Fast HPLC Method for the Determination of Piroxicam and its Application to Stability Study

2017 ◽  
Vol 68 (4) ◽  
pp. 701-706 ◽  
Author(s):  
Alina Diana Panainte ◽  
Madalina Vieriu ◽  
Gladiola Tantaru ◽  
Mihai Apostu ◽  
Nela Bibire
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Calibration Graph ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
System Suitability ◽  
Optimum Separation

A fast and robust RP-HPLC isocratic method was developed for determination of piroxicam in bulk materials and pharmaceutical formulations. Optimum separation of piroxicam and stress induced degradation a product was achieved using a SB-C18 Eclipse column (150x4.6; 5�m). The mobile phase was a mixture of water: acetonitrile (50:50) with a flow rate of 0.5mL/min. The UV detection was performed at 360nm. The method was validated in accordance with the current ICH guidelines in terms of linearity, limit of detection, limit of quantification, precision, accuracy, recovery and system suitability. The retention time for piroxicam was 2.55 min. The calibration graph was linear in the concentration range 5-90�g/mL. The assay proved to be sensitive, specific and reproducible. The method was applied for the determination of piroxicam in tablets.

scholarly journals Determination of Enalapril maleate from tablets using a new HPLC method

2021 ◽  
Vol 32 (1) ◽  
pp. 70-75
Author(s):  
Simona Gherman ◽  
Daniela Zavastin ◽  
Adrian Şpac ◽  
Alina Diana Panainte
Keyword(s):  
Detection Limit ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Enalapril Maleate ◽  
Ich Guidelines ◽  
System Suitability

Abstract For the determination of enalapril maleate in tablets a new, simple and economical HPLC method was developed and fully validated. Chromatographic separation was achieved on Hewlett Zorbax SB-C 18 (150 x 4.6 mm, 5 μm) column and the mobile phase consisted of acetonitrile: 0.025 M phosphate buffer adjusted to pH 3 (70:30 v/v) pumped at a flow rate 0.8 mL/min and UV-detection was performed at 210 nm. The proposed method was validated according to ICH guidelines (linearity, limit of detection, limit of quantification, precision, accuracy, recovery and system suitability). The total run time was less than 3 min and the retention time for Enalapril maleate was 2.3 min. The calibration graph was linear in the concentration range between 10 – 100 μg/mL with the correlation coefficient r2 = 0.9998. The developed and validated method was successfully applied to determine the Enalapril maleate in tablets. Therefore, this method proved to be sensitive, specific and reproducible and can be applied for routine analysis of enalapril maleate from pharmaceutical formulation due to its simplicity of application.

scholarly journals Rapid, Simple, and Sensitive Spectrofluorimetric Method for the Estimation of Ganciclovir in Bulk and Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Garima Balwani ◽  
Emil Joseph ◽  
Satish Reddi ◽  
Vibhu Nagpal ◽  
Ranendra N. Saha
Keyword(s):  
Standard Deviation ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Calibration Graph ◽  
Limit Of Quantification ◽  
Average Percentage ◽  
Ich Guidelines ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A new, simple, rapid, sensitive, accurate, and affordable spectrofluorimetric method was developed and validated for the estimation of ganciclovir in bulk as well as in marketed formulations. The method was based on measuring the native fluorescence of ganciclovir in 0.2 M hydrochloric acid buffer of pH 1.2 at 374 nm after excitation at 257 nm. The calibration graph was found to be rectilinear in the concentration range of 0.25–2.00 μg mL−1. The limit of quantification and limit of detection were found to be 0.029 μg mL−1and 0.010μg mL−1, respectively. The method was fully validated for various parameters according to ICH guidelines. The results demonstrated that the procedure is accurate, precise, and reproducible (relative standard deviation <2%) and can be successfully applied for the determination of ganciclovir in its commercial capsules with average percentage recovery of 101.31 ± 0.90.

DEVELOPMENT AND VALIDATION OF RP HPLC METHOD FOR THE ESTIMATION OF SOFOSBUVIR IN BULK, TABLET AND INDUSTRIAL WASTE WATER

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (06) ◽  
pp. 59-66
Author(s):  
V Dhanunjayachary ◽  
◽  
V.L.S. Likhitha ◽  
Sri K. Vijaya ◽  
M. A Madhuri
Keyword(s):  
Industrial Waste ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Limit Of Quantitation ◽  
Development And Validation

The study was aimed at development and validation of RP-HPLC method for estimation of sofosbuvir in bulk, pharmaceutical dosage form and pharmaceutical industrial waste. The chromatographic separation was performed on Agilent Syncronis C 18 (100 mm × 4.6 mm, 5μm) column, with a mobile phase comprising of a mixture of methanol: acetonitrile: water (45:30:25 v/v/V). The flow rate was 1.0 mL/min with detection at 260 nm. Retention time of sofosbuvir was found to be 2.040 min. As per ICH guidelines, the method was validated for linearity, accuracy, limit of detection, limit of quantitation, precision, robustness and system suitability. Linearity was found to be in the range of 4-24 μg/mL with regression equation y = 675284.x + 49120 and correlation coefficient 0.999. The low % RSD values indicate the method to be accurate and precise. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.046 and 0.1400 μg/mL, respectively. The % recovery of tablets was found to be in the range of 99.9– 101.3%. It can be concluded that this validated HPLC method is easy, precise, accurate, sensitive and selective for estimation of sofosbuvir in bulk, tablet and applicable for analyses of in pharmaceutical industrial waste.

scholarly journals DEVELOPMENT AND VALIDATION OF HPLC-DAD METHOD FOR THE DETERMINATION OF BISOPROLOL IN TABLET DOSAGE FORMS

2017 ◽  
Vol 9 (6) ◽  
pp. 54 ◽  
Author(s):  
Yuliya Kondratova ◽  
Liliya Logoyda ◽  
Yuliia Voloshko ◽  
Ahmed Abdel Megied ◽  
Dmytro Korobko ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Label Claim ◽  
Development And Validation ◽  
Tablet Dosage

Objective: A rapid, simple and sensitive RP-HPLC method was developed and validated for the determination of bisoprolol fumarate in bulk and pharmaceutical dosage form.Methods: Chromatographic separation was achieved within 2.5 min on ACQUITY Arc System, Waters Symmetry C18 column (3.9 mm i.d. X 150 mm, 5 μm particle sizes) using a mobile phase consisted of acetonitrile: phosphate buffer (25:75 v/v) in an isocratic mode at a flow rate of 1.4 ml/min. The pH of the mobile phase was adjusted to 7.0 with orthophosphoric acid and UV detection was set at 226 nm.Results: The retention time for bisoprolol fumarate was found to be 2.09 min. The proposed method was validated according to ICH guidelines with respect to linearity, specificity precision, accuracy and robustness. The limit of detection and limit of quantification are calculated and found to be 0.4825 and 1.4621 μg/ml; respectively.Conclusion: The proposed method can help research studies, quality control and routine analysis with lesser resources available. The results of the assay of pharmaceutical formulation of the developed method are highly reliable and reproducible and is in good agreement with the label claim of the medicines.Keywords: Bisoprolol, High-Performance Liquid Chromatography, Validation, ICH guidelines

scholarly journals Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

2015 ◽  
Vol 2015 ◽  
pp. 1-9 ◽  
Author(s):  
Małgorzata Dołowy ◽  
Alina Pyka
Keyword(s):  
Silica Gel ◽  
Mobile Phase ◽  
Research Study ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Simple Economic

This research study describes the applicability of silica gel 60 RPW18F254plates for the development and validation of new, simple, economic, accurate, and precise RPHPTLC-densitometric method suitable for the quantification of nicotinamide (asVitamin PP) in three marketed preparations. The mobile phase used was methanol-water in volume composition 3 : 7. Detection wavelength was 200 nm. The proposed method was validated according to ICH guidelines and also based on Ferenczi-Fodor and Konieczka reports. Results were found to be linear over a range of 1.00 to 2.00 μg/spot. Limit of detection (LOD) and limit of quantification (LOQ) were 0.15 μg/spot and 0.45 μg/spot, respectively. The percent content of nicotinamide in the investigated preparations was found to be 99.2% (Product 1), 99.3% (Product 2), and 99.4% (Product 3). Developed method is accurate and precise (CV<3%) and may be successfully applied for the quality control of pharmaceutical formulations containing nicotinamide in the presence of its derivatives, such as N,N-diethylnicotinamide, N-methylnicotinamide, and nicotinic acid.

scholarly journals Optimization and validation of an RP-HPLC method for the estimation of 6-mercaptopurine in bulk and pharmaceutical formulations

2014 ◽  
Vol 50 (4) ◽  
pp. 793-797 ◽  
Author(s):  
Vanita Somasekhar
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Rp Hplc ◽  
Accuracy And Precision

A reverse phase HPLC method is described for the determination of 6-mercaptopurine in bulk and tablets. Chromatography was carried on a C18 column using a mixture of acetonitrile and 0.05 mol/L sodium acetate buffer (10:90 v/v) as the mobile phase at a flow rate of 1 mL/min-1 with detection at 324 nm. The retention time of the drug was 3.25 min. The detector response was linear in the concentration of 0.01-5 μg/mL. The limit of detection and limit of quantification were 17 and 52 ng/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of mercaptopurine in bulk and tablets.

scholarly journals A simple HPLC method containing greener modifier and slighter temperature elevated for simultaneous determination of three statin drugs in tablets

2021 ◽  
Author(s):  
Wael Alshitari ◽  
Fatimah Al-Shehri ◽  
Deia Abd El-Hady ◽  
Hassan M. Albishri
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Optimal Conditions ◽  
Limit Of Quantification ◽  
Column Temperature ◽  
Pharmaceutical Tablets ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Statin Drugs

AbstractStatins drugs are thought to be among the most prescribed drugs worldwide for the treatment of hypercholesterolaemia. A simple and reliable RP-HPLC method has been successfully employed for simultaneously separating and qualifying three statin drugs including atorvastatin, rosuvastatin and simvastatin in pharmaceutical tablets. The optimal conditions were mobile phase 50:50 (v/v) (formic acid pH 2.50: ETOH), column temperature 40.00 °C, detection wavelength 238.00 nm, and flow rate 1.00 mL/min. The proposed method has been validated based on the ICH guidelines in terms of linearity, precision, accuracy, and limit of detection and limit of quantification. The linear range investigated 2.0–80.0, 4.0–100.00, and 12.00–120.00 µg/mL for rosuvastatin, atorvastatin and simvastatin respectively with coefficients of determination (R2) within the range of 0.9993–0.9995. The LOD and LOQ for rosuvastatin, atorvastatin and simvastatin were (1.57, 4.76 µg/mL), (1.87, 5.66 µg/mL), (3.46, 10.49 µg/mL) respectively. In addition, in order to evaluate the feasibility of the method developed, it was employed towards the quantification of the pharmaceutical tablets for the analytes investigated and excellent recovery was obtained.

scholarly journals Validated LC Method for the Estimation of Dorzolamide HCl (Carbonic Anhydrase Inhibitor) in Ophthalmic Solutions

2012 ◽  
Vol 9 (3) ◽  
pp. 1238-1243 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Eye Drops ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Ich Guidelines ◽  
Ophthalmic Solutions ◽  
Isocratic Mode

A reverse phase HPLC method is described for the determination of Dorzolamide in eye drops. Chromatography was carried on an Inertsil ODS 3V column using Acetonitrile : (0.02M) 1,Octane Sulphonic acid buffer (pH 3.5) (36:64 v/v) on isocratic mode at a flow rate of 1 mL/min with UV detection at 254 nm. The detector response was linear in the concentration range 4-720 µg/mL. The limit of detection and limit of quantification are found to be 0.7041 and 2.3483 µg/mL respectively. The method was validated as per the ICH guidelines. The proposed method is rapid, accurate and precise and can be applied for the routine analysis of dorzolamide in ophthalimic solutions.

Quality by Design (QbD) Approach to Develop and Validate a HPLC Method for Piroxicam from Serum

2018 ◽  
Vol 69 (8) ◽  
pp. 2167-2171 ◽  
Author(s):  
Adrian Florin Spac ◽  
Alina Monica Miftode ◽  
Iuliean Vasile Asaftei ◽  
Ion Sandu
Keyword(s):  
Detection Limit ◽  
Hplc Analysis ◽  
Quality By Design ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Mobile Phases ◽  
Ich Guidelines ◽  
Precision And Accuracy

Piroxicam belongs to the non-steroidal antiinflammatory class, it is utilized as analgesic, anti-inflammatory and antipyretic. A simple and accurate HPLC method was optimized and validated in the QbD approach, for the determination of piroxicam in serum. The optimization of HPLC analysis was performed using different columns, mobile phases and flows. The HPLC method was appropriately validated for linearity, limit of detection, limit of quantification, precision and accuracy in accordance with the ICH guidelines. The optimized and validated method proved to be simple, precise, and accurate, and can be successfully applied for the determination of piroxicam in serum.

scholarly journals Quantitative determination and validation of ethylhexylglycerin using Gas chromatography method

2018 ◽  
Vol 9 (1) ◽  
pp. 30
Author(s):  
Rambabu Arla ◽  
Srinivasa Rao J ◽  
Kailasam Koumaravelou
Keyword(s):  
Chromatographic Method ◽  
Limit Of Detection ◽  
Pharmaceutical Formulations ◽  
Stability Studies ◽  
Limit Of Quantification ◽  
Chromatography Method ◽  
Ich Guidelines ◽  
Clear Peak ◽  
Gas Chromatographic Method

Ethylhexylglycerin, an alkyl glyceryl ether, used in various cosmetics and deodorants is also known to have anti-microbial activity and hence used as an adjuvant along with other preservatives to produce synergistic effect. In the present study, a gas chromatographic method has been employed and validated to determine the presence of impurities along with ethylhexylglycerin. A column having the dimension of DB-1 30m x 0.32mm; 0.25µm with acetone as solvent was found to be optimal for the ideal separation of ethylhexylglycerin from its impurities. Injection volume was set to 1 µl and temperature was maintained at 240°C. A clear peak was observed with the retention time of 8.002 minutes. As per ICH guidelines, the developed method was validated with respect to specificity, sensitivity, Limit of detection, Limit of quantification, linearity, precision, and also stability studies. As per the method, it shows a good correlation co-efficient (R2) value of 0.999 within the concentration range of 0.1- 0.75µg. Therefore, a gas chromatographic method was proposed which can be precise, specific and can be employed for the determination of ethylhexylglycerin in various pharmaceutical formulations. Keywords: Ethylhexylglycerin; Adjuvant; ICH guidelines; Validation; Stability studies

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