Validated Chromatographic Methods for the Simultaneous Estimation of Etamsylate and Mefenamic Acid in the Presence of Their Main Impurities

2019 ◽  
Vol 15 (6) ◽  
pp. 624-631
Author(s):  
Asmaa Ahmed El-Zaher ◽  
Marianne Alphonse Mahrouse ◽  
Ahmed Mohammed Al-Ghani
Keyword(s):  
Quality Control ◽  
Mefenamic Acid ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Routine Analysis ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Chromatographic Methods ◽  
Rp Hplc ◽  
Ich Guidelines

Background: Etamsylate (ETS), a haemostatic drug, is formulated with mefenamic acid (MFA) for pain relief. Objective: The aim of this work was to develop chromatographic methods for the estimation of ETS and MFA in the presence of their main impurities. These methods could be used in the routine analysis in quality control laboratories. Methods: The first method was RP-HPLC method, the separation was carried out on an Inertsil® ODS- 3V C18 column using a mobile phase composed of acetonitrile: potassium dihydrogen phosphate buffer adjusted to pH 7 with 0.1 N NaOH (55: 45, v/v) at a flow rate of 1 ml/ min. The detection was carried out at 220 nm. The second method was a TLC-densitometric method where the studied components were separated using a developing system composed of dichloromethane: ethyl acetate: methanol: triethylamine (6: 2: 2: 0.5, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 300 nm. Results: In RP-HPLC method, the peaks were sharp and well separated, good retention times were obtained. Linearity was obtained over the concentration range 20-90 µg/ml, for both ETS and MFA. In the TLC-densitometric method, well separation of drug spots and linear relationship were achieved over the concentration range of 0.4-2.8 µg/spot, for both ETS and MFA. Method validation was conducted according to ICH guidelines. Conclusion: The developed methods were applied for the determination of the cited drugs in laboratory prepared mixtures and in tablets containing the two drugs. The methods are simple and precise and can be used for routine analysis of the drugs in combined dosage forms in quality control laboratories.

Validated Chromatographic Methods for Simultaneous Estimation of Cinnarizine in Binary Mixture with Domperidone and Paracetamol in Tablets

2019 ◽  
Vol 15 (5) ◽  
pp. 429-438
Author(s):  
Marianne Alphonse Mahrouse ◽  
Asmaa Ahmed El-Zaher ◽  
Ahmed Mohammed Al-Ghani
Keyword(s):  
Quality Control ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Chromatographic Methods ◽  
Treatment And Prevention ◽  
Rp Hplc ◽  
Linear Relationships ◽  
Ich Guidelines ◽  
Analytical Tools

Background:Cinnarizine, an antihistaminic drug, is commonly formulated in combination with domperidone and with paracetamol for treatment and prevention of motion sickness and migraine.Objective:The aim of this work was to develop new, simple, precise and selective chromatographic methods (RP-HPLC and TLC-densitometric methods) for the determination of these drugs. These methods can be used as analytical tools in the routine examination in quality control laboratories.Methods:The first method was RP-HPLC method, the separation was carried out on an Inertsil® ODS- 3V C18 column (250 mm × 4.6 mm, 5 µm) using a mobile phase composed of methanol: acetonitrile (45: 55, v/v) at a flow rate of 1 ml/min. The detection was carried out at 220 nm. The second method was a TLC-densitometric method where the studied components were separated using a developing system composed of toluene: ethyl acetate: methanol: triethylamine (5: 4.3: 0.7: 0.5, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 270 nm.Results:In RP-HPLC method, the peaks were sharp and well separated, the retention times were 5.25, 3.48 and 2.78 min, for cinnarizine, domperidone and paracetamol, respectively. Linearity was obtained over the concentration ranges 1-22, 0.75-16.5 and 25-550 µg/ml, for cinnarizine, domperidone and paracetamol, respectively. In TLC-densitometric method, good separation of spots and linear relationships were achieved over the concentration ranges of 0.2-2, 0.15-1.5 and 5-50 µg/spot, for cinnarizine, domperidone and paracetamol, respectively. Method validation was conducted according to ICH guidelines in terms of linearity, accuracy, selectivity, precision and robustness.Conclusion:The developed methods were applied for the determination of the cited drugs in tablets containing binary drug mixtures. The methods are simple and precise and can be used for routine analysis of the labelled drugs in combined dosage forms in quality control laboratories.

Stability Indicating Assay Method Development and Validation of Simultaneous Estimation of Chlorzoxazone, Diclofenac Sodium and Paracetamol in Bulk Drug and Tablet by RP-HPLC

2021 ◽  
pp. 5024-5028
Author(s):  
Krutika Patel ◽  
Sudheer Kumar Verriboina ◽  
S.G. Vasantharaju
Keyword(s):  
Method Development ◽  
Diclofenac Sodium ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Bulk Drug

A simple, accurate, specific and stability-indicating RP-HPLC method was developed for simultaneous determination of chlorzoxazone, diclofenac sodium and paracetamol, using C18 Vydac Monomeric 120A (250 × 4.6mm, 5μ) at 40ºC. The mobile phase contains a mixture of 20mM potassium dihydrogen phosphate buffer (pH 6.2 adjusted with potassium hydroxide) and acetonitrile (30:70 v/v). The flow rate was 1ml/min and detection was carried out at 275nm using PDA detector. The retention time of paracetamol, chlorzoxazone and diclofenac sodium were 3.28mins, 13.27mins and 15.61mins respectively. The analytical curve was linear over a concentration range of 0.65- 6.5μg/ml for paracetamol, 1-10μg/ml for chlorzoxazone and 0.1-1μg/ml for diclofenac sodium. The drugs in bulk and tablet were subjected to acid and alkali hydrolysis, oxidation, thermal and photolytic degradation. This method can be successfully employed for simultaneous quantitative analysis of Chlorzoxazone, Diclofenac sodium and Paracetamol in bulk drug and tablet formulation.

scholarly journals Implementation of QbD Principles for Simultaneous Quantitative Expression of Olmesartan Medoxomil, Telmisartan and Hydrochlorothiazide by RP-HPLC

2021 ◽  
pp. 50-61
Author(s):  
Binny Mehta ◽  
Hirak Joshi ◽  
Ujash Shah ◽  
Pinak Patel
Keyword(s):  
Data Analysis ◽  
Study Design ◽  
Potassium Dihydrogen Phosphate ◽  
Olmesartan Medoxomil ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Quantitative Expression ◽  
Rp Hplc ◽  
Development Cycle ◽  
Ich Guidelines

Aim and Study Design: Aims: The current research paper describes the RP-HPLC Method for estimation of Olmesartan Medoxomil, Telmisartan, and Hydrochlorothiazide and implements the role of QbD for Data Analysis Study design: Mentioned study is simple, rapid, economical, accurate, and robust RP-HPLC Method for Olmesartan Medoxomil, Telmisartan, and Hydrochlorothiazide and implementing QbD Approach for Data Analysis. Place and Duration of Study: The present study was carried out at Smt. S. M. Shah Pharmacy College, Mahemdabad, Gujarat, India from October 2019 to February 2020. Methodology: The separation was done on Hypersil ODS C18 column with dimensions (250mm x 4.6ID, Particle size: 5 microns) and Methanol: 0.02M potassium dihydrogen phosphate buffer (60:40%v/v) pH 3 used as mobile phase. The flow rate was 1.2ml/min; detection at 254nm. QbD approach was applied for data analysis. The method was validated according to ICH guidelines. Results: The RP-HPLC method was developed and validated for Linearity and Range through the QbD approach. Factorial Design was developed through Design Expert Software for estimation of Telmisartan, Olmesartan Medoxomil, and Hydrochlorothiazide. 27 experiments were constructed and its effect was seen on Resolution, Tailing factor, and Retention Time. Conclusion: It was clear that the proposed method was suitable for the QbD approach and identification and validation approaches. This process helps in the proper understanding of the parameters and less amount of time for the development cycle of the analytical method.

scholarly journals Development and Validation of RP-HPLC Method for Estimation of Teneligliptin and its Impurity in Tablet

2021 ◽  
Vol 69 (02) ◽  
Author(s):  
Bhoomi Dineshkumar Patel ◽  
Nidhi J. Dharsandiya ◽  
Ankit Chaudhary
Keyword(s):  
Present Method ◽  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Development And Validation ◽  
Tablet Dosage

The objective of the study is a simple, precise and accurate stability RP-HPLC method has been developed and subsequently validated for the estimation of Teneligliptin and its impurity in tablet formulation. The adequate separation was carried out using Grace Smart C18 column (250mm x 4.6mm, 5?m particle size), mixture of 0.05M Potassium dihydrogen phosphate PH 4.0 and Acetonitrile 80:20 % v/v as a mobile phase with a flow rate of 1 ml/min and the effluent was monitored at 242 nm using PDA detector. The retention time of Teneligliptin, Impurity B and Impurity G were 7.443 min, 6.650 min and 8.473 min respectively. Linearity for Teneligliptin, Impurity B and Impurity G were found in the range of 500-3000 µg/ml (R2 = 0.998), 5-15 µg/ml (R2 = 0.994) and 5-15 µg/ml (R2 = 0.998) respectively. The accuracy of the present method was evaluated at 50%, 100% and 150%. The % recoveries of drug were found to be in range of 99.315 ± 0.283 for Teneligliptin. Precision studies were carried out and the RSD values were less than two. The method was found to be robust. The proposed method was found to be specific, accurate, precise and robust can be used for simultaneous estimation of these drugs in tablet dosage form.

scholarly journals Validated stability-indicating RP-HPLC method for simultaneous estimation of cilnidipine and chlorthalidone in tablet dosage form

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 2435-2441
Author(s):  
Ashok B. Patel ◽  
Amitkumar J. Vyas ◽  
Shital Faldu ◽  
Arvind N Lumbhani ◽  
Nikunj J. Patel ◽  
...  
Keyword(s):  
Phosphoric Acid ◽  
Dosage Form ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Tablet Dosage ◽  
Ich Guideline

A novel, simple, specific, accurate & precise stability-indicating Gradient reverse-phase high-performance liquid chromatography (RP-HPLC) method was developed for simultaneous estimation of Cilnidipine & Chlorthalidone in tablet dosage form, validated as per ICH guideline. The separation was achieved on Inertsil ODS column (250 mm x 4.6 mm, 5 μm) in a gradient mode.  The mobile phase consisted of Methanol, 0.025 M Potassium dihydrogen phosphate Buffer pH 5.5 adjusted by 10% v/v Ortho Phosphoric Acid (50:50 v/v) (Solution A) and Acetonitrile, 0.025 M Potassium dihydrogen phosphate Buffer pH 5.5 adjusted by 10%v/v Ortho Phosphoric Acid (75:25 v/v) (Solution B), gradient programming for 20 min at 1 ml/min rate of flow and response was detected at 225 nm. The retention time was found to be 3.580 min and 12.606 mins for Chlorthalidone and Cilnidipine, respectively. The method is validated according to ICH guideline, which includes linearity, specificity, accuracy, precision and robustness. Linearity was obtained over the concentration range of 10-60 μg/ml for Cilnidipine and 6.25-37.5 μg/ml for Chlorthalidone, had a regression coefficient (r2) almost 0.9966. The % Recovery was found to be 99.63-100.59 % and 100.24-100.51 % for Cilnidipine and Chlorthalidone, respectively. The method was found to be specific enough to separate all degradation products from the active compound. Drug samples were exposed to various stress conditions like photolysis, oxidation, heat conditions, and hydrolysis (acidic and alkaline), there was no interference of any degradants and excipient in the determination of drugs so that methods can be successfully applied for routine QC analysis.

scholarly journals A Validated RP-HPLC Method for Simultaneous Estimation of Antidiabetic Drugs Pioglitazone HCl and Glimepiride

2013 ◽  
Vol 16 (1) ◽  
pp. 69-75 ◽  
Author(s):  
Khohinur Hossain ◽  
Asma Rahman ◽  
Md Zakir Sultan ◽  
Farhana Islam ◽  
Md Akteruzzaman ◽  
...  
Keyword(s):  
High Performance ◽  
Potassium Dihydrogen Phosphate ◽  
Pharmaceutical Journal ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Allowable Limit ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc

A simple, fast and economic reversed phase high performance liquid chromatographic (RP-HPLC) method has been developed and validated for simultaneous and quantitative analyses of pioglitazone HCl and glimepiride in pharmaceutical dosage forms. The method was developed using the mobile phase comprising of potassium dihydrogen phosphate buffer (KH2PO4) at pH 3.4 and acetonitrile in the ratio of 40:60 (v/v) over C-18 bonded silica column (250 x 4.6 mm, 5 um, Phenomenex Inc.) at ambient temperature. The flow rate was at 0.8 min/min and the eluent was monitored by UV detection at 235 nm. The recoveries were found to be >97% for pioglitazone and >99% for glimepiride, demonstrative of accuracy of the protocol. Inter-day and intra-day precision of the new method were less than the maximum allowable limit (RSD% ? 2.0) according to ICH, USP and FDA guidelines. The method showed linear response with correlation coefficient (r2) values of 0.9991 for pioglitazone and 0.9999 for glimepiride. Therefore, the method was found to be accurate, reproducible, sensitive and less time consuming and can be successfully applied for the assay of pioglitazone and glimepiride in combined formulations. DOI: http://dx.doi.org/10.3329/bpj.v16i1.14497 Bangladesh Pharmaceutical Journal 16(1): 69-75, 2013

DEVELOPMENT AND VALIDATION OF LIQUID CHROMATOGRAPHIC METHOD FOR SIMULTANEOUS ESTIMATION OF STRYCHNINE AND GALLIC ACID

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (06) ◽  
pp. 46-50
Author(s):  
V. V. Khanvilkar ◽  
◽  
M Toraskar
Keyword(s):  
Gallic Acid ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic

An accurate, precise and robust RP-HPLC method was developed for the simultaneous estimation of strychnine and gallic acid. The markers were resolved using HiQ C18HS column with methanol and potassium dihydrogen phosphate buffer (10 mM, pH 3) (60:40 V/V) as mobile phase at flow rate of 1 mL per minute and run time of 6 minutes. Retention times of strychnine and gallic acid were 3 and 4.7 minutes, respectively at 264 nm. The linearity range for strychnine and gallic acid was found to be 0.5-3 μg/mL and 1-3.5 µg/mL, respectively with coefficient of linear regression greater than 0.99 for both the markers. The developed method was validated as per ICH Q2 (R1) guidelines and the results obtained were satisfactory. The method was applied for quantification of markers in marketed and In-house formulations of Agnitundi Vati, a polyherbal ayurvedic formulation. The developed method thus could be used for standardization of Agnitundi Vati and other herbal preparations containing these two markers.

Validation of RP-HPLC Method for Simultaneous Estimation of Cefixime Trihydrate and Clavulanate Potassium in Tablets

2013 ◽  
Vol 6 (2) ◽  
pp. 2033-2039
Author(s):  
S.S. Zade ◽  
Bhatpalliwar V.B ◽  
N S Mendhule ◽  
M V Murkhekar ◽  
R S Alaspure ◽  
...  
Keyword(s):  
Method Development ◽  
Potassium Dihydrogen Phosphate ◽  
Correlation Coefficients ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Ich Guidelines ◽  
Optimum Wavelength ◽  
Hplc Method Development ◽  
Tablet Dosage

A simple, accurate, precise, rapid and economic HPLC method has been developed and validated for the simultaneous estimation of cefixime trihydrate and clavulanate potassium in tablet dosage forms. The chromatographic separation was achieved on a Hypersil C18 column (4.6 x 250 mm, 5 μm particle size). For HPLC method development, a mobile phase consisting of methanol: 30 mM potassium dihydrogen phosphate buffer pH 3.0 adjusted with orthophosphoric acid (30:70 v/v) was used at flow rate of 1.0 ml/min. The optimum wavelength selected was 278 nm. Under these chromatographic conditions, cefixime trihydrate and clavulanate potassium peaks were well resolved, with retention times of cefixime trihydrate and clavulanate potassium being 5.8266 and 3.2633 min, respectively. The proposed method was found to have excellent linearity in the concentration range 20-100 μg/ml with correlation coefficients r2 = 0.9946 and 0.9926, respectively. The method was validated for linearity, precision, LOD, LOQ and robustness. The proposed method was optimized and validated as per the ICH guidelines.

Simultaneous Estimation and Validation of Tenofovir Disoproxil Fumarate, Emtricitabine and Efavirenz by RP-HPLC Method in Combined tablet Dosage Form

2019 ◽  
Vol 15 (6) ◽  
pp. 561-567 ◽  
Author(s):  
Mehdi Rezaei ◽  
Ali Ramazani ◽  
Fahimeh Hokmabadi
Keyword(s):  
Tenofovir Disoproxil Fumarate ◽  
Dosage Form ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Assay Method ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Rp Hplc ◽  
Successful Separation ◽  
Tablet Dosage

Introduction: The purpose of this study is the development and validation of assay test for Tenofovir Disoproxil Fumarate (TDF), Emtricitabine (FTC) and Efavirenz (EFV) in combined tablet dosage form by Reverse Phase (RP) HPLC. Materials and Methods: The assay method by HPLC was found to be linear in the concentration range of 15-150 µg/mL, 10-100 µg/mL and 30-300 µg/mL for TDF, FTC, and EFV, respectively. Successful separation of combined drugs was achieved by isocratic elution on a Phenomenex® C8 column (250 mm × 4.6 mm, 5µm). The mobile phase was composed of buffer pH: 7.0 ± 0.05 potassium dihydrogen phosphate, acetonitrile and methanol (40:40:20 v/v) at the flow rate of 1 mL/min using UV detection at 262 nm, column oven temperature 25ºC, and injection volume 20 µL. Results: The analytical results were validated by recovery studies. All the parameters of validation were in the acceptance range. This developed method was successfully applied for simultaneous estimation the amount of TDF, FTC and EFV in the bulk and marketed dosage forms.

scholarly journals A NOVEL RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF BERBERINE, QUERCETIN, AND PIPERINE IN AN AYURVEDIC FORMULATION

2019 ◽  
Vol 11 (1) ◽  
pp. 94
Author(s):  
Swati Sahani ◽  
Vandana Jain
Keyword(s):  
High Performance ◽  
Quantitative Estimation ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Raw Material ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Rp Hplc ◽  
Relative Standard

Objective: The objective of this study was to develop and validate a novel, simple, rapid, precise and accurate reversed-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous quantitative estimation of berberine, quercetin, and piperine in Ayurvedic formulation.Methods: The chromatographic separation was achieved using a stationary phase C18 shim-pack (150 mm x 4.6 mm, 5µ) column and mobile phase consisted of acetonitrile: 0.04 M potassium dihydrogen phosphate buffer (pH 3.0 adjusted using orthophosphoric acid) in a ratio of 65:35 v/v, with a flow rate of 1 ml/min and UV detection at 255 nm.Results: The retention time of berberine, quercetin, and piperine were found to be 2.7, 3.0 and 6.3 min respectively. Linearity for berberine, quercetin, and piperine were found in the range of 12-28 µg/ml. All calibration curve showed good linear correlation coefficients (r2˃ 0.999) within the tested ranges. Mean percent recoveries for berberine, quercetin, and piperine were found to be within the acceptance limits (98-120%). The percent relative standard deviation (% RSD) for precision was found to be less than 2% which indicates method is precise.Conclusion: The developed method is novel, simple, precise, accurate and can be used for quantitative analysis and quality control of the raw material as well as other commercial formulations containing these three markers.

Sign in / Sign up

Export Citation Format

Share Document