scholarly journals Chromatographic Method for Quantification of Tenofovir in Pharmaceutical Formulations: Comparison with Spectrophotometric Method

2021 ◽  
pp. 272-280
Author(s):  
Erten Akbel ◽  
Ibrahim Bulduk
Keyword(s):  
Analytical Methods ◽  
Raw Materials ◽  
Pure Water ◽  
Antiviral Agent ◽  
Pharmaceutical Formulations ◽  
Therapeutic Drug ◽  
Uv Spectrum ◽  
Relative Standard ◽  
Significant Difference ◽  
Liquid Chromatographic

Aims: An efficient therapeutic drug or antiviral agent to treat Covid-19 is still not available. But, previously licensed pharmaceuticals to treat other virus infections are usedon an off-label basis either alone or in combination. Tenofovir emerged as a promising treatment for Covid-19 in September 2020. It is an antiretroviral drug that is active against many viruses. This study explains the development and asessment of liquid chromatographic and UV spectrophotometric methods to quantify tenofovir in raw materials and tablets. Methods: HPLC analyzes were performed using a C18 column and a mobile phase composed of 20 mM KH2PO4, with a flow rate of 0.8 mLmin-1 and UV detection at 260 nm. For the spectrophotometric analyzes, ultra-pure water was used as a solvent. UV spectrum of standard and sample solution were recorded between 200 and400 nm and Tenofovir was detected using a wavelength of 260 nm. Both methods have been validated according to the procedures described in ICH guidelines Q2(R1) for the validation of analytical methods. Results: The results showed that both spectrophotometric and liquid chromatographic methods were linear, precise, accurate, rugged and robust with relative standard deviation R.S.D.% values less than 1%, and the recovery percentage was within standard limits (98-102%). Then a statistical comparison of these two analytical methods was performed, and the results of both methods showed no significant difference. It was found that both methods were not statistically significant with respect to each other in the 95% confidence interval (p<0.05). As a result, the proposed methods were found to be highly effective and could be used for routine analysis of tenofovir in pharmaceutical formulations.

scholarly journals Spectrophotometric and High Performance Liquid Chromatographic Determination of Carbamazepine in Tablets Dosage Form

2021 ◽  
pp. 731-741
Author(s):  
Ibrahim Bulduk ◽  
Serdar Gungor
Keyword(s):  
Analytical Methods ◽  
High Performance ◽  
Neurological Diseases ◽  
Pharmaceutical Formulations ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Solution Ph ◽  
Significant Difference ◽  
Liquid Chromatographic

Today, millions of people suffer from epilepsy, one of the most common chronic neurological diseases worldwide. Carbamazepine is a first-line drug used in the treatment of epilepsy. High performance liquid chromatographic and spectrophotometric methods have been developed for the determination of carbamazepine in tablet dosage forms. UV spectrums were recorded in the wavelength range of 200-800 nm using methanol solvent, and the wavelength for determining carbamazepine was selected as 286 nm. LC analysis was performed using Agilent Extend-C18 column and mobile phase composed of KH2PO4 solution(pH: 3.5) and acetonitrile (40:60 v/v) at a flow rate of 1.2 mlmin-1. These analytical methods were validated in agreement with the International Conference on Harmonization (ICH) guidelines using the following analytical parameters: specificity, linearity, precision, accuracy, detection and quantification limits, and robustnes. Analytical methods showed wonderful linearity (r2>0.999) in the concentration range of 5-25 μg mL-1 for boths methods. Precision (R.S.D%<1.17) and recevery for both methods was in the range of 99-101%, which shows accuracy of these methods. These proposed methods were found to be accurate, reliable, fast, simple, The F-test and t-test were used to perform statistical comparison of these methods, and the results of both analytical methods indicated no significant difference. As a result, the proposed methods can be used to analyze carbamazepine in pharmaceutical formulations.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

scholarly journals Column High-Performance Liquid Chromatographic Determination of Norfloxacin and Its Main Impurities in Pharmaceuticals

2008 ◽  
Vol 91 (2) ◽  
pp. 332-338 ◽  
Author(s):  
Branislava Mielji ◽  
Gordana Popovi ◽  
Danica Agbaba ◽  
Slavko Markovi ◽  
Breda Simonovska ◽  
...  
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Array Detector ◽  
Chromatographic Separations ◽  
Experimental Conditions ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A gradient reversed-phase column high-performance liquid chromatographic method was developed for the detection and quantification of norfloxacin and its major impurities in norfloxacin-containing pharmaceuticals. Chromatographic separations were performed under the following experimental conditions: column, Zorbax SB RP-18 (5 m, 250 4.6 mm); injection volume, 20 L; mobile phase, 0.05 M NaH2PO4 (pH 2.5)acetonitrile (87 + 13) for 16 min and (58 + 42) for 9 min (stepwise gradient); and flow rate, 1.3 mL/min. All analyses were performed at 25C, and the eluate was monitored at 275 nm using a diode array detector. Linearity (correlation coefficient = 0.999), recovery (99.3101.8), relative standard deviation (0.20.7), and quantitation limit (0.120.47 g/mL) were evaluated and found to be satisfactory. The method is simple, rapid, and convenient for purity control of norfloxacin in both raw materials and dosage forms.

scholarly journals Validation of UV Spectrophotometric and Nonaqueous Titration Methods for the Determination of Carvedilol in Pharmaceutical Formulations

2005 ◽  
Vol 88 (5) ◽  
pp. 1299-1303 ◽  
Author(s):  
Carine Viana Silva Ieggli ◽  
Simone Gonçalves Cardoso ◽  
Luziane Potrich Belle
Keyword(s):  
Pharmaceutical Formulations ◽  
The United States ◽  
Violet Crystal ◽  
Relative Standard ◽  
Significant Difference ◽  
Precision And Accuracy ◽  
States Pharmacopeia ◽  
Interday Precision ◽  
Volumetric Methods

Abstract Ultraviolet (UV) spectrophotometric and nonaqueous volumetric methods are described for the determination of carvedilol in pharmaceutical formulations. Linearity, precision, and accuracy were evaluated according to the validation guidelines of the International Conference on Harmonizationand the United States Pharmacopeia for both methods. The UV spectrophotometric procedure was performed in ethanol at 244 nm. Good linearity was obtained between 2 and 7 μg/mL with a correlation coefficient of 0.9999. The intra- and interday precision values were &lt;2% for all samples analyzed. The accuracy, determined from recovery studies, was between 97.5 and 102.2%. The other procedure was based on the volumetric quantitation of carvedilol in a nonaqueous medium with 0.01M perchloric acid and 1% violet crystal as the indicator. The validation of the volumetric method yielded good results that included linearity (r of &gt;0.999), precision (relative standard deviations of &lt;2% for intra- and interday precision), and accuracy (96.4–102.4%). The methods were applied to tablets and compounded capsules. Statistical analysis by analysis of variance showed no significant difference between the results obtained by the proposed methods.

Liquid Chromatographic Determination of Glyburide (Glibenclamide) and Its Related Compounds in Raw Materials

1993 ◽  
Vol 76 (5) ◽  
pp. 962-965
Author(s):  
Normand Beaulieu ◽  
Susan J Graham ◽  
Edward G Lovering
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A liquid chromatographic method has been developed for the determination of glyburide and 3 known related compounds in drug raw materials. The lower limit of quantitation of the related compounds is about 0.02%. Evaluation of 9 drug raw materials revealed total impurities ranging from 0.17 to 0.65%. The relative standard deviation of the assay method is &lt;1%.

scholarly journals UV Spectrophotometry and Nonaqueous Determination of Terbinafine Hydrochloride in Dosage Forms

1999 ◽  
Vol 82 (4) ◽  
pp. 830-833 ◽  
Author(s):  
Simone Gonçalves Cardoso ◽  
Elfrides E S Schapoval
Keyword(s):  
High Performance ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
High Performance Liquid Chromatographic ◽  
Volumetric Method ◽  
Uv Spectrophotometry ◽  
Terbinafine Hydrochloride ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract An ultraviolet spectrophotometric and a nonaqueous volumetric method for determining terbinafine hydrochloride (TH) in pharmaceutical formulations are presented. The UV spectrophotometric procedure was developed for assay of TH in raw materials, tablets, and creams. The method was tested for linearity (0.8–2.8 μg/mL, r = 0.9997), recovery (102.00% for creams and 99.90% for tablets) and precision (101.3%, CV = 0.96%, n = 9, for creams; 100.25%, CV = 1.08%, n = 9, for tablets). The volumetric method involves titration of TH with 0.05M perchloric acid with crystal violet as indicator. This method was used for quantitative determination of TH in raw materials and tablets. Mean recovery and precision were, respectively, 100.41 and 101.18% (CV = 1.64%, n = 9) for TH in tablets. There were no significant differences between the proposed methods and a previously described high-performance liquid chromatographic method. The UV spectrophotometric and titrimetric methods are potentially useful for a routine laboratory because of their simplicity, rapidity, and accuracy.

scholarly journals Development and Validation of Column High-Performance Liquid Chromatographic and Ultraviolet Spectrophotometric Methods for Citalopram in Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 52-58 ◽  
Author(s):  
Jlia Menegola ◽  
Martin Steppe ◽  
Elfrides E S Schapoval
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference ◽  
Liquid Chromatographic

Abstract Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection, and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30 triethylamine solutionacetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10 ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.0070.00 g/mL, and 2.5017.50 g/mL for the UV spectrophotometric method. The interday and intraday assay precision was &lt;1.5 (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70101.35 for the LC method and 98.4898.65 for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets.

scholarly journals Ultraviolet spectrophotometric method for analytical determination of mianserin hydrochloride in coated tablets and comparison with LC

2015 ◽  
Vol 51 (4) ◽  
pp. 833-837 ◽  
Author(s):  
Letícia Lenz Sfair ◽  
Jeferson Scarpari Graeff ◽  
Martin Steppe ◽  
Elfrides Eva Scherman Schapoval
Keyword(s):  
Low Cost ◽  
Potassium Phosphate ◽  
Analytical Determination ◽  
Potassium Phosphate Buffer ◽  
Precision Data ◽  
Relative Standard ◽  
Significant Difference ◽  
Precision And Accuracy ◽  
Liquid Chromatographic

abstract Ultraviolet spectrophotometric (UV) and Liquid Chromatographic (LC) methods for the determination of mianserin hydrochloride in pharmaceutical formulation were developed and validated. The various parameters, such as specificity, linearity, precision and accuracy were studied according to International Conference on Harmonization (ICH, 2005). For UV method, mianserin hydrochloride was determinate at 278 nm using HCl 0.1 M as the solvent. The response was linear in the concentration range of 20.0 - 140.0 µg/mL (r = 0.9998). Precision data evaluated by relative standard deviation was lower than 2%. The UV method was simple, rapid and low cost. Chromatographic analyses were performed in an Ace C18 column and the mobile phase was composed of methanol, 50 mM monobasic potassium phosphate buffer and 0.3% triethylamine solution adjusted to pH 7.0 with phosphoric acid 10% (85:15). LC method was specific, linear, precise, exact and robust. The results confirmed that the both methods are valid and useful to the routine quality control of mianserin hydrochloride in coated tablets. Statistical analysis by Student´s t-test showed no significant difference between the results obtained by UV and LC methods.

scholarly journals A comparative study of HPLC and UV spectrophotometric methods for oseltamivir quantification in pharmaceutical formulations

2021 ◽  
Author(s):  
Serdar Gungor ◽  
Ibrahim Bulduk ◽  
Beyza Sultan Aydın ◽  
Rahsan Ilikci Sagkan
Keyword(s):  
Mobile Phase ◽  
Antiviral Drug ◽  
Pharmaceutical Formulations ◽  
Influenza Viruses ◽  
Dihydrogen Phosphate ◽  
Phosphate Solution ◽  
Uv Spectrum ◽  
Mobile Phase Flow Rate ◽  
Relative Standard

AbstractOseltamivir is an antiviral drug and is used in the treatment of all influenza viruses. It is the most effective antiviral option against all influenza viruses that can infect humans. UV and LC methods have been developed and validated according to ICH guidelines for various parameters like selectivity, linearity, accuracy, precision, LOD and LOQ, robustness for the quantitative determination of oseltamivir in pharmaceutical formulations. LC method has been performed using reverse phase technique on a C-18 column with a mobile phase consisting of 20 mM potassium dihydrogen phosphate solution and acetonitrile (60:40, v/v) at 25 °C. The mobile phase flow rate was 1.2 mL min−1. For the determination of oseltamivir, UV spectrum has been recorded between 200 and 800 nm using methanol as solvent and the wavelength of 215 nm has been selected. Both methods have demonstrated good linearity, precision and recovery. No spectral and chromatographic interferences from the capsule excipients were found in UV and LC methods. In both methods, correlation coefficients were greater than 0.999 within a concentration range of 10–60 mg mL−1 using UV and LC. Intra-day and inter-day precision with low relative standard deviation values were observed. The accuracy of these methods was within the range 99.85–100.17% for LC and from 99.26 to 100.70% for UV. Therefore UV and LC methods gave the most reliable outcomes for the determination of oseltamivir in pharmaceutical formulation.

scholarly journals Quality of Ceftriaxone Sodium in Lyophilized Powder for Injection Evaluated by Clean, Fast, and Efficient Spectrophotometric Method

2017 ◽  
Vol 2017 ◽  
pp. 1-4 ◽  
Author(s):  
Patrícia Vidal de Aléssio ◽  
Ana Carolina Kogawa ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Spectrophotometric Method ◽  
Pharmaceutical Formulations ◽  
Uv Detector ◽  
Ceftriaxone Sodium ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Significant Difference ◽  
Gram Negative Organisms ◽  
Comparison Of The Results

Ceftriaxone sodium, an antimicrobial agent that plays an important role in clinical practice, is successfully used to treat infections caused by most Gram-positive and Gram-negative organisms. Since there are few rapid analytical methods for ceftriaxone analysis to use in the pharmaceutical routine, the aim of this research was to develop a new method able to quantify this cephalosporin. Therefore, a sensitive, rapid, simple UV spectrophotometric method for the determination and quantification of ceftriaxone sodium was proposed. The UV detector was set at 241 nm. Beer’s law obeyed the concentration range of 10–20 µg mL−1. Statistical comparison of the results with a well-established reported method showed excellent agreement and proved that there is no significant difference in the accuracy and precision. Intra- and interday variability for the method were less than 2% relative standard deviation. The proposed method was applied to the determination of the examined drugs in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise, and reproducible as the official methods.

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