Development of a validated liquid chromatographic method for the determination of related substances and assay of tenofovir disoproxil fumarate

Ashenafi, Dunge; Chintam, Varalaxmi; Veghel, Daisy van; Dragović, Sanja; Hoogmartens, Jos; Adams, Erwin

doi:10.1002/jssc.201000039

Cited by 18 publications

(17 citation statements)

References 7 publications

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“…Only one method made use of ultraviolet (UV) for detection of TEN at 259 nm [15]. Other HPLC methods are applied for assay of TEN in bulk powder and in pharmaceutical preparations [20][21][22].…”

Section: Fig 1 Structures Of Tenofovir Disproxyl Fumarate (Ten) Andmentioning

confidence: 99%

Selective RP-HPLC DAD method for determination of tenofovir fumarate and emtricitabine in bulk powder and in tablets

Abdelhay¹,

Gazy²,

Shaalan³

et al. 2015

Acta Chromatographica

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Summary.A simple and selective liquid chromatographic method was developed for the simultaneous determination of tenofovir disoproxil fumarate (TEN) and emtricitabine (EMT) in combined tablets. The method is based on separation of TEN and EMT on a Zorbax SB-C8 column, 5 μm, 4.6 × 250 mm, with a mobile phase consisting of 50 mM disodium hydrogen phosphate-acetonitrile (50:50, v/v). The mobile phase contains 0.1% triethylamine (TEA) and was adjusted to pH 6.0. Quantification of the analytes is achieved with diode array -ultraviolet detector (DAD-UV) at 260 and 280 nm for TEN and EMT, respectively, based on peak area. Different variables affecting the method were carefully investigated and optimized. Reliability and analytical performance of the proposed method, including linearity, range, precision, accuracy, and detection and quantitation limits, were statistically validated. The high-performance liquid chromatography (HPLC) method was successfully applied for determination of each drug in their binary tablets.

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Section: Fig 1 Structures Of Tenofovir Disproxyl Fumarate (Ten) Andmentioning

confidence: 99%

Selective RP-HPLC DAD method for determination of tenofovir fumarate and emtricitabine in bulk powder and in tablets

Abdelhay¹,

Gazy²,

Shaalan³

et al. 2015

Acta Chromatographica

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“…A study was carried out to test the effect of the divisor concentration (EMT) on the obtained calibration curves, hence the absorption spectra of standard solutions of TEN in the concentration range stated in Table 1 were divided by the corresponding amplitudes of standard solutions of EMT (10,15,20, and 40 g mL −1 ). The resultant ratio spectra were then differentiated.…”

Section: Optimization Of the Derivative Ratio Spectrophotometricmentioning

confidence: 99%

“…Only one method made use of UV for detection of TEN at 259 nm [15]. Other HPLC methods are applied for assay of TEN in bulk powder and in pharmaceutical preparations [20][21][22].…”

Section: Introductionmentioning

confidence: 99%

Simple Spectrophotometric Methods for Determination of Tenofovir Fumarate and Emtricitabine in Bulk Powder and in Tablets

Abdelhay

Gazy

Shaalan

et al. 2013

Journal of Spectroscopy

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Two simple and selective methods were developed for the simultaneous determination of tenofovir fumarate (TEN) and emtricitabine (EMT) in combined tablets. The first method involves the application of first derivative spectrophotometry where the first derivative amplitudes were measured at 298.5 nm for determination of EMT in presence of TEN. The second method involves first derivative of ratio spectra spectrophotometry where the amplitudes at 251.5 nm have been used for quantitation of TEN in the presence of EMT. Different variables affecting each method were carefully investigated and optimized. Reliability and analytical performance of the proposed methods, including linearity, range, precision, accuracy, detection, and quantitation limits, were statistically validated. The methods were successfully applied for the determination of EMT and TEN in laboratory-prepared mixtures and in their combined tablets.

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“…The literature search revealed that there are number of analytical methods have been reported for single molecule or simultaneous estimation of TDF and FTC by HPLC [5][6][7][8][9][10][11][12] , by UPLC [13][14][15][16] , by mass spectroscopy 17 . Till date no stability indicating HPLC method has been reported for simultaneous estimation of related substances of TDF and FTC by QbD life cycle approach.…”

Section: Introductionmentioning

confidence: 99%

Application of QBD Life Cycle Approach for Stability Indicating HPLC Method Development and Validation for the Estimation of Impurities in Tenofovir Disoproxil Fumarate and Emtricitabine Combination Tablets

Vihol¹,

Kothari²,

Patel³

et al. 2019

Int. Res. J. Pharm.

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Statistical experimental design was used to optimize the chromatographic separations of two potential impurities in fixed dose combination tablets. Risk assessment has been made based on knowledge gathered during development activity. The Critical Quality Attributes (CQA's) selected were Trifluoroacetic acid (TFA) concentration, organic solvent and column temperature. A Box-Behnken Design was utilized using Minitab software to study the effects of these CQA's on closely eluting peaks of S-Oxide and Tenofovir. The effect of these three CQA's on resolution is depicted in the form of the p and f values between the various combination and permutations of these three CQAs. The chromatographic method employed a HPLC, Zorbax SB-Phenyl C18 column (150 x 4.6 mm i.e., 3.5µm particle size) with the mobile phase consisting of a TFA buffer and Methanol: TFA ((85:15 v/v) in a gradient program. The flow rate, injection volume and detection were 1.0 mL/min, 15 μL and 262 nm respectively. As per design space, 15 validation runs were performed and out of which Run 11 gave more resolution, i.e., of 4.4 at 45 °C column temperature with 0.11 % TFA concentration in mobile phase A and Methanol: 0.1% TFA in water (85:15 % v/v) in mobile phase B which was studied with different plots like interaction plot and overlaid contour plots. The results clearly showed that the quality by design concept could be effectively applied to optimize HPLC chromatographic method parameters with fewer trials and error-free experimentation.

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Development of a validated liquid chromatographic method for the determination of related substances and assay of tenofovir disoproxil fumarate

Cited by 18 publications

References 7 publications

Selective RP-HPLC DAD method for determination of tenofovir fumarate and emtricitabine in bulk powder and in tablets

Selective RP-HPLC DAD method for determination of tenofovir fumarate and emtricitabine in bulk powder and in tablets

Simple Spectrophotometric Methods for Determination of Tenofovir Fumarate and Emtricitabine in Bulk Powder and in Tablets

Application of QBD Life Cycle Approach for Stability Indicating HPLC Method Development and Validation for the Estimation of Impurities in Tenofovir Disoproxil Fumarate and Emtricitabine Combination Tablets

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