Simultaneous determination of elbasvir and grazoprevir in their pharmaceutical formulation by synchronous fluorescence spectroscopy coupled to dual wavelength method.
05 Mar 2021-Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy (Elsevier)-Vol. 248, pp 119157-119157
TL;DR: A sensitive, selective and accurate synchronous fluorescence spectroscopic method was utilized for simultaneous estimation of elbasvir and grazoprevir in their pharmaceutical formulation and was successfully applied to the quantitative analysis of the two drugs in Zepatier® tablets.
About: This article is published in Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy.The article was published on 2021-03-05. It has received 13 citations till now. The article focuses on the topics: Elbasvir & Grazoprevir.
Citations
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TL;DR: In this paper, two different high precision sensitive fluorescence spectroscopic methods were developed for quantitative analysis of the above drugs in pharmaceutical dosage form and spiked human plasma, and the proposed methods were successfully applied to the quantification of the two drugs in the pharmaceutical dosage-form Yosprala ® and in spiked human plasmate.
10 citations
TL;DR: In this paper, Artificial Neural Networks and GANs were used for the quantitative analysis of elbasvir and grazoprevir in their newly FDA approved pharmaceutical dosage form, and the results were statistically compared with another reported HPLC quantitative analytical method with no significant difference by applying Student t-test and variance ratio F-test.
8 citations
TL;DR: In this paper , an integrated green computational spectrophotometric method was developed for the determination of molnupiravir, which is an oral antiviral drug developed to provide significant benefit in reducing hospitalizations or deaths in mild COVID-19.
8 citations
TL;DR: In this article , a sensitive synchronous fluorescence spectroscopic method was applied in conjunction with first derivative for quantitative estimation of fexofenadine hydrochloride and pseudoephedrine hydrochlorides in pure form, pharmaceutical tablets and spiked human plasma.
Abstract: Fexofenadine hydrochloride and pseudoephedrine hydrochloride are prescribed in a combined dosage form for the treatment of allergic rhinitis. In the present work, a sensitive synchronous fluorescence spectroscopic method was applied in conjunction with first derivative for quantitative estimation of fexofenadine hydrochloride and pseudoephedrine hydrochloride in pure form, pharmaceutical tablets and spiked human plasma. Fexofenadine hydrochloride showed its conventional emission spectrum at 294 nm when excited at 267 nm. On the other hand, pseudoephedrine hydrochloride showed its conventional emission spectra at 286 nm when excited at 261 nm. The fluorescence intensities were greatly enhanced by the use of sodium dodecyl sulphate as a micellar surfactant. Application of the synchronous mode to measure the fluorescence spectra of the above drugs provided sharp narrowing bands, but the overlap was not completely resolved. Derivatization of the synchronous spectra to the first order completely resolved the overlap of the fluorescence spectra and allowed simultaneous quantitative determination of the drugs under study. Fexofenadine hydrochloride and pseudoephedrine hydrochloride could be determined from their first-order synchronous spectra at 286 and 294 nm, respectively, without interfering with each other. The method showed linearity with an excellent correlation coefficient in the concentration range of 100-1500 ng/mL for Fexofenadine hydrochloride and 50-1000 ng/mL for pseudoephedrine hydrochloride. The method was successfully applied for the simultaneous determination of the studied drugs in pharmaceutical formulation, with mean percent recoveries for Fexofenadine hydrochloride and pseudoephedrine hydrochloride of 99.49 ± 0.931 and 98.67 ± 0.634, respectively, and in spiked human plasma, with mean percent recoveries for Fexofenadine hydrochloride and pseudoephedrine hydrochloride of 95.21 ± 1.938 and 94.89 ± 1.763, respectively. Furthermore, the greenness of the described method was assessed using four different tools namely, the national environmental method index, the analytical eco-scale, the green analytical procedure index and the AGREE evaluation method. The proposed method seemed to be superior to the reported HPLC method with respect to the metrics of the greenness characters.
7 citations
TL;DR: A simple synchronous spectrofluorimetric approach was established that was validated according to International Conference on Harmonization guidelines and further applied to commercial pharmaceutical preparations with good results, allowing a significant bioanalytical application.
Abstract: Abstract Coronavirus disease 2019 (COVID‐19) is a contagious viral infection caused by coronavirus 2 (SARS‐CoV‐2) that causes severe acute respiratory syndrome. It has ravaged several countries and burdened many healthcare systems. As the process of authorizing a novel treatment for human use is extensive and involves multiple phases to obtain safety information and identify potential concerns. Therefore, the fastest and easiest choice was to use United States Food and Drug Administration (US FDA)‐approved drugs such as favipiravir and hydroxychloroquine. For the simultaneous estimation of both medications, a simple synchronous spectrofluorimetric approach was established in which both drugs were measured at 372 and 323 nm, respectively in the presence of each other without interference at Δλ 60 nm. The effect of various experimental conditions on synchronous fluorescence intensities were thoroughly investigated and optimized. The maximum synchronous fluorescence intensities were obtained at pH 5.4 using acetate buffer (0.2 M, 0.5 ml) and ethanol as a diluent. Excellent linearity ranges were obtained using 1.0–18.0 ng/ml and 10.0–120.0 ng/ml for favipiravir and hydroxychloroquine, respectively. The approach exhibited high sensitivity with detection limits down to 0.25 ng/ml and 1.52 ng/ml and quantitation limits down to 0.77 ng/ml and 4.62 ng/ml, respectively. Spiking human plasma samples with the studied drugs yielded high % recoveries, allowing a significant bioanalytical application. Moreover, the method was validated according to International Conference on Harmonization guidelines and further applied to commercial pharmaceutical preparations with good results.
7 citations
References
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01 Apr 2005
TL;DR: In this article, the authors present a set of confidence limits of the geometric mean for a log-normal distribution for a given value and the confidence limits for a large sample for a small sample.
Abstract: 1 Introduction 11 Analytical problems 12 Errors in qunatitative analysis 13 Types of error 14 Random and systematic errors in titrimetric analysis 15 Handling systematic errors 16 Planning and design of experiments 17 Calculators and computers in statistical calculations 2 Statistics of Repeated Measurements 21 Mean and standard deviation 22 The distribution of repeated measurements 23 Log-normal distribution 24 Definition of a 'sample' 25 The sampling distribution of the mean 26 Confidence limits of the mean for large samples 27 Confidence limits of the mean for small samples 28 Presentation of results 29 Other uses of confidence limits 210 Confidence limits of the geometric mean for a log-normal distribution 211 Propagation of random errors 212 Propagation of systematic errors 3 Significance Tests 31 Introduction 32 Comparison of an experimental mean with a known value 33 Comparison of two experimental means 34 Paired t-test 35 One-sided and two-sided tests 36 F-test for the comparison of standard deviations 37 Outliers 38 Analysis of variance 39 Comparison of several means 310 The arithmetic of ANOVA calculations 311 The chi-squared test 312 Testing for normality of distribution 313 Conclusions from significance tests 314 Bayesian Statistics 4 The Quality of Analytical Measurements 41 Introduction 42 Sampling 43 Separation and estimation of variances using ANOVA 44 Sampling strategy 45 Quality control methods - Introduction 46 Stewhart charts for mean values 47 Stewhart charts for ranges 48 Establishing the process capability 49 Average run length: cusum charts 410 Zone control charts (J-charts) 411 Proficiency testing schemes 412 Method performance studies (collaborative trials) 413 Uncertainty 414 Acceptable sampling 415 Method validation 5 Calibration Methods in Instumental Analysis 51 Introduction: instrumentational analysis 52 Calibration graphs in instrumental analysis 53 The product-moment correlation coefficient 54 The line of regression of y on x 55 Errors in the slope and intercept of the regression line 56 Calculation of a concentration and its random error 57 Limits of detection 58 The method of standard additions 59 Use of regression lines for comparing analytical methods 510 Weighted regression lines 511 Intersection of two straight lines 512 ANOVA and regression calculations 513 Curvilinear regression methods - Introduction 514 Curve fitting 515 Outliers in regression 6 Non-parametric and Robust Methods 61 Introduction 62 The median: initial data analysis 63 The sign test 64 The Wald-Wolfowitz runs test 65 The Wilcoxon signed rank test 66 Simple tests for two independent samples 67 Non-parametric tests for more than two samples 68 Rank correlation 69 Non-parametric regression methods 610 Robust methods: introduction 611 Simple robust methods: trimming and winsorization 612 Further robust estimates of location and spread 613 Robust ANOVA 614 Robust regression methods 615 Re-sampling statistics 616 Conclusions 7 Experiimental Design and Optimization 71 Introduction 72 Randomization and blocking 73 Two-way ANOVA 74 Latin squares and other designs 75 Interactions 76 Identifying the important factors: factorial designs 77 Fractional factorial designs 78 Optimization: basic principles and univariate methods 79 Optimization using the alternating variable search method 710 The method of steepest ascent 711 Simplex optimization 712 Simulated annealing 8 Multivariate Analysis 81 Introduction 82 Initial analysis 83 Prinicipal component analysis 84 Cluster analysis 85 Discriminant analysis 86 K-nearest neighbour method 87 Disjoint class modelling 88 Regression methods 89 Multiple linear regression 810 Principal component regression 811 Partial least squares regression 812 Natural computation methods artificial neural networks 813 Conclusions Solutions to Exercises Appendix 1 Commonly used statistical significance tests Appendix 2 Statistical tables Index
3,668 citations
TL;DR: A review of synchronous fluorescence scan (SFS) methods for analysis of multi-component systems can be found in this paper, where the authors discuss the use of SFS in the analysis of complex multichannel mixtures.
Abstract: The ability to analyse complex multi-component mixtures without resorting to tedious separation procedures is extremely useful for routine analysis. Single-wavelength fluorescence measurement is limited in its ability to analyse complicated multi-component samples when they have severely overlapping emission and/or excitation spectra. This can be overcome by using synchronous fluorescence scan (SFS), where overlapping of spectra can be minimized. The selectivity of SFS can still be increased by taking derivative spectrum, applying different multivariate methods, selective fluorescence quenching, three-dimensional synchronous measurement or using some of these procedures in combination. Recent developments in various synchronous fluorescence methods for analysis of multi-component systems are discussed in this review.
277 citations
TL;DR: The high sensitivity attained by the synchronous fluorometric method allowed the determination of cinnarizine in real and spiked human plasma and the results obtained were in good agreement with those obtained with reference methods.
Abstract: A rapid, simple and highly sensitive second derivative synchronous fluorometric method has been developed for the simultaneous analysis of binary mixture of cinnarizine (CN) and domperidone (DOM). The method is based upon measurement of the native fluorescence of these drugs at Δλ = 80 nm in aqueous methanol (50% V/V). The different experimental parameters affecting the native fluorescence of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.1 to 1.3 μg mL−1 and 0.1–3.0 μg mL−1 for CN and DOM, respectively with lower detection limits of 0.017 and 5.77 × 10−3 μg mL−1 and quantification limits of 0.058 and 0.02 μg mL−1 for CN and DOM. The proposed method was successfully applied for the determination of the studied compounds in synthetic mixtures and in commercial tablets. The results obtained were in good agreement with those obtained with reference methods. The high sensitivity attained by the synchronous fluorometric method allowed the determination of CN in real and spiked human plasma. The mean % recoveries in case of spiked human plasma (n = 3) were 96.39 ± 1.18 while that in real human plasma (n = 3) was 104.67 ± 4.16.
45 citations
TL;DR: A novel, fast, simple, ultrasensitive and cost‐effective spectrofluorimetric method designed for determination of DCS and LDS in miscellaneous matrices was designed and validated in compliance with ICH guidelines and US‐FDA guidelines.
33 citations
TL;DR: The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form and there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.
29 citations