scholarly journals Development and Validation of a Diethyl Phosphite Content in Foscarnet Sodium USP by GC MS Technique

2021 ◽  
pp. 192-201
Author(s):  
Mohan Bhatale ◽  
Neelakandan Kaliyaperumal ◽  
Gopalakrishnan Mannathusamy ◽  
Gurunathan Ramalingam
Keyword(s):  
Dosage Forms ◽  
Control Mode ◽  
Internal Diameter ◽  
Diethyl Phosphite ◽  
Separation Flow ◽  
Total Flow ◽  
Total Flow Rate ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Chromatographic Mass

A simple, rapid, selective, and reproducible Gas chromatographic mass spectrometry (GC-MS) method has been developed and validated for the estimation of Diethyl Phosphite content in Foscarnet Sodium USP Drug substance. The drugs were estimated using HP-5, Length-30 M, Internal diameter 0.32 mm; Film thickness 1 μ at a total flow rate of 11.9 ml/min, and column flow of 1.49 ml/min was used for the separation. Flow control mode was pressure. Column oven temperature 70°C and injector temperature 220°C. Oven program modified for proper elution of peak. The linearity range used was 0.025-0.120µg/ml and (Rt) was 6.7 min. The correlation coefficient values were found to be 0.997. Precession studies showed % RSD values less than 15.0% for all the selected concentrations. The percentage recovery of Diethyl phosphite from LOQ to 150% was found in range of 100.7 -116.7%. The content results of Phophite content were within the limits of less than 0.12 ppm. The method was validated as per the International Conference on Harmonization (ICH) guidelines. The developed method was successfully used for the quantitative analysis of commercially available dosage forms.

DEVELOPMENT AND VALIDATION OF RP-HPLC-PDA METHOD FOR THE ESTIMATION OF SARPOGRELATE HYDROCHLORIDE IN BULK AND DOSAGE FORMS

INDIAN DRUGS ◽  
2018 ◽  
Vol 55 (04) ◽  
pp. 77-80
Author(s):  
M Vijaya Lakshmi ◽  
◽  
K Hima Bindu ◽  
M. Pravallika ◽  
B. N. Nalluri
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Control Analysis ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Anti Platelet Drug ◽  
Sarpogrelate Hydrochloride ◽  
The Mean ◽  
Development And Validation

A simple and precise RP-HPLC method has been developed and validated for the estimation of sarpogrelate hydrochloride, an anti-platelet drug in bulk and pharmaceutical dosage forms. Sarpogrelate is an antagonist at 5HT2A and 5HT2B receptors which blocks serotonin induced platelet aggregation and has application in the treatment of diseases including diabetes mellitus, Raynaud’s disease, angina pectoris and atherosclerosis. Chromatography was carried out on a Phenomenex C18 (250 x 4.6mm, 5μm) column with a mobile phase of 10mM ammonium acetate and acetonitrile (45:55% v/v). The flow rate was 1.2mL/min. The detection wavelength was carried out at 220nm. The retention time is 3.356 minutes for sarpogrelate hydrochloride. The linearity was found in the range of 10-50 μg/ml (R = 0.999) and % RSD is less than 2%. The mean recoveries obtained for sarpogrelate hydrochloride were in the range of 98.73-100.67%. The method is validated as per ICH guidelines and can be applied for the estimation of percentage purity in Sarpogrelate hydrochloride for quality control analysis in bulk and its dosage forms.

scholarly journals Development and Validation of Stability Indicating RP-HPLC Method for the Estimation of Cinacalcet Hydrochloride in Bulk and Their Formulations

2020 ◽  
Vol 10 (6) ◽  
pp. 6610-6618
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Cinacalcet Hydrochloride ◽  
Development And Validation ◽  
Tablet Dosage

A Simple, selective, accurate, precise, linear, and stability-indicating RP-HPLC method was developed and validated for the estimation of Cinacalcet hydrochloride in bulk and tablet dosage forms. Chromatographic separation was achieved on X-Terra Symmetry C18 (4.6 x 150mm; 5 m) with mobile phase containing Phosphate buffer: Acetonitrile (40:60 v/v) pH adjusted to 3.0 ±0.05 with diluted ortho-phosphoric acid. The flow rate was maintained at 0.9 mL/min. The eluent was monitored at 282 nm. Moreover, the retention time of Cinacalcet was 2.8 minutes. The method was validated for linearity, accuracy, precision, and robustness as per ICH guidelines. The developed method was found linear between 25-150 μg/ml, and the linear regression coefficient was 0.999. The % RSD values are less than 2 % indicating the accuracy and precision of the method. The percentage of recovery was obtained from 98-102%. The system suitability parameters were found to be within the limit. Forced degradation studies were conducted under various conditions. The proposed method is simple, rapid, precise, and accurate. It can be used for the quantitation of Cinacalcet hydrochloride in bulk and commercial pharmaceutical dosage forms.

DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR ESTIMATION OF EDOXABAN TOSYLATE IN TABLET DOSAGE FORMS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (07) ◽  
pp. 47-51
Author(s):  
B. Anupama ◽  
P. Tejaswi ◽  
KNV. Chenchu Lakshmi ◽  
A. Vishwanadh
Keyword(s):  
High Performance ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Hplc Method ◽  
Control Analysis ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage ◽  
Isocratic Mode

A rapid, simple and precise reversed phase high performance liquid chromatography (RP-HPLC) method was developed for the estimation of edoxabantosylate in tablets. The quantification was carried out using a Phenomenex C-18 column (250×4.6 mm i.d., 5µm particle size) in isocratic mode with mobile phase comprising of ammonium acetate buffer andacetonitrile in the ratio of 50:50 (V/V) at a flow rate 1 mL/min. The eluent was monitored at 240 nm. The retention time of the drug was 3.486 min. The calibration curve was linear in the concentration range of 5-25 µg/mL and per cent recovery ranged from 98.25-101.6.The developed method was validated as per ICH guidelines and the results obtained were satisfactory.The method can be applied for routine quality control analysis of edoxabantosylate in tablet dosage forms.

Development and validation of Stability-indicating RP-UPLC Method for the Simultaneous Determination of Ivacaftor, Tezacaftor and Elexacaftor in bulk and their Formulation

2021 ◽  
Vol 25 (12) ◽  
pp. 107-115
Author(s):  
V.V.S.S.N. Raju Sri Datla ◽  
Manikandan Ayyar
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
Drug Product ◽  
Dosage Forms ◽  
Combination Drug ◽  
Ultraviolet Detection ◽  
Stability Indicating ◽  
Ich Guidelines ◽  
Development And Validation

A simple reproducible stability indicating RP-UPLC method was developed for the simultaneous determination of Ivacaftor, Tezacaftor and Elexacaftor in their combined dosage forms using HSS C18, 1.8μm, 100mm x2.1 mm i.d. column. A mobile phase of phosphate buffer (10mM) pH-4.8 and acetonitrile in the ratio of 70: 30v/v mixture was used for separation and quantification of ivacaftor, tezacaftor and elexacaftor. The present drug analytes were run at a flow-rate of 0.3ml/ min at 30°C temperature. The injection volume was 2μL and with ultraviolet detection at 270nm. Under these conditions, elexacaftor, ivacaftor and tezacaftor were eluted at 0.72min, 1.4min and 1.9min respectively with a total run time shorter than 5min. The developed method was validated according to International Conference on Harmonization (ICH) guidelines. The developed RP-UPLC method was applied successfully for quality control assay of Ivacaftor, Tezacaftor and Elexacaftor in their combination drug product.

scholarly journals Development and validation of new analytical method for the simultaneous estimation of ibuprofen and diphenhydramine in bulk and pharmaceutical dosage form by RP-HPLC

2018 ◽  
Vol 1 (1) ◽  
pp. 13-17
Author(s):  
V Pavan Kumar ◽  
T Supriya ◽  
B Sivagami ◽  
R Sireesha ◽  
R Charan Kumar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Control Analysis ◽  
Pharmaceutical Dosage Form ◽  
Quality Control Analysis ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

A simple, accurate, rapid and precise method was developed for the simultaneous estimation of Ibuprofen and Diphenhydramine in Pharmaceutical dosage form. Chromatogram was run through Inertsil ODS (250x4.6mm) 5µ. Mobile phase used was Acetonitrile and Phosphate buffer (45:55) at a flow rate of 1.0 ml/min and detection wavelength was found to be 260 nm. The retention time was found to be 2.32 min and 2.93 min for Ibuprofen and Diphenhydramine respectively. The accuracy and reliability of the method was assessed by evaluation of linearity, precision (intra-day and inter-day % RSD >2), accuracy (98-102%), specificity, LOD, LOQ values in accordance with ICH guidelines. The developed method is applicable for routine quality control analysis of selected combined dosage forms.

scholarly journals Development and Validation of a Versatile UPLC-PDA Method for Simultaneous Determination of Paracetamol, Tizanidine, Aceclofenac, and Nimesulide in Their New Combinations

2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Sami Bawazeer ◽  
Khalid M. Badr El-Din ◽  
Ahmed M. Abdel-Megied
Keyword(s):  
Limit Of Detection ◽  
Dosage Forms ◽  
New Combination ◽  
Development Method ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Acquity Uplc ◽  
Development And Validation ◽  
Tablet Dosage

A simple, rapid, and validated UPLC method was developed for the simultaneous quantitation of paracetamol (PAR), tizanidine (TIZ), aceclofenac (ACF), and nimesulide (NIM) either in pure forms or in their different tablet dosage forms. Chromatographic separation was attained on an ACQUITY UPLC™ BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with a mobile phase consisting of 20 mM phosphate buffer (pH 7.0) : acetonitrile in the proportion (60 : 40 v/v) isocratically pumped at a flow rate of 1.25 mL·min−1, and detection was monitored at 305 nm. All analytes were separated simultaneously at a retention time (tr) of 1.42, 2.31, 3.63, and 5.62 min for PAR, TIZ, ACF, and NIM, respectively, with a total run time less than 6.0 min. The proposed method was validated according to ICH guidelines with respect to accuracy, precision, linearity, limit of detection, limit of quantitation, and robustness. Linearity was obtained over a concentration range of 81.25–487.5, 0.5–3.5, 25–150, and 25–150 µg·mL−1 for PAR, TIZ, ACF, and NIM, respectively. The development method can be successfully employed in QC laboratories for the routine analysis of the investigated drugs in their new combination.

scholarly journals Development and Validation of UV-Spectrophotometric Method for Estimation of Metformin Hydrochloride and Pioglitazone in Tablet Dosage Form

2019 ◽  
Vol 9 (4-A) ◽  
pp. 381-384
Author(s):  
Rupali S. Joshi ◽  
Ajit K. Nangare ◽  
Deepali S. Sanap ◽  
Surekha M. Sase
Keyword(s):  
Dosage Form ◽  
Estimation Method ◽  
Pharmaceutical Formulations ◽  
Dosage Forms ◽  
Dual Wavelength ◽  
Metformin Hydrochloride ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

Simple, sensitive, rapid and accurate UV spectroscopic methods have been developed for the estimation of metformin hydrochloride and pioglitazone in tablet dosage forms. Simultaneous estimation and dual-wavelength methods were developed and validated using solvent methanol. Both drugs show linearity at 5-40 µg/ml for both methods. The suggested techniques have been effectively implemented in pharmaceutical formulations to the evaluation of quoted drugs. Recovery research was conducted to verify the method's accuracy, precision. The techniques have been validated under ICH guidelines. Keywords: Metformin hydrochloride, Pioglitazone, Simultaneous estimation method and Dual wavelength method.

scholarly journals Development and validation of RP HPLC method for the estimation of Sofosbuvir and related impurity in bulk and pharmaceutical dosage form

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Shiny Ganji ◽  
Satyavati Dhulipala ◽  
Appala Raju Nemala
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Extensive Literature ◽  
Uv Detector ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Relative Standard ◽  
Development And Validation

Abstract Background The present work is aimed at development and validation of RP HPLC method which is simple, specific, precise, and accurate for estimation of Sofosbuvir and its process-related impurity in bulk and pharmaceutical dosage forms. Extensive literature survey revealed no method for estimation of the above said. The chromatographic separation was achieved on Agilent Eclipse XDB-C18, 4.6 × 250 mm, 5 μm with mobile phase composed of 0.1% trifluoroacetic acid in 1000 ml of water:acetonitrile (50:50) using an isocratic mode of elution. Detection was made using UV detector at 260.0 nm and LC solution software for analysis of data. The developed method was validated according to ICH guidelines. Results The linearity of calibration curve for Sofosbuvir in concentration range of 160-480 μg/ml was good. The curve was linear for its process related impurity (Phosphoryl) in concentration range of 10-30 μg/ml. There exists a good correlation between peak area and analyte concentration. Retention time for Sofosbuvir was found to be 3.674 min and its impurity was 5.704 min. Relative standard deviation values for Sofosbuvir is 1.741 and its process related impurity is 0.043. LOD for Sofosbuvir and its impurity was found to be 0.01% (0.04 μg) and 0.03% (0.12 μg) respectively. LOQ for Sofosbuvir and its impurity was found to be 0.50% (0.125 μg) and 1.50% (0.375 μg) respectively. Conclusion All the results reveal that the proposed method was found to be highly sensitive, simple, precise, accurate, robust, and fast. Large number of samples can be analyzed in shorter time due to shorter retention times, so it can be successfully applied for routine analysis of Sofosbuvir and related phosphoryl impurity in bulk and pharmaceutical dosage forms.

Development and validation of an HPLC method for five gliptins in pharmaceutical dosage forms in finished marketed products

2020 ◽  
Vol 17 ◽  
Author(s):  
Zainab Alkather ◽  
Mohammad Hailat ◽  
Ramadan Al-Shdefat ◽  
Wael Abu Dayyih
Keyword(s):  
Flow Rate ◽  
Analytical Method ◽  
Drug Dosage ◽  
Dosage Forms ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Inactive Ingredients ◽  
Development And Validation

Background:: Metformin is the most used antihyperglycemic drug in diabetes, and therefore it is preferred to be combined with other classes of antihyperglycemic drugs, specially gliptins. Formulating of these two classes of drug in one pharmaceutical dosage form would be more efficacious to control hyperglycemia than having either drug alone. Objective:: This study was designed and performed to develop a new, simple, and reliable method of analysis for assaying simultaneously five types of gliptins (Alogliptin, Linagliptin, Saxagliptin, Sitagliptin and Vildagliptin) and Metformin which has not been documented before. Methods:: The present method was carried out using a C18 column (250x4.6 mm), 5μm particle size, mobile phase consisting of water to acetonitrile ratio 85:15% (v/v) and the pH was set by orthophosphoric acid at 3, 10 μl injection volume, 0.5 ml flow rate, 25oC temperature and the eluent was monitored at 232 nm. Results:: The selectivity of the assay showed no interference with inactive ingredients in the formulation, and the %recovery from each drug dosage forms at three different concentrations were within the acceptable limits of the ICH guidelines. Although the method showed robustness towards flow rate, it showed significant change at 230 or 234 nm. Conclusion: The present analytical method is comprehensive and universal for measuring the five drugs and Metformin. Such an analytical method can be applied to the present available combined drug dosage forms of Metformin and one type of gliptins and the possible future of triple combinations of two gliptins and Metformin.

scholarly journals Development and validation of new analytical method for the simultaneous estimation of omeprazole and domperidone in pharmaceutical dosage form by UV spectrophotometry

2019 ◽  
Vol 1 (2) ◽  
pp. 44-46
Author(s):  
V. Pavan Kumar ◽  
C. Bhanu Chandra ◽  
N. Devendra ◽  
M. Kishor Kumar ◽  
S. Reddy Basha ◽  
...  
Keyword(s):  
Dosage Form ◽  
Simultaneous Equation ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Development And Validation

A simple, rapid and precise method was developed for the quantitative simultaneous determination of Omeprazole and Domperidone in combined pharmaceutical-dosage forms. The method was based on UV-Spectrophotometric determination of two drugs, using simultaneous equation method. It involves absorbance measurement at 291 nm (λmax of Omeprazole) and 289 nm (λmax of Domperidone) in Methanol: Acetonitrile (30:70 v/v). For UV Spectrophotometric method, linearity was obtained in concentration range of 1-15 µg/ml for Domperidone and 1-50 µg/ml for Omeprazole respectively, with regression 0.999 and 0.999 for Domperidone and Omeprazole respectively. Recovery was in the range of 99 -103%; the value of standard deviation and %R.S.D were found to be < 2 %; shows the high precision of the method., in accordance with ICH guidelines. The method has been successively applied to pharmaceutical formulation and was validated according to ICH guidelines.

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