Development and Validation of Stability-indicating Reverse Phase HPLC Assay for Tramadol in Bulk and Tablet Formulations

2019 ◽  
Vol 12 (3) ◽  
pp. 4544-4552
Author(s):  
Pankaj Padmakar Nerkar ◽  
Vaishali Badjuar ◽  
Pradyum Ige ◽  
Hitendra Mahajan ◽  
Sameer Ansari
Keyword(s):  
Orthophosphoric Acid ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Ich Guidelines ◽  
Tablet Formulations ◽  
Development And Validation

This manuscript describes the development and validation of a simple, isocratic, and accurate reversed-phase HPLC method for the assay of tramadol in bulk powder form and tablet formulations. The chromato-graphic separation was achieved on an Qualisil BDS C18 (250 mm x 4.6mm, 5μm) column using acetonitrile: methanol: phosphate buffer pH 3.4 adjusted with orthophosphoric acid: (20:10:70, v/v) as a mobile phase, at a flow rate of 1 mL/min and detection at 271 nm. The linear range for tramadol were 2.0 to 10 μg/mL was obtained with correlation coefficients ≥ 0.999. The retention time was found to be 4.47 min for tramadol that was subjected to stress conditions, such as hydrolysis, oxidation, photolysis and thermal degradation, and the stressed samples were analyzed using the above methodology. The method was validated for the precision, accuracy, linearity and robustness. The developed stability-indicating method for tramadol was validated as per ICH guidelines.

Development and Validation of Stability Indicating RP-HPLC Method for Determination of Enzalutamide

2019 ◽  
Vol 12 (5) ◽  
pp. 4635-4645
Author(s):  
Pankaj Padmakar Nerkar ◽  
Sameer Ansari ◽  
Shailesh Chalikwar
Keyword(s):  
Ammonium Acetate ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation

A simple, isocratic, and accurate reversed phase HPLC method was developed for the quantitative determination of enzalutamide. The chromatographic separation was achieved on an Qualisil BDS C18 (250 mm x 4.6mm, 5 μm) column using methanol: ammonium acetate buffer pH 4.2 adjusted with glacial acetic acid: (60:40, v/v) as a mobile phase, at a flow rate of 1 ml/min and detection at 236nm. The linear range for enzalutamide were 2.0 to        10 μg/mL was obtained with correlation coefficients ≥ 0.998. The retention time was found to be 6.30min. Enzalutamide was subjected to stress conditions hydrolysis (acid, base) oxidation, photolysis and thermal degradation and the stressed samples were analysed by the developed method. The method was validated for the precision, accuracy, linearity and robustness. The developed stability indicating method for enzalutamide was validated as per ICH guidelines.

scholarly journals Development and Validation of an HPLC Stability-Indicating Method for Identification and Assay of Elemental Iron(II) in Pharmaceutical Drug Products Using Reversed-Phase HPLC

2011 ◽  
Vol 94 (4) ◽  
pp. 1233-1239
Author(s):  
Neil C Dias ◽  
Abu M Rustum
Keyword(s):  
Ferrous Sulfate ◽  
Methanesulfonic Acid ◽  
Reversed Phase ◽  
Hplc Method ◽  
Elemental Iron ◽  
Stability Indicating ◽  
Drug Products ◽  
Stability Indicating Method ◽  
The Matrix ◽  
Development And Validation

Abstract Ferrous sulfate tablets are a supplementary iron source for people who suffer from iron defciency anemia. A simple, fast, and QCfriendly HPLC method was developed and validated to determine elemental iron in ferrous sulfate drug products. A TSK-GEL Super octadecylsilyl column (50 × 4.6 mm id, 2 µm particle size) with a mobile phase consisting of 0.06 M methanesulfonic acid in water–acetonitrile (40 + 60, v/v) and UV detection at 282 nm were used for this method. Separation of the elemental iron peak from the matrix was achieved within 5 min. This method was successfully validated according to International Conference on Harmonization guidelines, and shown to be stability-indicating for the shelf-life samples of ferrous sulfate tablets, as well as selective for the analyte of interest.

DEVELOPMENT AND VALIDATION OF NEW STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF ELBASVIR AND GRAZOPREVIR IN BULK AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (09) ◽  
pp. 53-59
Author(s):  
Girija Dandu ◽  
Basu Venkateswara Reddy
Keyword(s):  
Dosage Form ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Hplc Grade Water ◽  
Development And Validation

The present study describes the development and validation of a new stability indicating RP-HPLC method for simultaneous estimation of elbasvir and grazoprevir in bulk and pharmaceutical dosage form. The chromatographic separation was done by using reverse phase YMC column (4.6 x 250mm, 5μm).The mobile phase used was mixture of HPLC grade water acetonitrile (70:30V/V) at flow rate of 1ml/ min in isocratic mode and detection was carried out using PDA detector at 244nm.The developed method showed a good linearity in the range of 100-500μg/mL for elbasvir and 200-1000 μg/mL for grazoprevir with regression co-efficient of 0.999 for both the drugs. The % recovery of drugs was found to be 100.1% for elbasvir and 100.38% for grazoprevir. The proposed stability indicating method was accurate, precise, robust, stable and specific. The developed method was validated in accordance with ICH guidelines.

scholarly journals Development and Validation of a Stability-Indicating HPLC Method for the Simultaneous Determination of Florfenicol and Flunixin Meglumine Combination in an Injectable Solution

2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Nidal Batrawi ◽  
Hani Naseef ◽  
Fuad Al-Rimawi
Keyword(s):  
Simultaneous Determination ◽  
Reversed Phase ◽  
Hplc Method ◽  
Base Hydrolysis ◽  
Water Mixture ◽  
Stability Indicating ◽  
Stability Indicating Method ◽  
Flunixin Meglumine ◽  
Development And Validation

The combination of the powerful antimicrobial agent florfenicol and the nonsteroidal anti-inflammatory flunixin meglumine is used for the treatment of bovine respiratory disease (BRD) and control of BRD-associated pyrexia, in beef and nonlactating dairy cattle. This study describes the development and validation of an HPLC-UV method for the simultaneous determination of florfenicol and flunixin, in an injectable preparation with a mixture of excipients. The proposed RP-HPLC method was developed by a reversed phase- (RP-) C18e (250 mm × 4.6 mm, 5 μm) column at room temperature, with an isocratic mobile phase of acetonitrile and water mixture, and pH was adjusted to 2.8 using diluted phosphoric acid, a flow rate of 1.0 mL/min, and ultraviolet detection at 268 nm. The stability-indicating method was developed by exposing the drugs to stress conditions of acid and base hydrolysis, oxidation, photodegradation, and thermal degradation; the obtained degraded products were successfully separated from the APIs. This method was validated in accordance with FDA and ICH guidelines and showed excellent linearity, accuracy, precision, specificity, robustness, LOD, LOQ, and system suitability results within the acceptance criteria.

scholarly journals Development and Validation of RP-HPLC Method for Simultaneous Estimation of Aspirin and Esomeprazole Magnesium in Tablet Dosage Form

2013 ◽  
Vol 2013 ◽  
pp. 1-5 ◽  
Author(s):  
Dipali Patel ◽  
Nishitkumar Patel ◽  
Reeta Vaishy ◽  
Viral Patel ◽  
Chiragsinh Solanki ◽  
...  
Keyword(s):  
Dosage Form ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Ich Guidelines ◽  
The Mean ◽  
Esomeprazole Magnesium ◽  
Development And Validation ◽  
Tablet Dosage

A simple, specific, precise, and accurate reversed-phase HPLC method was developed and validated for simultaneous estimation of aspirin and esomeprazole magnesium in tablet dosage forms. The separation was achieved by HyperChrom ODS-BP C18column (200 mm × 4.6 mm; 5.0 μm) using acetonitrile: methanol: 0.05 M phosphate buffer at pH 3 adjusted with orthophosphoric acid (25 : 25 : 50, v/v) as eluent, at a flow rate of 1 mL/min. Detection was carried out at wavelength 230 nm. The retention times of aspirin and esomeprazole magnesium were 4.29 min and 6.09 min, respectively. The linearity was established over the concentration ranges of 10–70 μg/mL and 10–30 μg/mL with correlation coefficients (r2) 0.9986 and 0.9973 for aspirin and esomeprazole magnesium, respectively. The mean recoveries were found to be in the ranges of 99.80–100.57% and 99.70–100.83% for aspirin and esomeprazole magnesium, respectively. The proposed method has been validated as per ICH guidelines and successfully applied to the estimation of aspirin and esomeprazole magnesium in their combined tablet dosage form.

scholarly journals Method Development and Validation of Gemifloxacin in Tablet Dosage Form by RP-HPLC

2020 ◽  
Vol 10 (4) ◽  
pp. 97-101
Author(s):  
Mithun Rudrapal ◽  
Nazim Hussain
Keyword(s):  
Dosage Form ◽  
Method Development ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Forms ◽  
Average Percentage ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Development And Validation ◽  
Tablet Dosage

A simple, precise and accurate RP-HPLC method was developed and validated for the estimation of gemifloxacin in the tablet dosage form. The separation was achieved on a reversed-phase C-18 column (250 x 4.6 mm i.d., 5 µm) using a mobile phase consisting of acetonitrile/acetate buffer of pH 4.5 (70:30 v/v) at a flow rate of 1.0 ml/min and a detection wavelength of 244 nm. The separation was carried out on an isocratic mode at room temperature. The method was validated as per ICH guidelines for linearity, accuracy, precision, robustness, LOD, LOQ and specificity. The developed method showed good linearity over the concentration range of 50-150 µg/ml (r2=0.995). The average percentage recovery was 99.77%. The LOD and LOQ were 12.678 µg/ml and 14.261 µg/ml, respectively. Based upon validation studies, the developed method can be successfully applied for the routine analysis of gemifloxacin in bulk drugs as well as pharmaceutical dosage forms. Keywords: Gemifloxacin, Tablet dosage form, RP-HPLC, Validation, ICH guidelines

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.

scholarly journals Validated Stability Indicating Chromatographic Methods for Quantification of Imidocarb Dipropionate; Application for the Determination of Its Residues in Bovine Meat and Milk Samples

2020 ◽  
Vol 103 (4) ◽  
pp. 980-988
Author(s):  
Ghada AbdElHamid Sedik ◽  
Doha Mohamed Naguib ◽  
Fahima Morsy ◽  
Hala Elsayed Zaazaa
Keyword(s):  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Stability Indicating ◽  
Milk Samples ◽  
Chromatographic Methods ◽  
Ich Guidelines ◽  
Imidocarb Dipropionate ◽  
Tlc Plates

Abstract Background Imidocarb dipropionate (IMD) is an immunomodulator agent commonly used for treatment of anaplasmosis in cattle. Objective Thus, two sensitive, specific, and precise stability-indicating chromatographic methods have been developed, optimized, and validated for its determination in presence of its acid, alkaline, and oxidative stressed degradation products. Method The first method is based on separation of IMD and its forced induced degradation products on reversed phase cyano column using isocratic elution system consisted of sodium acetate buffer–methanol–acetonitrile (55: 30:15, v/v/v), pH 4.6 at a flow rate of 1.2 mL/min, and UV detection at 254 nm. The second method utilized TLC combined with densitometric determination of the separated bands at 254 nm. The separation was achieved using silica gel 60 F254 TLC plates with a mixture of ethyl acetate–methanol–ammonia–water (8.5:1:0.5:0.2, v/v/v/v) as a developing system. Results HPLC analysis was applied in range of 0.25–40 µg/mL with LOD of 0.073 µg/mL. While densitometric measurements showed linearity in the range of 0.1–1.8 µg/band with LOD of 0.02 µg/band. Conclusions The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for determination of IMD in its commercial veterinary formulations with good recoveries. Furthermore, the proposed HPLC method was extended to the determination of IMD residues in bovine meat and milk samples Highlights Bovine meat, HPLC, Imidocarb dipropionate, Milk, TLC.

Development and Validation of Stability Indicating RP-HPLC Method for Estimation of Voriconazole in Bulk Drug

2010 ◽  
Vol 3 (2) ◽  
pp. 978-986
Author(s):  
Wamorkar V V ◽  
C S Ramaa ◽  
Manjunath S Y ◽  
V Malla Reddy
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Good Resolution ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Bulk Drug ◽  
Development And Validation ◽  
Different Levels

RP-HPLC method has been developed and validated for the determination of voricaonazole in bulk drug. The developed method is found to be specific, reproducible, and stability indicating. The Hypersil, C18 (250 X 4.6 mm) 5μ column was used and mobile phase consisting of water:acetonitrile to achieve good resolution and retention of the analyte and its impurities. The detector linearity was established from concentrations ranging from 5-100 μg/ml. The method was tested at different levels of specificity and accuracy as per requirements given in ICH guidelines. The molecule was exposed to the stress conditions such as acid, base, oxidation, heat and light as per the recommendations of ICH guidelines. The method was proved to be robust with respect to changes in flow rate, mobile phase composition and allied columns. The proposed method is found to be sensitive, precise, rapid, reproducible, and offers good column life.

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