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A validated method for development of tenofovir as API and tablet dosage forms by UV spectroscopy
Abstract
A simple new spectrophotometric method has been developed for estimation of Tenofovir disoproxil fumarate in bulk and tablet dosage form. Tenofovir disoproxil fumarate is estimated to be 261 nm in triple distilled water. The Beer′s law is obeyed in the concentration range of 5 - 90 µg/mL of the drug. The slope and intercept values are 0.0109 and 0.1075, respectively. Results of analysis of this method have been validated statically and by recovery studies. The method is applied to the marketed tablet formulation. A result of the analysis of tablet formulation, given as a percentage of label claim ± standard deviation is 98.15 ± 0.76. The precision and accuracy has been examined by performing recovery studies and found to be 100.06 ± 1.24. The developed method is simple, sensitive, and reproducible, and can be used for the routine analysis of Tenofovir disoproxil fumarate in bulk and tablet dosage form.
... Te mixture was held at 37 ± 0.5°C and swirled continuously at 100 rpm using a magnetic stirrer (REMI 2MLH). Te dissolution analysis was conducted under two distinct conditions: initially, in simulated stomach fuid (pH 1.2) and then in simulated intestinal fuid (pH 6. was used to evaluate each sample at 262 nm [51]. Te amount of drug released was then used to calculate the cumulative percentage of drug release: amount release � test absorbance × dilution factor × vol. of dissolution medium standard absorbance × 1000 × standard concentration, % drug release � amount release total drug used in the formulation × 100. ...
Purpose: The current study aimed to improve the oral bioavailability of tenofovir (TNF), an antihuman immunodeficiency viral (HIV) drug, by integrating it into solid lipid nanoparticles (SLNs), an emerging lipid formulation.
Method: The suggested SLNs were generated utilizing the microemulsion process, using Compritol 888 ATO. A Box–Behnken experimental design was attempted to analyze the impact of critical quality attributes (CQAs), such as lipid and surfactant content and homogenization duration on response metrics such as particle size (PS) and percentage entrapment. The prepared SLNs were assessed for entrapment efficiency, zeta potential (ZP), PS, polydispersity index, and in vitro drug release. Moreover, ex vivo permeation tests employing goat intestinal sacs, solid-state characterization by DSC and PXRD, surface morphology by SEM, and in vivo pharmacokinetic evaluation using albino Wistar rats were conducted.
Results: The research findings demonstrated that a formulation composed of 5.5% lipid and 2% surfactant had a comparatively smaller PS (449.90 ± 4.79 nm), a narrow size distribution (0.304 ± 0.004), and strong stability with an entrapment efficiency of 83.13 ± 6.34% and a negative ZP (−18.10 ± 2.35 mV). According to in vitro drug release experiments, first-order kinetics were followed and 99% of the medication was released over the time course of 24 h. In albino Wistar rats, an in vivo pharmacokinetic analysis of the optimized formulation (F10) showed a 12.4-fold improvement in bioavailability over pure TNF solution.
Conclusion: This study suggests the potential of SLNs in overcoming bioavailability issues, particularly low permeability, gut metabolism, and P-gp efflux transport.
... It is also reverse transcriptase inhibitor most commonly used in antiviral combination therapy. Based on literature as of now different analytical method were reported for both Emtricitabine and TAF individually [2][3][4][5][6][7][8]. Along with the individual methods, analytical and bio analytical methods were available in simultaneous estimation in combination with other antiviral drugs [9,10]. ...
Aim: The primary objective of the research work is to develop a effective, sensitive, economical and simple reverse phase HPLC method to estimate Emtricitabine and tenofovir alafenamide fumarate in its pure and binary mixture of tablets. Study Design: HPLC based Quantification Studies. Place and Duration of Study: 1Department of Chemistry, Acharya Nagarjuna University,Guntur, Andhra Pradesh between April 2019 and August 2020. Methodology: Separation of the analytes were done by using Eclipse XDB-Phenyl (250 x 4.6mm, 5µ,100 A0) column and a mobile phase ratio of 30:10:70 percentage of 0.1% trifluoro acetic acid: acetonitile: methanol at a flow rate of 1 ml/min. The injected standard and sample solutions were detected 260nm wavelength. Results: The retention time of Emtricitabine and tenofovir alafenamide fumarate were found at 2.3min and 2.8 min respectively. The method has good linearity range about 50 to 150µg/ml of Emtricitabine and 6.5 to 19.5 µg/ml of tenofovir alafenamide fumarate. The method has validated as per ICH guidelines and all the validation parameterwere satisfy the ICH Q2 specification acceptance limits Conclusion: The developed method said to be highly sensitive, accurate, specific and robust, therefore this method has high probability to adopt in pharmaceutical industry for regular analysis of Emtricitabine and tenofovir alafenamide.
... The method was validated according to International Conference on Harmonization (ICH) guidelines to determine the linearity, limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, ruggedness, and robustness of the method [17][18][19][20][21][22][23][24]. ...
Objective: The objective of this research work was to develop and validate a simple, precise, and accurate new ultraviolet-spectrophotometric method for the simultaneous estimation of emtricitabine (EMT), tenofovir disoproxil fumarate (TDF), cobicistat (COB), and elvitegravir (ELV) in pure and pharmaceutical marketed dosage form (stribild).Methods: Simultaneous equation method (Vierordt’s method) was developed for simultaneous determination of several mixtures containing two or more absorbing drugs (p, q, r, and s) each of which absorbs at the λ max of the other. Forced degradation studies were also conducted, and the drugs were subjected to various stress conditions such as acid hydrolysis, base hydrolysis, oxidative, photolytic, and thermal degradation.Results: The λ max of EMT, ten TDF, COB, and ELV are 283 nm, 259 nm, 240 nm, and 258 nm, respectively. The linearity ranges for the four drugs are EMT (4–24 μg/ml), TDF (10–50 μg/ml), COB (10–120 μg/ml), and ELV (2–10 μg/ml).Conclusion: The Vierordt’s method was successfully applied for simultaneous determination of EMT, TDF, COB, and ELV in a mixture of sample solution (pharmaceutical dosage form) and the results obtained were validated and found to be accurate, precise, linear, rugged, and robust.
... The method is more sensitive than previously reported methods based on RP-HPLC, 38 ion-pair RP-HPLC, 39 spectrophotometry, 40 HPLC with spectrofluorimetric detection 7 and UV spectroscopy. 41 ...
The electrochemical reduction of the antiretroviral drug, tenofovir (TNF), was studied in Britton Robinson (BR) buffer at the hanging mercury drop electrode (HMDE). Tenofovir showed one well-defined reduction peak in the potential range -1.2 to -1.4 V (vs. Ag/AgCl) due to reduction of the C = N bond of the imidazole ring. A method based on square-wave cathodic adsorptive stripping voltammetry (SWCAdSV) was optimized and validated for assay of TNF in human plasma and a tablet formulation. Sample preparation of plasma involved protein precipitation with acetonitrile. The method was linear in the concentration range 0.5-5.0 mu g/mL in both standard solutions and plasma with lower limits of quantitation (LLOQ) of 0.39 and 0.76 mu g/mL respectively. Accuracy was within the acceptance criteria of 100 +/- 15% of the theoretical value except at the LLOQ where it was 100 +/- 20%. Precision was within the criteria of 15% at all concentration levels. The proposed method was successfully applied to the determination of TNF in human plasma and a tablet formulation.
... Simple spectrophotometric techniques have been published involving determination of TEN by direct methods [4,5], derivative calculation [6][7][8]. Other spectrophotometric methods published include colorimetric assay using various derivatizing reagents [9][10][11][12]. ...
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.
... [1,2] It has been approved by United State Food and Drug Administration for the treatment of heavy metal poisoning and radioactive contamination, as decorporating agent, examples are mercury, plutonium, curium, cobalt, and americium. [5,7891011 Chelation therapy using disodium edetate is medically accepted treatment for lead poisoning and digoxin toxicity.12131415 Various methods such as thin layer chromatography (TLC), high pressure liquid chromatography (HPLC) and high pressure thin layer chromatography (HPTLC) have been reported for the estimation of disodium edetate in different formulations,16171819 but they are time consuming, costly, and require expertise.20212223 ...
... [1,2] It has been approved by United State Food and Drug Administration for the treatment of heavy metal poisoning and radioactive contamination, as decorporating agent, examples are mercury, plutonium, curium, cobalt, and americium. [5,[7][8][9][10][11] Chelation therapy using disodium edetate is medically accepted treatment for lead poisoning and digoxin toxicity. [12][13][14][15] Various methods such as thin layer chromatography (TLC), high pressure liquid chromatography (HPLC) and high pressure thin layer chromatography (HPTLC) have been reported for the estimation of disodium edetate in different formulations, [16][17][18][19] but they are time consuming, costly, and require expertise. ...
A simple, sensitive, cost-effective and reproducible UV-spectrophotometric method has been developed and validated for the estimation of disodium edetate in topical gel formulations. Solution of disodium edetate reacts with ferric chloride to form complex in 0.1 N HCl giving λmax at 270 nm. Beer's law was obeyed in the concentration range of 5-50 μg/mL (r (2)= 0.9997). The limit of detection and limit of quantitation were found to be 1.190 and 3.608 μg/mL, respectively. The results show that the procedure is accurate, precise, and reproducible (relative standard deviation < 1%), while being simple and less time consuming. The study concluded that the UV-spectrophotometric method could be used for the quantification of disodium edetate in pure form as well as in pharmaceutical formulations.
This study presents a novel method for the selective synthesis of 4‐, 5‐, 6‐, or 8‐alkylamino derivatives of quinoline and 8‐alkylaminoisoquinoline. The method leverages direct oxidative substitution of hydrogen with an alkylamino group within the molecules of 3(5,6,7,8)‐nitroquinolines and 5‐nitroisoquinoline in an aqueous environment. Notably, the regioselectivity of these reactions is solely governed by the presence of the nitro group. Its preservation in products makes it possible for further, deeper transformations in the molecule. This method is distinguished by its simplicity and scalability. image
Objective: A reverse- phase high performance liquid chromatographic (RP-HPLC) method was developed and validated for estimation of combined formulation containing tenofovir(disoproxilfumarate) (TDF) and emtricitabine (EMT). Method: Chromatographic separation was performed on RP-C18 column. The optimized mobile phase of composition (Methanol: Water and pH adjusted to 3.8 with acetic acid was pumped withflow rate of 0.8ml/min in the 70:30% v/v) ratio and the eluents were monitored at 261nm. Results: The assay was performed with tablet and percentage of assay was found to 99.91% for TDF and 99.69% for EMT respectively. Linearity was obtained in the concentration range of 2-12µg/ml for TDF and 2-12µg/ml for EMT. The method was statistically validated and RSD was found to be <2%, indicating high degree of accuracy and precision of the proposed RP-HPLC method. Conclusion: The method suggests usefulness of unique mobile phase during the estimation of combination of dosage forms. Due to its simplicity, rapidness, high precision and accuracy, the proposed RP-HPLC method can be applied for simultaneous determination of TDF and EMT in pharmaceutical dosage form.
A simple, efficient and reproducible Reverse Phase-High Performance Liquid Chromatography (RP-HPLC) method for the estimation of Tenofovir Disoproxil Fumarate in Pharmaceutical formulation has been validated. The Separation was carried out on C-18 column 4.6 mm x 250 cm x 5 µm column at ambient temperature using Buffer: Acetonitrile in the ratio of 60: 40 as a mobile phase. The flow rate was 1 ml/min and effluent was detected at 260nm. The retention times was found to be 3 mts. The percentage recovery was within the range between 99.23% to 101.44 %. The method was linear in the range of 50%-150% for Tenofovir Disoproxil Fumarate where r2 = 0.999. The percentage relative standard deviation for accuracy and precision was found to be less than 2%. The method was validated according to ICH guidelines and the acceptance criteria for specificity, linearity, accuracy, precision, ruggedness and robustness were met in all cases in detecting Tenofovir Disoproxil Fumarate. Hence the method could be successfully applied for routine analysis of Tenofovir Disoproxil Fumarate in the solid dosage form.
A simple, precise, accurate RP-HPLC method with PDA detector has been developed and subsequently validated for the simultaneous estimation of Emtricitabine and Tenofovir in pure and pharmaceutical dosage form. The estimation was carried out on Hyperclone C18 (250mm x 4.6mm i.d; particle size 5µm) column with a mixture of potassium di hydrogen phosphate buffer (pH-2.5 adjusted with orthophosphoric acid) and methanol in the ratio of 35:65 v/v as mobile phase at flow rate 1ml/min with UV detection performed at 254 nm. The retention times of Emtricitabine and Tenofovir were 2.580 min & 3.711 min respectively. The concentration range was found to be linear 30-70 µg/ml for Emtricitabine and 45-105 µg/ml for Tenofovir. The correlation coefficient (r2) was found to be 0.999 for both the drugs. The limit of detection was found to be 2.92 and 3.05 and the limit of quantification was found to be 3.05µg/ml and 10.07µg/ml for Emtricitabine and Tenofovir. The %RSD values were less than 2 for both the drugs. The assay of Emtricitabine and Tenofovir was found to be 99.77% and 100.12% respectively. The method was validated for linearity, accuracy, precision, robustness, LOD, LOQ as per ICH guidelines. The developed method was successfully used for the quantitative analysis of commercial available dosage form.
Tinofovir Disoproxil Fumarate (TDF) is an acyclic nucleotide diester analog of adenosine monophosphate from the antiviral
category utilized in the AIDS and hepatitis B treatment. In the present study, two analytical methods, i.e. UV and HPLC
were developed for the TDF’s estimation in pharmaceutical preparation. In the UV method, the mobile phase used was
Methanol and water in 60:40 ratio for estimation of the drug at 260 nm and an assay of the (TDF) obtained was 99.53%.
The method’s validation was carried out as per ICH Q2 R1 guidelines in which linearity was detected from 10-50 μg/ml
range with a regression value of 0.999 Percent RSD value of accuracy, precision and robustness were below 2. In the HPLC
method estimation of (TDF) was evaluated on Cosmosil C-18 (250mm×4.6ID, Particle size: 5 μ) column utilizing Methanol:
Water (60:40), 0.9 ml/min of flow rate, detection wavelength was 260 nm and the time of retention observed was around
4.63 minutes with the assay value 99.07%. HPLC method was also validated according to ICH guidelines, where linearity
was detected in the 10-50 μg/ml of range with the regression coefficient value 0.999. The % RSD of precision, accuracy, and
robustness was below 2%. The study of forced degradation was also performed by the HPLC method utilizing methanol:
water (60:40) at 260nm. From this study, it can be concluded that the developed methods for estimation of (TDF) drug in
pharmaceutical preparation are simple, accurate, precise, and can be utilized in the routine analysis for quantification of
the drug in a dosage form
Tenofovir Disoproxil Fumarate (TDF) is antiretroviral medicine used treat AIDS as well as chronic Hepatitis-B. TDF is a prodrug of tenofovir and exists as dominant form due to lesser oral bioavailability of parent drug. TDF is now available in a fixed-dose combination with various antiretrovirals like Cobicistat, Efavirenz, Elvitegravir, Emtricitabine, Lamivudine, Rilpivirine, and Nevirapine. Hence, pharmaceutical analysis of TDF and applicability of different analytical methods have gained crucial importance. The present review article assesses the published analytical methods and a variety of approach for investigation of TDF in bulk drug as well as pharmaceutical formulations including combinations. This detailed review includes examination of around eighty analytical methods published during 2008 to 2016 using various techniques which include HPLC, HPTLC, and UV/ Visible-Spectrophotometry. The review also illustrates the scope and limitations of many published analytical methods for analysis of TDF. Such detailed review will be of great help to the researcher who is working on TDF. Miscellaneous methods of rare but unique pharmaceutical distinction have also been given due consideration. The diagrammatic illustrations provide the statistical overview about the various methods referred for analysis of TDF.
Tenofovir Disoproxil Fumarate and Emtricitabine are very effectively used in the prevention of HIV-1 infections. They are generally administered as tablets. These are Nucleotide Reverse Transcriptase Inhibitors (NtRTIs), an acyclic nucleoside phosphonate (nucleotide) analog of adenosine 5′-monophosphate. Emtricitabine and Tenofovir disoproxil fumarate reveals equally prevention of the enzyme that is HIV-1 reverse transcriptase. For determination of Tenofovir disoproxil fumarate and Emtricitabine in bulk and pharmaceutical dosage form, several analytical methods including UV, HPLC, UPLC and HPTLC techniques are reported in literature. For qualitative and quantitative estimation of Tenofovir disoproxil fumarate and Emtricitabine these analytical methods can be used and also for the related degradants in bulk formulations and biological fluid. The present paper illustrates the review on analytical methods which involves the estimation of the antiviral drugs. Keywords: Emtricitabine, Tenofovir disoproxil fumarate, UV Spectroscopy, RP-HPLC, UPLC, HPTLC.
A novel, simple, precise, accurate stability indicating liquid chromato-graphy method was developed for the separation and simultaneous quantification of bictegravir, emtricitabine, tenofovir in bulk drug and pharmaceutical formulations. Separation was achieved on ProntoSILHypersorb ODS C18 column using mobile phase of 0.1 M sodium perchlorate, methanol in the ratio of 65:35 (v/v), pH 4.8 at a flow rate of 1.0 mL/min and UV detection was monitored at a wavelength of 258 nm. In these conditions, well resolved peaks were observed with acceptable system suitability at a retention time of 4.6 min for bictegravir, 7.0 min for emtricitabine and 10.1 min for tenofovir. Very high correlated linearity range was found to be 5-30 μg/mL for bictegravir, 20-120 μg/mL for emtricitabine and 2.5-15 μg/mL for tenofovir. The method can separate and identify the unknown degradation compounds formed during stress degradation study.
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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