND: Safinamide, a highly specific inhibitor of monoamine oxidase B, is a new approved prodigious therapy used to cure Parkinson's disease (PD). OBJECTIVE: Before marketing and selling a medicine, manufacturers must guarantee that the manufacturing process is consistent by monitoring levels of process-related chemicals and drug contaminants. Therefore, five precise, fast, and accurate spectrophotometric techniques were employed and evaluated for the simultaneous measurement of safinamide and its synthetic precursor, 4-hydroxybenzaldehyde. METHODS: The first derivative, derivative ratio, ratio difference, dual wavelength, and Fourier self-deconvolution methods worked well to resolve spectral overlap of safinamide and its synthetic precursor, 4-hydroxybenzaldehyde. RESULTS: Safinamide detection limits ranged from 0.598 to 1.315 µg/mL, whereas the 4-hydroxybenzaldehyde detection limit was found to be as low as 0.327 µg/mL. CONCLUSION: According to International Council for Harmonisation (ICH) criteria, all procedures were verified and confirmed to be accurate, robust, repeatable, and precise within reasonable range. No considerable variation was found when comparing the outcomes of the suggested approaches to the findings of previously published methods. The ecological value of established methods was measured: the national environmental methods index (NEMI), the analytical eco-scale, the analytical greenness metric (AGREE), and the green analytical process index (GAPI) were used. HIGHLIGHTS: This is the first spectrophotometric determination of safinamide drug in the presence of its synthetic precursor. Five simple and efficient spectrophotometric approaches were employed to determine a newly approved antiparkinsonian drug in the presence of its synthetic precursor simultaneously. Ecological appraisal was performed for the developed methods using four assessment tools.

Simultaneous analysis of two drugs used as supportive treatment for COVID-19: comparative statistical studies and analytical ecological appraisal.

Pharmaceutical quality control products (QC) demand quick, sensitive, and cost-effective methods to ensure high production at a low cost. Green analytical methods are also becoming more common in pharmaceutical research to cut down on the amount of waste that goes into the environment. Meclizine hydrochloride (MZH) and pyridoxine hydrochloride (PYH) are reported to be excellent for calming down COVID-19. As a result, the amount of MZH and PYH manufactured by multinational pharmaceutical organizations has increased considerably during the last several months. The present work proposes three environmentally friendly, straightforward, and sensitive spectrophotometric procedures for quantification of MZH in the presence of PYH in a pure and marketable formulations. The approaches under examination include ratio subtraction (RSM), induced dual wavelength (IDW), and Fourier self-deconvolution (FSD). PYH, on the other hand, was directly quantified at 290 nm. For both drugs, the procedures follow Beer's law in the range of (5-50 µg/mL). The RSM, IDW, and FSD methods, as well as the zero-order approach for PYH, have all been verified in accordance with ICH standards. The ecological value of established methodologies was determined using four distinct ways: the national environmental methods index (NEMI), the analytical Eco-scale, the Analytical Greenness Metric (AGREE), and the green analytical process index (GAPI). Comparing the findings to those of the previously described spectrophotometric technique, no major changes were identified.

Effects of bee venom and dopamine-loaded nanoparticles on reserpine-induced Parkinson's disease rat model.

Parkinson's disease (PD) is a progressive chronic neurodegenerative condition characterized by the loss of dopaminergic neurons within the substantia nigra. Current PD therapeutic strategies are mainly symptomatic and can lead to motor complications overtime. As a result, alternative medicine may provide an effective adjuvant treatment for PD as an addition to or as a replacement of the conventional therapies. The aim of this work was to evaluate the effects of Bee Venom (BV) and dopamine (DA)-loaded nanoparticles in a reserpine-induced animal model of PD. After inducing PD with reserpine injection, different groups of male rats were treated with L-Dopa, BV, DA-nanoparticles. Our findings showed that BV and DA-nanoparticles administration restored monoamines, balanced glutamate/GABA levels, halted DNA fragmentation, decreased pro-inflammatory mediators (IL-1ß and TNF-α), and elevated anti-inflammatory mediators (PON1) and neurotropic factor (BDNF) levels in comparison with conventional therapy of PD. Furthermore, in a reserpine-induced PD rat model, the ameliorative effects of BV were significantly superior to that of DA-nanoparticles. These findings imply that BV and DA-nanoparticles could be useful as adjuvant treatments for PD.

Utility of Silver-nanoparticles for Nano Spectrofluorimetric Determination of Meropenem and Ertapenem: Bio-analytical Validation.

Bio-analytical, nano-quantitative spectrofluorimetric estimation of two non-classical ß-lactam antibiotics; meropenem (MP) and ertapenem (EP) is presented. The method is based on the enhancement of the fluorescence intensity of MP-Eu3+/EP-Eu3+ with silver nanoparticles (AgNPs). AgNPs were synthesized and characterized by UV and transmission electron microscope (TEM). The plasmon resonance produced an intense absorption maximum at 398.0 nm. TEM micrograph showed the particle morphology with an average particles size of 13.0 ± 2.95 nm. The fluorescence intensities were measured against blank reagents at λem of 396.0 nm and 405.0 nm after excitation at λex 305.0 nm and 303.0 nm for MP and EP, respectively. Under optimum conditions, the relative fluorescence intensity showed a good linear relationship with the concentration ranges of 4.0-14.0 and 4.0 -12.0 ng/mL with excellent correlation coefficients of 0.9998 and 0.9997, and limit of detection of 0.84 and 0.86 ng/mL for MP and EP, respectively. The method was successfully applied for direct analysis of MP and EP in their drug substances and pharmaceutical vials. The significant, sensitivity and practicality of the method facilitated MP detection in real plasma samples. Bio-analytical validation was performed according to FDA. The method was rectilinear over the ranges of, 5.0 -75.0 µg/mL plasma. Interestingly, this described system has a promising benefit for various applications exploiting the dramatically enhanced-fluorescence occurrence.

Selective spectrofluorimetric determination of two corticosteroids along with their co-formulated drugs and degradation products in ophthalmic solution and aqueous humour.

Prednisolone acetate (PNO) and fluorometholone (FRT) are corticosteroids, co-formulated with moxifloxacin HCl (MFX) and cromolyn sodium (CML), respectively. PNO has a negligible quantum yield and its hydrolytic degradation products have enhanced fluorescence, which is 250-fold greater. FRT is a nonfluorescent drug, but its hydrolytic degradation products show reasonable fluorescence; MFX and CML have native fluorescence. Two methods were proposed based on the determination of PNO and FRT via their hydrolytic degradation products in the presence of other degradation products. Method (A) was developed for simultaneous determination of PNO and MFX in the presence of PNO degradation products by measuring peak amplitudes of the first derivative (1 D) of its enhanced fluorescence; PNO and MFX were measured at 345 and 473 nm, respectively. Method (B) is a synchronous fluorescence spectroscopic method for simultaneous determination of FRT and its co-formulated drug CML in the presence of its degradation products. Fluorescence intensities were measured at λem 283 and 347 nm for FRT and CML, respectively, using Δλ = 99.20 nm. Validation of the proposed methods was conducted as per International Council for Harmonisation (ICH) guidelines. The proposed methods were successfully applied for the determination of the proposed drugs in bulk powder, ophthalmic solution, and rabbit's aqueous humour.

Determination of terazosin in the presence of prazosin: Different state-of-the-art machine learning algorithms with UV spectroscopy.

Counterfeit drugs have adverse effects on public health; chromatographic methods can be used but they are costly. In this study, we developed cost-effective and environmentally friendly methodology for the analysis of terazosin HCl (TZ) in the presence prazosin hydrochloride (PZ) using UV spectroscopy in conjunction with machine learning (ML) models. Variable selection algorithms were applied to select most informative spectral variables. Thirty-five ML models were assessed and their performances were compared. The models covered a wide range of prediction mechanisms, such as tree-based, linear, self-organizing maps, neural network, Gaussian process, boosting, bagging, Bayesian models, kernel methods, and quantile regression. The values of the root mean square error (RMSE), coefficient of determination (R2), and absolute mean error (MAE) were obtained for the evaluation of the developed models. According to the results of these performance indices, linear model showed the highest prediction capacity among all other models. RMSE, R2 and MAE values of (0.159, 0.997 and 0.131) and (0.196, 0.99 and 0.161) were obtained for train and test datasets, respectively. The predictive models in this study can be useful for the researchers who are interested to work on the determination of active ingredients in pharmaceutical dosage forms in the presence of interference using UV spectroscopy; therefore, it was used to determine TZ without interference of PZ.

Nanomaterial-Based Carbon Paste Electrodes for Voltammetric Determination of Naproxen in Presence of Its Degradation Products.

The present work describes a novel, simple, and fast electroanalytical methodology for naproxen (NAP) determination in pharmaceutical formulations and biological fluids in the presence of its degradation products. Carbon paste electrodes (CPEs) modified with different carbon nanomaterials, namely, glassy carbon powder (GCE), multiwall carbon nanotubes (MWCNTs), single-walled carbon nanotubes (SWCNTs), graphene nanosheets (Gr), and graphene oxides (GO) were tested. Comprehensive studies were performed on the electrode matrix composition including the nature of the pasting liquids, pH, carbon nanomaterials, and mode of electrode modification. Two anodic oxidation peaks were recorded at 0.890 and 1.18 V in 1 × 10-1 mol·L-1 phosphate buffer solution at pH 6. Oxidation of naproxen (NAP) is an irreversible diffusion-controlled process. Calibration plots were rectilinear in the concentration ranging from 0.067 to 1.0 µg·mL-1 with correlation coefficient 0.9979. Photodegradation of NAP resulted in disappearance of the oxidation peak at 1.18 V, allowing simultaneous determination of NAP in presence of its degradation product. The achieved high sensitivity and selectivity suggest the application of the proposed protocol for naproxen determination in pharmaceutical preparations and human blood plasma.

Data on validation using accuracy profile of HPLC-UV method.

The data presented are related to the article entitled "Six Sigma quality approach for HPLC-UV method optimization" Ibrahim et al., 2019. The raw data of HPLC analysis of ascorbic acid (AS), paracetamol (PA) and guaifenesin (GU) are presented. Calibration standards were prepared at six concentrations levels (25%, 50%, 75%, 100%, 125% and 150%) each day and measured in triplicate. Validation standards were prepared at four concentration levels (25%, 60%, 100% and 150%) each day and measured in quintet. Three different series were used for method validation and prepared at the rate of one series per day.

Selective and Sensitive Chromatographic Methods for Determination of a Co-Formulated Binary Mixture in Antibacterial Eye Drops and Aqueous Humor in the Presence of Their Degradation Products and Potential Impurities.

Prednisolone acetate (PDN) is a corticosteroid anti-inflammatory liable to degradation under different conditions and used with antibiotics in eye drops. Two selective stability-indicating separation techniques were developed for simultaneous determination of PDN and moxifloxacin HCl (MXF) binary mixture in pure forms, ophthalmic formulation, in the presence of PDN impurities and in the presence of their degradation products. The first method was based on HPTLC separation using silica gel 60 F254 HPTLC plates, and a developing system of toluene: ethyl acetate: methanol: ammonia (5.0: 6: 2.0: 0.05, v/v/v/v) is used with detection at 254 nm. The second method was HPLC using a mobile phase of acetonitrile: methanol: deionized water, pH 2.8 (25.0: 35.0: 40.0, v/v/v), at 254 nm. A kinetic study utilizing the developed HPLC method for PDN degradation under different stress conditions was performed. Furthermore, the method was applied for determination in rabbit aqueous humor. Validation was conducted as per ICH guidelines, and system suitability was ascertained. The calibration curves were constructed in the range 0.10-25.00 and 0.20-50.00 µg band-1, for PDN and MXF by HPTLC, while for HPLC, it was 0.02-50.00 and 0.10-50.00 µg mL-1 for both drugs, in order.

Highly Sensitive Voltammetric Sensor Using Carbon Nanotube and an Ionic Liquid Composite Electrode for Xylazine Hydrochloride.

Electrochemical techniques were used for estimating xylazine HCl (XLZ) in bulk powder, medicinal manufacturing and human serum. Electro-oxidation of XLZ at carbon multiwalled nanotube (MWCNT), 1-n-butyl-3-methylpyridinium hexafluorophosphate ion crystal (BMH) and sodium dodecyl sulfate (SDS) MWCNT-BMH-SDS electrode in 0.04 M Britton-Robinson buffer (BR) with pH 7.0, was studied in numerous buffer structures and at different pH values. The experimentation and instrumental parameters to assessable commitment of XLZ had been optimized, and a detection limit was observed as 4.80 nM. The precision and accuracy for the recognized method was tested by retrieval studies with good repeatability and reproducibility of the estimated method. The projected method was practiced successfully to the dosage form and spiked serum.

Synthesis and characterization of metals-substituted cobalt ferrite [Mx Co(1-x) Fe2O4; (M = Zn, Cu and Mn; x = 0 and 0.5)] nanoparticles as antimicrobial agents and sensors for Anagrelide determination in biological samples.

Nanocrystalline spinel ferrite nanoparticles [MxCo(1-x)Fe2O4;(M = Zn,Cu,Mn;x = 0 and 0.5)] like: Cobalt ferrite (CFO), Zinc Cobalt ferrite (ZCFO), Copper Cobalt ferrite (CCFO), and Manganese Cobalt ferrite (MCFO) modified carbon paste electrodes (CPE) were synthesized via sol-gel technique utilizing citric acid and ethylene glycol as a polymerization agent. The synthesized ferrite NPs were used as bi-functional smart biosensor, not only used to determine the drug Anagrelide-HCl (ANDH) in urine and serum samples, but also possesses antimicrobial potential against some pathogenic microbes, founded in the biological samples. The synthesized ferrite NPs were confirmed by XRD, FTIR spectroscopy, SEM, EDX, and elemental mapping images. Antimicrobial activities of ferrite NPs against selected urinary tract infected microbes were investigated. From XRD data and FTIR spectroscopy it is found that the average crystallite size is lies in the range 12.86 to 33.92 ±â€¯1.5 nm, also the bond lengths RA and RB increase from 1.8986 to 1.9145 Šand from 2.0434 to 2.0606 Šrespectively and Debye temperature θD lies in the range of 681.52-708.87 K. Our study describes the improvement of a screen-printed sensor, modified with ferrite NPs materials for rapid, sensitive and cost-effective quantification of ANDH present in the real samples such as blood serum samples, urine and in the pharmaceutical formulations. The results obtained postulate a linear regression between the ANDH charge density of peak current and its concentration in the range from (0.64-8.18 µg/ml) with DL 0.31 µg/ml and QL 0.94 µg/ml. Antimicrobial results indicated that ZCFO NPs were a novel antibacterial agent against Klebsiella pneumoniae (28.0 mm ZOI), and multidrug-resistant bacteria Enterococcus faecalis (27.0 mm ZOI). Additionally, ZCFO NPs were active against Candida albicans (18.0 mm ZOI) seems to be a smart antifungal agent. Therefore, ZCFO NPs can be used as applicant resources for industrial, medical, and biological applications.

Resolution and Quantitation of Triamcinolone Acetonide and Its Coformulated Drug in the Presence of Its Impurities and Degradation Products by HPTLC and HPLC.

Two specific, sensitive, and precise stability-indicating chromatographic methods have been developed for the determination of triamcinolone acetonide (TMC) and its coformulated drug, econazole nitrate (ECZ), in the presence of TMC impurities and degradation products. The first method was based on HPTLC-spectrodensitometry in which resolution and quantitation was achieved by using silica gel 60 F254 HPTLC plates and an ethyl acetate-tetrahydrofuran-ammonia mobile phase (10.0 + 7.0 + 0.1, v/v/v). The second method was a reversed-phase HPLC method in which separation was achieved using an acetonitrile-methanol-0.05 M potassium dihydrogen phosphate mobile phase, pH 3.0 (25.0 + 15.0 + 60.0, v/v/v). In both methods, the separated components were detected at 225 nm. Validation of both methods was conducted in compliance with International Conference on Harmonization (ICH) guidelines, and system suitability was confirmed. The linearity ranges were 0.20-28.00 and 0.50-55.00 µg/band for TMC and ECZ by HPTLC, whereas for HPLC, the range was 0.05-30.00 and 1.00-40.00 µg/mL for both drugs, respectively. The methods were successfully applied for the analysis of a pharmaceutical formulation and were compared with the reported method with no significant difference.

Zero and second-derivative synchronous fluorescence spectroscopy for the quantification of two non-classical ß-lactams in pharmaceutical vials: Application to stability studies.

The formation of metal chelates with various ligands may lead to the production of fluorescent chelates or enhance the fluorescence of the chelating agent. This paper describes two sensitive, selective and computer-solved methods, namely, zero order (SF) and second-derivative synchronous spectrofluorimetry (SDSFS) for nano-quantitation of two carbapenems; meropenem (MP) and ertapenem (EP). The methods are based on the chelation of MP with Tb3+ and EP with Zr4+ in buffered organic medium at pH 4.0 to produce fluorescent chelates. In the zero order method, the relative synchronous fluorescence intensity is measured at 327.0 nm at Δλ = 70.0 and 100.0 nm for MP and EP, respectively. The second method utilizes a second-derivative technique to enhance the method selectivity and emphasize a stability-indicating approach. The peak amplitudes (2 D) of the second-derivative synchronous spectra were estimated to be 333.06 and 330.06 nm for MP and EP, respectively. The proposed synchronous spectrofluorimetric methods were validated according to the International Conference on Harmonization (ICH) guidelines and applied successfully for the analysis of MP and EP in pure forms, pharmaceutical vials and in synthetic mixtures with different degradants of both drugs. Under optimum conditions, the mole-ratio method was applied and the co-ordination ratios of MP-Tb3+ and EP-Zr4+ chelates were found to be 1:1 and 1:3. The formation constants for the chelation complexes were evaluated using the Benesi-Hildebrand's equation; the free energy change (ΔG) was also calculated. The results indicated that EP-Zr4+ was more stable than the MP-Tb3+ chelate. Moreover, the developed methods were found to be selective and inexpensive for quantitative determination of both drugs in quality control laboratories at nano-levels.