Micelle-Enhanced conventional and synchronous spectrofluorimetric methods for the simultaneous determination of lesinurad and febuxostat: Application to human plasma

Magdy, Galal; Belal, Fathalla; Abdel‐Megied, Ahmed M.; Hakiem, Ahmed Faried Abdel

doi:10.1016/j.saa.2020.119239

Cited by 28 publications

(18 citation statements)

References 38 publications

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“…From the literature survey, few methods were reported for LES analysis either alone or in combination with other drugs. The reported methods involve LC-MS/MS [10,11], HPLC-UV detection [12,13], CZE [14], and spectrofluorimetry [15,16]. Concerning FEB, a number of HPLC methods had been reported using photo diode array [8,17], fluorescence [18,19], and mass detection [20][21][22].…”

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confidence: 99%

“…Concerning FEB, a number of HPLC methods had been reported using photo diode array [8,17], fluorescence [18,19], and mass detection [20][21][22]. It was also investigated by high-performance TLC [23,24], GC [25], MEKC [26], and spectrofluorimetric methods [15,27]. Different methods were also reported for DIF analysis including HPLC [28][29][30], CE [31], high-performance TLC [32], GC [33], and spectrofluorimetric methods [9,30].…”

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confidence: 99%

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A novel quality by design approach for development and validation of a green reversed‐phase HPLC method with fluorescence detection for the simultaneous determination of lesinurad, febuxostat, and diflunisal: Application to human plasma

Magdy

Hakiem

Belal

et al. 2021

J of Separation Science

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A novel and eco‐friendly reversed‐phase HPLC method with fluorescence detection was developed for simultaneous estimation of two co‐administered antigout drugs (lesinurad and febuxostat) with diflunisal as a nonsteroidal anti‐inflammatory drug. Unlike routine methodology, the developed method was optimized using analytical quality by design approach. A full factorial design was applied to optimize the effect of variable factors on chromatographic responses. The chromatographic separation was performed using isocratic elution on the Hypersil BDS C18 column at 40°C. The mobile phase consisted of acetonitrile:potassium phosphate buffer (30.0 mM; pH 5.5, 32.2:67.8% v/v) pumped at a flow rate of 1.0 mL/min and injection volume of 20.0 μL was employed. The proposed method was able to separate the ternary mixture in <10 min. The calibration curves of diflunisal, lesinurad, and febuxostat were linear over concentration ranges of 50.0–500.0, 50.0–700.0, and 20.0–700.0 ng/mL, respectively. Recovery percentages ranging from 98.1 to 101.3% with % relative standard deviation of <2% were obtained upon spiking to human plasma samples, indicating high bioanalytical applicability. Furthermore, the method was found to be excellent green when it was assessed according to Green Analytical Procedure Index and analytical Eco‐Scale guidelines.

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A novel quality by design approach for development and validation of a green reversed‐phase HPLC method with fluorescence detection for the simultaneous determination of lesinurad, febuxostat, and diflunisal: Application to human plasma

Magdy

Hakiem

Belal

et al. 2021

J of Separation Science

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“…The value of Δλ has a significant impact on the synchronous fluorescence properties regarding sensitivity and resolution. It has a significant impact on the spectral pattern, signal's value, and synchronous band width 47 , 48 . PHL and EPH SF spectra were examined at a wide Δλ scale (20–140 nm).…”

Section: Resultsmentioning

confidence: 99%

Determination of pholcodine alone or in combination with ephedrine in human plasma using fluorescence spectroscopy

Elmansi

Belal

Magdy

2022

Sci Rep

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In this study, sensitive, facile, and cost-effective spectrofluorimetric approaches were developed for the determination of pholcodine and ephedrine. Method I is a novel spectrofluorimetric method depending on measuring the native fluorescence of pholcodine at 337 nm after excitation at 284 nm over a concentration range of 0.01–2.4 μg/mL. The method sensitivity reached quantitation and detection limits down to 10.0 and 5.0 ng/mL, respectively. Method II relied on the simultaneous estimation of pholcodine and ephedrine using synchronous fluorimetry for the first time. The cited drugs were measured concurrently at 286 and 304 nm for pholcodine and ephedrine, respectively at Δλ of 40 nm without interference. Excellent linear relationship between concentration and response was obtained over the ranges of 0.05–6.0 μg/mL and 0.02–1.0 μg/mL for pholcodine and ephedrine, respectively. The method showed distinct sensitivity and exhibited quantitation limits of 20.0 and 10.0 ng/mL and detection limits of 10.0 and 5.0 ng/mL, respectively. The method was successfully applied to the syrup dosage form. The two developed approaches were also applied to in-vitro plasma samples, showing good bioanalytical applicability and providing further insights for monitoring drug abuse. The proposed methods were validated according to ICHQ2(R1) guidelines. The proposed methodologies' greenness profiles were evaluated using two greenness assessment tools.

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“…From the literature survey, the analysis of FEB was performed using different methods including spectrofluorimetry [10][11][12][13], spectrophotometry [14,15], HPLC [9,[16][17][18][19], LC-MS [20][21][22], micellar electrokinetic capillary chromatography [23], HPTLC [24][25][26][27] and GC [28]. Similarly, the assay of IBU has been achieved applying different methods including spectrofluorimetry [29][30][31][32], spectrophotometry [33,34], HPLC [35][36][37], LC-MS [38,39], HPTLC [37], capillary zone electrophoresis [40,41], potentiometry [42] and GC [43,44].…”

Section: Introductionmentioning

confidence: 99%

“…Data accessibility. Data are available at the Dryad Digital Repository: https://doi.org/10.5061/dryad.r4xgxd2bv[61]. Authors' contributions.…”

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Two different synchronous spectrofluorimetric approaches for simultaneous determination of febuxostat and ibuprofen

et al. 2021

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Two green, simple and sensitive synchronous spectrofluorimetric methods were developed for the first time for the simultaneous estimation of febuxostat (FEB) and ibuprofen (IBU). Method I is constant-wavelength synchronous spectrofluorimetry where FEB and IBU were recorded at 329 and 258 nm, respectively, using Δ λ of 40 nm. Method II is constant-energy synchronous spectrofluorimetry using a wavenumber interval of −4000 cm −1 . All measurements were carried out in a borate buffer of pH 7 and distilled water for dilution which increased the methods' greenness. The two methods were rectilinear over concentration ranges of 30.0–700.0 ng ml −1 and 0.5–9.0 µg ml −1 in the first method and 20.0–500.0 ng ml −1 and 0.1–8.0 µg ml −1 in the second method for FEB and IBU, respectively. High sensitivity was attained for the two drugs with limits of quantitations (LODs) down to 0.41 and 5.51 ng ml −1 in the first method and 0.25 and 3.32 ng ml −1 in the second method for FEB and IBU, respectively. Recovery percentages were in the range of 97.3–101.9% after extraction from spiked human plasma samples, demonstrating high bioanalytical applicability. The two methods were further applied to tablet dosage forms with good recovery results. The methods' greenness was assessed according to the analytical Eco-Scale and Green Analytical Procedure Index guidelines.

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Micelle-Enhanced conventional and synchronous spectrofluorimetric methods for the simultaneous determination of lesinurad and febuxostat: Application to human plasma

Cited by 28 publications

References 38 publications

A novel quality by design approach for development and validation of a green reversed‐phase HPLC method with fluorescence detection for the simultaneous determination of lesinurad, febuxostat, and diflunisal: Application to human plasma

A novel quality by design approach for development and validation of a green reversed‐phase HPLC method with fluorescence detection for the simultaneous determination of lesinurad, febuxostat, and diflunisal: Application to human plasma

Determination of pholcodine alone or in combination with ephedrine in human plasma using fluorescence spectroscopy

Two different synchronous spectrofluorimetric approaches for simultaneous determination of febuxostat and ibuprofen

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