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1.
Spectrochim Acta A Mol Biomol Spectrosc ; 313: 124115, 2024 May 15.
Article in English | MEDLINE | ID: mdl-38484641

ABSTRACT

In this study, five earth-friendly spectrophotometric methods using multivariate techniques were developed to analyze levofloxacin, linezolid, and meropenem, which are utilized in critical care units as combination therapies. These techniques were used to determine the mentioned medications in laboratory-prepared mixtures, pharmaceutical products and spiked human plasma that had not been separated before handling. These methods were named classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), genetic algorithm partial least squares (GA-PLS), and artificial neural network (ANN). The methods used a five-level, three-factor experimental design to make different concentrations of the antibiotics mentioned (based on how much of them are found in the plasma of critical care patients and their linearity ranges). The approaches used for levofloxacin, linezolid, and meropenem were in the ranges of 3-15, 8-20, and 5-25 µg/mL, respectively. Several analytical tools were used to test the proposed methods' performance. These included the root mean square error of prediction, the root mean square error of cross-validation, percentage recoveries, standard deviations, and correlation coefficients. The outcome was highly satisfactory. The study found that the root mean square errors of prediction for levofloxacin were 0.090, 0.079, 0.065, 0.027, and 0.001 for the CLS, PCR, PLS, GA-PLS, and ANN models, respectively. The corresponding values for linezolid were 0.127, 0.122, 0.108, 0.05, and 0.114, respectively. For meropenem, the values were 0.230, 0.222, 0.179, 0.097, and 0.099 for the same models, respectively. These results indicate that the developed models were highly accurate and precise. This study compared the efficiency of artificial neural networks and classical chemometric models in enhancing spectral data selectivity for quickly identifying three antimicrobials. The results from these five models were subjected to statistical analysis and compared with each other and with the previously published ones. Finally, the whiteness of the methods was assessed by the recently published white analytical chemistry (WAC) RGB 12, and the greenness of the proposed methods was assessed using AGREE, GAPI, NEMI, Raynie and Driver, and eco-scale, which showed that the suggested approaches had the least negative environmental impact. Furthermore, to demonstrate solvent sustainability, a greenness index using a spider chart methodology was employed.


Subject(s)
Anti-Bacterial Agents , Anti-Infective Agents , Humans , Linezolid , Meropenem , Levofloxacin , Spectrophotometry/methods , Critical Care , Least-Squares Analysis
2.
Arch Pharm (Weinheim) ; 357(2): e2300509, 2024 Feb.
Article in English | MEDLINE | ID: mdl-37939289

ABSTRACT

This study introduces a new method for analyzing rifampicin, moxifloxacin, and metronidazole using a green micellar High Performance Liquid Chromatography-Ultraviolet method in bulk drugs, different commercial formulations, and spiked human plasma. The combined therapy of these three broad-spectrum antibiotics is used to cure refractory hidradenitis suppurativa (HS), an inflammatory condition affecting the skin. The sustainable separation was attained on a reversed-phase C18 Kinetex® column maintained at ambient temperature in less than 5 min. The mobile phase comprises 0.1 M sodium dodecyl sulfate (SDS) in water, pH 3.5, adjusted using o-phosphoric acid, and 10% n-butanol. The flow rate was 1 mL/min, with 10 µL injection volume and UV detection at 230 nm. The impact of three key significant variables, SDS concentration, n-butanol percentage, and the mobile phase pH, on suitability parameters was studied. ICH and FDA guidelines were committed to when validating the technique. The results showed linear calibration graphs with high precision and accuracy, in both pure and spiked plasma. The method is efficient, easy to use, and has a high sample throughput, making it suitable for routine analysis in the quality control department and therapeutic monitoring. It is also evaluated as a green-and-white substitute for traditional reported methods.


Subject(s)
Hidradenitis Suppurativa , Micelles , Humans , Chromatography, High Pressure Liquid/methods , Hidradenitis Suppurativa/drug therapy , 1-Butanol , Structure-Activity Relationship
3.
Anal Methods ; 15(48): 6666-6678, 2023 12 14.
Article in English | MEDLINE | ID: mdl-38031474

ABSTRACT

It is crucial to have a reliable and sensitive method for separating common drugs used in SARS-CoV-2 pneumonia treatment protocols for ongoing treatment and upcoming investigations. This study presents an HPLC-FLD approach to analyze three co-administered medicines - remdesivir (RDV), hydroxychloroquine sulphate (HCQ), and levofloxacin hemihydrate (LVX) - in their pure forms, pharmaceutical preparations, and spiked human plasma. The HPLC-FLD analysis was conducted using a Symmetry® C18 column (100 mm × 4.6 mm ID, 3.5 µm particle size) at 40 °C, with (A) an aqueous mixture of 0.02 M phosphate buffer and 0.2% heptane-1-sulphonic acid sodium solutions (50 : 50) adjusted to pH 3, (B) acetonitrile, and (C) methanol as the mobile phase. The injection volume was 10 µL, and the flow rate was 1.5 mL min-1. The detection was done using a multi-wavelength excitation and emission fluorescence detector, with individual optimization for each drug. The drug separation time was less than 10 minutes, and the method showed sensitive and wide linearity ranges for all medicines, with r2 values of more than 0.999. The impact of the mobile phase pH and flow rate on suitability parameters (retention time and number of theoretical plates) was studied. The method was found to be environmentally friendly based on GAPI and AGREE metrics. The validity of the method was evaluated following ICH and FDA guidelines.


Subject(s)
COVID-19 , Humans , Chromatography, High Pressure Liquid/methods , SARS-CoV-2 , COVID-19 Drug Treatment , Pharmaceutical Preparations , Antiviral Agents/therapeutic use
4.
BMC Chem ; 17(1): 74, 2023 Jul 12.
Article in English | MEDLINE | ID: mdl-37438757

ABSTRACT

A novel, sensitive, and green micellar UPLC method was proposed and validated for the simultaneous determination of four hypoglycemic agents used in type II diabetes mellitus treatment namely, pioglitazone, alogliptin, glimepiride, and vildagliptin. The developed UPLC method was successfully applied for quantitative analysis of these drugs in bulk, in pharmaceutical formulations, and in spiked human plasma. Chromatographic separation was carried out on a Kinetex® 1.7 µm XB-C18 100 Å (50 × 2.1 mm) column, using a degassed and filtered mixture of (0.1 M SDS- 0.3% triethyl amine- 0.1% phosphoric acid (pH 6)) and n-propanol (85:15 v/v), at a flow rate of 0.2 mL/min. The experimental conditions of the suggested method were well investigated and optimized. The newly developed micellar UPLC method is capable of determining different dosage forms at the same time with the same solvents, saving time and effort. The method was found to be efficiently applicable in spiked human plasma and could be extended to study the pharmacokinetics of the cited drugs in real human plasma samples. The greenness of the developed method was evaluated by applying the Eco-scale scoring tool, which verified the excellent greenness of the analytical method.

5.
Spectrochim Acta A Mol Biomol Spectrosc ; 298: 122770, 2023 Oct 05.
Article in English | MEDLINE | ID: mdl-37119638

ABSTRACT

Two sensitive microbiological and charge transfer spectrophotometric methods have been developed for the quantitative determination of the antifungal drug, tioconazole, in its pure form and pharmaceutical preparations. The microbiological assay was based on the agar disk diffusion method by measuring the diameter of the inhibition zones related to different concentrations of tioconazole. The spectrophotometric method relied on charge transfer complex formation between tioconazole as an n-donor and chloranilic acid as a π-acceptor at room temperature. The formed complex was measured at λmax = 530 nm. The molar absorptivity and the formation constant of the formed complex were determined using different models, including the Benesi-Hildebrand, Foster-Hammick-Wardley, Scott, Pushkin-Varshney-Kamoonpuri, and Scatchard equations. Different thermodynamic parameters associated with the complex formation, including the free energy change (ΔG°), the standard enthalpy (ΔH°), and the standard entropy change (ΔS°), were evaluated. The two methods were validated in conformity with ICH-recommended guidelines and employed successfully for the quantification of tioconazole in both pure form and pharmaceutical formulations.


Subject(s)
Imidazoles , Spectrophotometry/methods , Thermodynamics
6.
BMC Chem ; 17(1): 20, 2023 Mar 15.
Article in English | MEDLINE | ID: mdl-36922875

ABSTRACT

BACKGROUND: Daclatasvir dihydrochloride has important roles not only in the management of COVID-19 pandemic symptoms but also in the treatment of chronic hepatitis C infection. OBJECTIVE: The current research presents four novel and simple platforms including silver-nanoparticles spectrophotometric technique and three electrochemical conductometric ones for daclatasvir analysis in its tablet, biological fluids, and dissolution media. METHODS: The spectrophotometric platform involved the synthesis of silvernanoparticles through a redox reaction between the reducing agent (daclatasvir) and the oxidizing agent (silver nitrate) in presence of polyvinylpyrrolidone as a stabilizing agent. The produced silver-nanoparticles have an intense surface plasmon resonance peak at 421 nm where the measured absorbance values were utilized for quantitative spectrophotometric determination of daclatasvir. While the electrochemical conductometric platforms involved the reaction of daclatasvir with three different precipitating reagents (silver nitrate, phosphomolybdic acid, and ammonium reineckate) to form ion associates between these reagents and daclatasvir in the aqueous system. RESULTS: All proposed platforms were validated in line with recommendations of the international conference on harmonization producing satisfactory outcomes within the agreed boundaries. CONCLUSION: The proposed platforms are green alternatives for routine rapid assay of daclatasvir at the cheapest cost because their results were observed to be nearly similar to those of the reported platform. Moreover, the suggested spectrophotometric platform's sensitivity can be employed for investigating daclatasvir bioequivalence.

7.
Spectrochim Acta A Mol Biomol Spectrosc ; 266: 120436, 2022 Feb 05.
Article in English | MEDLINE | ID: mdl-34619509

ABSTRACT

Aspirin and omeprazole combining has proven their effectiveness clinically in the treatment and prevention of cardiovascular diseases in patient with gastric diseases and gastric ulcers. Simultaneous determination of omeprazole and aspirin in their combination is a challenge due to the overlapping spectra of these drugs. Six smart and different spectrophotometric methods were developed for the analysis of omeprazole and aspirin in binary mixture and pharmaceutical dosage form. These smart methods characterized by simplicity and accuracy. The first two methods based on minimal mathematical data processing based on the zero order absorption spectra were; dual wavelength and advanced absorbance subtraction methods. The third method is first and second derivative spectrophotometric method that based on derivative spectra. The last three methods based on ratio spectra manipulation are named; ratio difference, mean centering and derivative ratio spectrophotometric methods. The linearity range of omeprazole was 2-20 µg/mL for dual wavelength method and 2-30 µg/mL for the other ones, while aspirin showed a good linearity over a range of 2.5-30 µg/mL for all methods. The correlation coefficients were greater than 0.999. The results of the developed methods are statistically compared with each other and with the results of the reported HPLC method showing no significant difference. The greenness of the developed methods was assessed using eco-scale scoring method revealing excellent greenness of the applied methods. This spectrophotometric methods is more sensitive and greener with comparing by the reported one so, these developed methods are considered eco-friendly to the environment.


Subject(s)
Omeprazole , Pharmaceutical Preparations , Aspirin , Humans , Spectrophotometry
8.
J AOAC Int ; 105(1): 309-316, 2022 Feb 04.
Article in English | MEDLINE | ID: mdl-34387326

ABSTRACT

BACKGROUND: A recent combination of aspirin (ASP) and omeprazole (OMP) has been presented in a fixed dosage form for the treatment of many cardiovascular diseases, particularly in patients with gastric diseases. However, ASP is very sensitive to degradation into salicylic acid (SAL) as its main degradation product. Hence, it is very important to develop methods for the determination of ASP and OMP in the presence of SAL. OBJECTIVE: In this study, UV spectrophotometry assisted by different univariate/multivariate post processing algorithms is presented for quantitative determination of ASP, OMP, and SAL without any prior separation. METHODS: The univariate/multivariate algorithms include double divisor ratio difference and double divisor mean centering as the univariate approaches while the multivariate methods include principal component regression (PCR) and partial least squares (PLS) models. Validation of the univariate methods was done according to International Conference on Harmonization guidelines, while the multivariate models were validated using an external validation set. RESULTS: The univariate algorithms displayed excellent regression and validation capabilities in terms of linearity, accuracy, precision, and selectivity. Regarding PCR and PLS, the number of latent variables were carefully optimized, and the model's validation criteria displayed excellent recoveries and lower errors of prediction. CONCLUSION: Our findings indicate that the developed methods were comparable to the reported chromatographic methods, but are simpler and have much shorter analysis times. HIGHLIGHTS: Overall, this report presents the first spectrophotometric methods applied for determination of possible combinations of ASP, OMP, and SAL, and poses these methods as valuable analytical tools for in-process testing and quality control analysis.


Subject(s)
Omeprazole , Salicylic Acid , Algorithms , Aspirin , Calibration , Humans , Least-Squares Analysis , Spectrophotometry
9.
Drug Dev Ind Pharm ; 47(9): 1469-1480, 2021 Sep.
Article in English | MEDLINE | ID: mdl-34727001

ABSTRACT

Miconazole nitrate (MIC) and nystatin (NYS) combination has proven its effectiveness as a prodigious therapy to cure women's common infections; vaginal candidiasis and vaginal mycosis. Herein, six smart UV-spectrophotometric platforms depending on minimal mathematical manipulation steps were first introduced for the simultaneous green analysis of MIC and NYS in their pure forms and commercial vaginal suppositories without any preliminary separation steps. These platforms included dual-wavelength, ratio difference, mean centering of ratio spectra, first derivative ratio, ratio subtraction, and absorption correction methods. All of the aforementioned platforms could estimate MIC in a linear range of 90-900 µg/ml. While NYS was computed directly by zero-order spectrophotometry at its λmax (304 nm) in a linear range of 1-15 µg/ml without any interference by MIC even in low or high concentrations. Dual-wavelength and zero-order spectrophotometric platforms were successfully applied to study the dissolution profile of MIC and NYS in their combined formulation in compliance with FDA recommendations without excipients interference. According to ICH guidelines, all platforms were validated regarding the accuracy, precision, and selectivity producing satisfactory results within the accepted limits. Also, the suggested platforms' results were statistically compared with each other and with those of the reported HPLC platform revealing no significant difference concerning accuracy and precision at p = .05. Accordingly, all proposed platforms are regarded as economic and eco-friendly alternatives to the expensive chromatographic platforms that utilize hazardous organic solvents during the analysis of cited drugs.


Subject(s)
Miconazole , Nystatin , Female , Humans , Miconazole/analysis , Solubility , Spectrophotometry/methods , Suppositories
10.
Drug Dev Ind Pharm ; 47(6): 867-877, 2021 Jun.
Article in English | MEDLINE | ID: mdl-34224277

ABSTRACT

Flumethasone pivalate (FP) and clioquinol (CL) formulation was developed as a prodigious remedy to cure the external ear inflammatory disorders. So, the current research introduces five smart and novel UV-spectrophotometric platforms relying on minimal mathematical manipulation steps for simultaneous green analysis of FP and CL with no preliminary separation in their formulation that suffered from the high difference of their ratio and severe spectral overlapping. These platforms involved dual-wavelength, first derivative ratio, Fourier self-deconvolution, area under the curve, and bivariate methods. The suggested platform' linearity was observed over the concentration range of 3-42 µg/ml for FP and 1.5-8 µg/ml for CL. All suggested platforms were validated according to ICH recommendations regarding accuracy, precision, repeatability, and selectivity producing satisfactory results within the accepted limits. These platforms were represented as rapid, green, and cheap alternatives to the reported chromatographic method due to lower solvent consumption and waste generation. Furthermore, they improved the determination sensitivity of the studied drugs and enhanced the recorded data signals or its spectral resolution by the newly introduced Fourier self-deconvoluted method. The statistical comparison between the results of the suggested platforms with each other and with those of the reported method showed no significant differences between them.


Subject(s)
Clioquinol , Flumethasone/analogs & derivatives , Spectrophotometry
11.
Spectrochim Acta A Mol Biomol Spectrosc ; 254: 119609, 2021 Jun 05.
Article in English | MEDLINE | ID: mdl-33684852

ABSTRACT

A new and simple spectrophotometric method was developed for the simultaneous determination of a new antidiabetic mixture of linagliptin and empagliflozin namely fourier self deconvulated method. The developed method based on minimal mathematical data processing on the zero order spectrum for solving sever overlapping spectra of the mentioned drugs in their pure forms and pharmaceutical dosage form. The zero order spectra of linagliptin and empagliflozin were deconvulated using Fourier transforms function. The peak amplitudes at 232 nm were selected for linagliptin and at 239 nm for empagliflozin. The constructed calibration graphs were linear over the range (5-30 µg/mL) and (2-12 µg/mL) for empagliflozin and linagliptin, respectively. The adopted method was simple, accurate, precise and validated according to the ICH guidelines.


Subject(s)
Glucosides , Linagliptin , Benzhydryl Compounds , Drug Compounding , Spectrophotometry
12.
Spectrochim Acta A Mol Biomol Spectrosc ; 248: 119258, 2021 Mar 05.
Article in English | MEDLINE | ID: mdl-33310272

ABSTRACT

Empagliflozin and linagliptin are newly approved FDA combination that used for the treatment of type 2 diabetes mellitus (T2DM) under trade name Glxambi. Two spectroflourimetric methods were developed for simple quantitative determination of empagliflozin and linagliptin in their pharmaceutical formulation and human plasma without need any tedious processing operations. Empagliflozin has a native fluorescence nature, therefore can be directly determined by measuring emission peak at 305 nm after excitation at 234 nm. There is no any interference from linagliptin at this emission wavelength. On the other hand, linagliptin is a very weak florescent compound that needs to react with fluorogenic reagent to be quantitatively determined without any reaction of empagliflozin. So, quantitative analysis of linagliptin was achieved by coupling with NBD-Cl which is an electro active halide reagent (targeting only Linagliptin with no effect on empagliflozin). Dark yellow fluorophore with high fluorescence is a result of this reaction and can be measured at emission wavelength 538 nm after excition at wavelength 469 nm. Experimental conditions of the suggested methods were well checked and optimized. The regression plots were found to be linear over the range of 40-1200 ng/mL and 3-700 ng/mL for empagliflozin and linagliptin, respectively. The obtained results by the suggested methods were statistically compared with those obtained by the reported methods, showing no significant difference with respect to accuracy and precision at p = 0.05.


Subject(s)
Diabetes Mellitus, Type 2 , Dipeptidyl-Peptidase IV Inhibitors , Benzhydryl Compounds , Diabetes Mellitus, Type 2/drug therapy , Drug Compounding , Glucosides , Humans , Hypoglycemic Agents , Linagliptin
13.
Spectrochim Acta A Mol Biomol Spectrosc ; 236: 118349, 2020 Aug 05.
Article in English | MEDLINE | ID: mdl-32305835

ABSTRACT

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.


Subject(s)
Counterfeit Drugs/analysis , Machine Learning , Prazosin/analogs & derivatives , Prazosin/analysis , Spectrophotometry, Ultraviolet/methods , Algorithms , Bayes Theorem , Green Chemistry Technology , Neural Networks, Computer , Spectrophotometry, Ultraviolet/statistics & numerical data , Tablets/analysis
14.
Spectrochim Acta A Mol Biomol Spectrosc ; 230: 118083, 2020 Apr 05.
Article in English | MEDLINE | ID: mdl-32004869

ABSTRACT

Five simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of Nebivolol hydrochloride (NEB) and Valsartan (VAL) in their binary mixtures and in pharmaceutical dosage form. The methods included Ratio Difference, First Derivative ratio, Mean Centering of ratio spectra, Bivariate and H-Point Standard additions method. The calibration curves were linear over the concentration range of 10-70 µg/ml and 20-60 µg/ml for NEB and VAL, respectively for Ratio Difference and First Derivative ratio method and over the concentration range of 10-70 µg/ml and 10-60 µg/ml for NEB and VAL, respectively for Mean Centering of ratio spectra, Bivariate and H-Point Standard additions method. These methods were examined by analyzing synthetic mixtures of the studied drugs and they were utilized to determine the studied drugs in their commercial pharmaceutical preparation. All methods were validated as per ICH guidelines and accuracy, robustness, repeatability and precision were found to be within the acceptable limits. The results of the proposed methods were compared to the results of reported methods with no significant difference between them.


Subject(s)
Nebivolol/analysis , Pharmaceutical Preparations/analysis , Pharmaceutical Preparations/chemistry , Spectrophotometry/methods , Valsartan/analysis , Calibration , Reproducibility of Results
15.
Spectrochim Acta A Mol Biomol Spectrosc ; 213: 288-300, 2019 Apr 15.
Article in English | MEDLINE | ID: mdl-30708286

ABSTRACT

Novel univariate and multivariate factor-based calibration-prediction techniques were validated for simultaneous ultraviolet spectrophotometric determination of ribavirin (RIV), daclatasvir (DAV), sofosbuvir (SOV), and sorafenib (SON) which are co-administered for treatment of hepatocellular carcinoma (HCC) that results from Hepatitis C-virus (HCV) infection in their commercial products and in biological fluids. Determination of these compounds is essential owing to their pharmacotherapeutic benefits. Due to spectral overlapping of RIV, DAV, SOV, and SON, univariate extended derivative ratio (EDR) method and multivariate partial least-squares (PLS) and principal component regression (PCR) methods were used for constructing the calibration curves. The extended derivative ratio (EDR) absorption maxima at 215 nm and minima at 310.5 nm was used for determination of RIV and DAV, respectively and absorption maxima at 240.3 nm and minima at 284.5 nm for determination of SOV and SON, respectively. The linearity was established over the range of 6-42 µg mL-1, 4-16 µg mL-1, 10-70 µg mL-1, and 3-9 µg mL-1 for RIV, DAV, SOV and SON with correlation coefficient (r2) of 0.9997, 0.9997, 0.9999 and 0.9997, respectively. This method was effectively applied to pure, pharmaceutical preparations and to spiked human urine and plasma. PLS and PCR models were established for the determination of the studied drugs in the range of 6-42, 4-16, 10-70 and 3-9 µg mL-1 for RIV, DAV, SOV, and SON, respectively. Furthermore, updating the PLS model (PLS model update) were allowed for the determination of these drugs in spiked human urine, plasma and drug-dissolution test of their tablets. The obtained results were compared to official and reported method showing that there were no significant differences. The results of applying PLS and PCR models for evaluation of RIV, DAV, SOV, and SON in human urine samples as real samples were also encouraging. It is expected that the suitable features of the proposed method make it helpful for biological and clinical applications.


Subject(s)
Antiviral Agents/blood , Antiviral Agents/urine , Carcinoma, Hepatocellular/drug therapy , Hepacivirus/physiology , Liver Neoplasms/drug therapy , Spectrophotometry/methods , Antiviral Agents/chemistry , Calibration , Humans , Least-Squares Analysis , Limit of Detection , Multivariate Analysis , Principal Component Analysis , Reproducibility of Results , Tablets
16.
Spectrochim Acta A Mol Biomol Spectrosc ; 202: 159-173, 2018 Sep 05.
Article in English | MEDLINE | ID: mdl-29783148

ABSTRACT

In accordance with International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH) guidelines, six novel, simple and precise sequential spectrophotometric methods were developed and validated for the simultaneous analysis of Ribavirin (RIB), Sofosbuvir (SOF), and Daclatasvir (DAC) in their mixture without prior separation steps. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. These techniques consisted of several sequential steps using zero, ratio and/or derivative spectra. DAC was first determined through direct spectrophotometry at 313.7 nm without any interference of the other two drugs while RIB and SOF can be determined after ratio subtraction through five methods; Ratio difference spectrophotometric method, successive derivative ratio method, constant center, isoabsorptive method at 238.8 nm, and mean centering of the ratio spectra (MCR) at 224 nm and 258 nm for RIB and SOF, respectively. The calibration curve is linear over the concentration ranges of (6-42), (10-70) and (4-16) µg/mL for RIB, SOF, and DAC, respectively. This method was successfully applied to commercial pharmaceutical preparation of the drugs, spiked human urine, and spiked human plasma. The above methods are very simple methods that were developed for the simultaneous determination of binary and ternary mixtures and so enhance signal-to-noise ratio. The method has been successfully applied to the simultaneous analysis of RIB, SOF, and DAC in laboratory prepared mixtures. The obtained results are statistically compared with those obtained by the official or reported methods, showing no significant difference with respect to accuracy and precision at p = 0.05.


Subject(s)
Imidazoles/blood , Imidazoles/urine , Ribavirin/blood , Ribavirin/urine , Sofosbuvir/blood , Sofosbuvir/urine , Spectrophotometry/methods , Carbamates , Humans , Imidazoles/chemistry , Limit of Detection , Pharmaceutical Preparations , Pyrrolidines , Reproducibility of Results , Ribavirin/chemistry , Sofosbuvir/chemistry , Solubility , Valine/analogs & derivatives
17.
Spectrochim Acta A Mol Biomol Spectrosc ; 202: 401-409, 2018 Sep 05.
Article in English | MEDLINE | ID: mdl-29807338

ABSTRACT

Charge-transfer complex (CTC) formation between tioconazole (TCZ) as an n-electron donor and 7, 7, 8, 8-tetracyanoquinodimethane (TCNQ) as a π-acceptor was studied spectrophotometrically with an accompanying kinetic and thermodynamic investigation. Multivariate data analysis via a set of experimental designs was executed for this purpose. A 23 - two-level full factorial design (FFD) was used for inspecting the proposed variables while a face-centered central composite design (FCCCD) was used to adjust the levels of variables proved to be significant. Two responses were quantified as a result of this interaction; complex I (Y1, measured at 743 nm) and complex II (Y2, measured at 842 nm). Derringer's function and overlaid contour plots were used to concurrently optimize both responses. Benesi-Hildebrand equation was applied to determine of formation constant (K), and the molar absorptivity (Ɛ) of the formed complex. Different thermodynamic parameters; the standard Gibbs free energy change (∆G°), the standard enthalpy of formation (∆H°) and the standard entropy change (∆S°) were determined for the reaction product. The proposed method was validated regarding the linearity, intra-, and inter-day precision and accuracy, limit of detection, limit of quantification and following the ICH standards. The proposed method was also applied for the determination of TCZ in its pharmaceutical preparations. Having a higher molar absorptivity and higher formation constant, complex II was of choice for all subsequent measurements. Application of Benesi-Hildebrand equation supported the formation of 1: 1 CTC. Thermodynamic study revealed the endothermic characters and the spontaneity of formation of the CTC at high temperature.


Subject(s)
Imidazoles/chemistry , Nitriles/chemistry , Kinetics , Limit of Detection , Multivariate Analysis , Thermodynamics , Time Factors
18.
Article in English | MEDLINE | ID: mdl-29660665

ABSTRACT

Simultaneous determination of sofosbuvir (SOF), and daclatasvir (DAC) in their dosage forms, human urine and human plasma using simple and rapid micellar high performance liquid chromatographic method coupled with UV detection (HPLC-UV) had been developed and validated. These drugs are described as co-administered for treatment of Hepatitis C virus (HCV). HCV is the cause of Hepatitis C and some cancers such as liver cancer (hepatocellular carcinoma) and lymphomas in humans. Separation and quantitation were carried out on anonyx™ C8 monolithic (100 × 4.6 mm (i.d.) analytical column maintained at 25 °C. The mobile phase consisted of 0.1 M sodium dodecyl sulfate (SDS) solution containing 20% (V/V) n-propanolol and 0.3% (V/V) triethylamine and pH was adjusted to 6.5 using 0.02 M phosphoric acid, respectively. The retention times of SOF and DAC were 4.8 min, and 6.5 min, respectively. Measurements were made at flow rate of 0.5 mL/min with injection volume of 20 µL and ultraviolet (UV) detection at 226 nm. Linearity of SOF and DAC was obtained over concentration ranges of 50-400, and 40-400 ng/mL, respectively in pure form, 60-300 and 50-300 ng/mL, respectively for human plasma and over 50-400, and 40-400 ng/mL, respectively for human urine with correlation coefficient >0.999. The proposed method demonstrated excellent intra- and inter-day precision and accuracy. The suggested method was applied for determination of the drugs in pure, dosage form, and in real human plasma, real human urine and drug-dissolution test of their tablets. The obtained results have been statistically compared to reported method to give a conclusion that there is no significant differences.


Subject(s)
Antiviral Agents/analysis , Chromatography, High Pressure Liquid/methods , Imidazoles/analysis , Sofosbuvir/analysis , Adult , Antiviral Agents/chemistry , Antiviral Agents/pharmacokinetics , Carbamates , Female , Hepacivirus , Humans , Imidazoles/chemistry , Imidazoles/pharmacokinetics , Limit of Detection , Linear Models , Male , Micelles , Pyrrolidines , Reproducibility of Results , Sofosbuvir/chemistry , Sofosbuvir/pharmacokinetics , Spectrophotometry, Ultraviolet , Valine/analogs & derivatives
19.
Luminescence ; 33(2): 326-335, 2018 Mar.
Article in English | MEDLINE | ID: mdl-29124884

ABSTRACT

An easy, quick, simple and accurate spectrofluorimetric method was recognized and validated for evaluation of sorafenib (SOR) in pure form and biologically in plasma. Cremophor RH 40 (Cr RH 40) used for enhancing the fluorescence activity of SOR in phosphate buffer (pH 7). Cr RH 40 improved the native fluorescence of SOR remarkably in water. The fluorescence spectrum of SOR was observed at 405 nm after excitation at 265 nm. The linearity appeared to be in the range of 5 to 600 ng ml-1 for pure and from 9 to 500 ng ml-1 for plasma using the protein precipitation (ppt) method while from 10 to 500 ng ml-1 for plasma using liquid-liquid extraction method. The precisions and the accuracy of the estimated method gave satisfactory results. The recommended method was effectively applied for determination of SOR in human plasma with high recovery values. The results of some compounds that are possibly found in plasma were studied. The proposed method was also focused on real volunteers and a drug dissolution test.


Subject(s)
Antineoplastic Agents/blood , Niacinamide/analogs & derivatives , Phenylurea Compounds/blood , Polyethylene Glycols/chemistry , Spectrometry, Fluorescence/methods , Antineoplastic Agents/chemistry , Fluorescence , Humans , Limit of Detection , Niacinamide/blood , Niacinamide/chemistry , Phenylurea Compounds/chemistry , Sorafenib , Spectrometry, Fluorescence/instrumentation
20.
Luminescence ; 33(1): 232-242, 2018 Feb.
Article in English | MEDLINE | ID: mdl-29094459

ABSTRACT

The following paper represents a simple, highly sensitive, responsive validated and developed spectrofluorimetric method for estimation of imatinib (IMB) in its pure, commercial preparation, human urine and human blood plasma. The calibration curve was in the range 4-900 ng ml-1 for pure form and urine and 8-900 ng ml-1 for plasma in a medium contains carboxymethyl cellulose (CMC) and acetate buffer (pH 5) with excitation wavelength (λex ) 230 nm and emission wavelength (λem ) 307 nm. The limit of detection (LOD) was 0.37 ng ml-1 for the pure form, 0.64 ng ml-1 for human urine, and 0.70 ng ml-1 for human plasma, while the limit of quantitation (LOQ) was 1.2 for pure form, 1.91 for urine and 2.1 for plasma. The suggested method was successfully applied for evaluation of IMB in tablets within 99% mean percentage recovery. The excipients that are usually used as additives in pharmaceutical dosage form did not interfere with the suggested method. The method was efficiently used for estimation of IMB in human urine and human plasma. The effect of some cations that might be present in urine and plasma was also studied. The method was also focused on human volunteers and in vitro drug release.


Subject(s)
Imatinib Mesylate/analysis , Pharmaceutical Preparations/analysis , Spectrometry, Fluorescence/methods , Humans , Molecular Structure
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