scholarly journals Development and Validation of a Novel Stability-Indicating Reversed-Phase Ion-Pair Chromatographic Method for the Quantitation of Impurities in Marbofloxacin Tablets

2018 ◽  
Vol 101 (4) ◽  
pp. 1021-1029
Author(s):  
Priyanka Maheshwari ◽  
Neelima Shukla ◽  
Manish Kumar Dare
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Reversed Phase ◽  
Ion Pair ◽  
Stress Conditions ◽  
Main Peak ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
The Stability

Abstract A stability-indicating isocratic reversed-phase ion-pair chromatographic method was designed for the separation of impurities in the presence of degradation products. Marbofloxacin tablets and a placebo were exposed to the stress conditions of oxidative, acid, base, humidity, thermal, and photolytic degradation. Significant and moderate degradation was observed in acidic and oxidative stress conditions, respectively. The degradation products were well resolved from the main peak and its impurities, thus proving the stability-indicating analytical method. The method was developed by using an XTerra RP18 3.5 μm (150 × 4.6 mm) column, with the mobile phase containing a mixture of buffer (pH 2.5)–methanol–glacial acetic acid (77 + 23 + 0.5, v/v). The flow rate of the mobile phase was 1.2 mL/min, with a column oven temperature of 40°C and a detection wavelength of 315 nm. The proposed method met Veterinary International Conference on Harmonization requirements and was successfully used for impurity quantitation in marbofloxacin tablets.

scholarly journals Development and Validation of a Stability-Indicating RP-HPLC Method for the Simultaneous Estimation of Guaifenesin and Dextromethorphan Impurities in Pharmaceutical Formulations

2013 ◽  
Vol 2013 ◽  
pp. 1-12 ◽  
Author(s):  
Thummala V. Raghava Raju ◽  
Noru Anil Kumar ◽  
Seshadri Raja Kumar ◽  
Annarapu Malleswara Reddy ◽  
Nittala Someswara Rao ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photolytic Degradation ◽  
The Stability

A sensitive, stability-indicating gradient RP-HPLC method has been developed for the simultaneous estimation of impurities of Guaifenesin and Dextromethorphan in pharmaceutical formulations. Efficient chromatographic separation was achieved on a Sunfire C18, 250 × 4.6 mm, 5 µm column with mobile phase containing a gradient mixture of solvents A and B. The flow rate of the mobile phase was 0.8 mL min−1 with column temperature of 50°C and detection wavelength at 224 nm. Regression analysis showed an r value (correlation coefficient) greater than 0.999 for Guaifenesin, Dextromethorphan, and their impurities. Guaifenesin and Dextromethorphan formulation sample was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal, and photolytic degradation. Guaifenesin was found stable and Dextromethorphan was found to degrade significantly in peroxide stress condition. The degradation products were well resolved from Guaifenesin, Dextromethorphan, and their impurities. The peak purity test results confirmed that the Guaifenesin and Dextromethorphan peak was homogenous and pure in all stress samples and the mass balance was found to be more than 98%, thus proving the stability-indicating power of the method. The developed method was validated according to ICH guidelines with respect to specificity, linearity, limits of detection and quantification, accuracy, precision, and robustness.

scholarly journals Stability-indicating HPLC determination of ciprofibrate in bulk drug and pharmaceutical dosage form

2012 ◽  
Vol 18 (1) ◽  
pp. 95-101 ◽  
Author(s):  
P.S. Jain ◽  
H.N. Jivani ◽  
R.N. Khatal ◽  
S.J. Surana
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Reversed Phase ◽  
Stress Conditions ◽  
Assay Method ◽  
Main Peak ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

A novel stability-indicating high-performance liquid chromatographic assay method was developed and validated for quantitative determination of ciprofibrate in bulk drugs and in pharmaceutical dosage form in the presence of degradation products. An isocratic, reversed phase HPLC method was developed to separate the drug from the degradation products, using an Ace5-C18 (250?4.6 mm, 5 ?m) advance chromatography column, and methanol and water (90:10 v/v) as a mobile phase. The detection was carried out at a wavelength of 232 nm. The ciprofibrate was subjected to stress conditions of hydrolysis (acid, base), oxidation, photolysis and thermal degradation. Degradation was observed for ciprofibrate in base, in acid and in 30% H2O2. The drug was found to be stable in the other stress conditions attempted. The degradation products were well resolved from the main peak. The percentage recovery of ciprofibrate was from (98.65 to 100.01%) in the pharmaceutical dosage form. The developed method was validated with respect to linearity, accuracy (recovery), precision, system suitability, specificity and robustness. The forced degradation studies prove the stability indicating power of the method.

scholarly journals Stability-Indicating Reversed-Phase Liquid Chromatographic Method for Simultaneous Determination of Simvastatin and Ezetimibe from Their Combination Drug Products

2007 ◽  
Vol 90 (5) ◽  
pp. 1242-1249 ◽  
Author(s):  
Bharat G Chaudhari ◽  
Natvarlal M Patel ◽  
Paresh B Shah
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Drug Product ◽  
Reversed Phase ◽  
Stress Conditions ◽  
Simultaneous Estimation ◽  
Combination Drug ◽  
Mobile Phase Flow Rate ◽  
Stability Indicating ◽  
Liquid Chromatographic

Abstract A simple, precise, and rapid stability-indicating reversed-phase column liquid chromatographic (RP-LC) method has been developed and subsequently validated for simultaneous estimation of simvastatin (SIM) and ezetimibe (EZE) from their combination drug product. The proposed RP-LC method utilizes a LiChrospher 100 C18, 5 m, 250 4.0 mm id column at ambient temperature; optimum mobile phase consisting of acetonitrilewatermethanol (60 + 25 + 15, v/v/v) with apparent pH adjusted to 4.0 0.1; mobile phase flow rate of 1.5 mL/min; and ultraviolet detection at 238 nm. SIM, EZE, and their combination drug product were exposed to thermal, photolytic, hydrolytic, and oxidative stress conditions, and the stressed samples were analyzed by the proposed method. There were no other coeluting, interfering peaks from excipients, impurities, or degradation products due to variable stress conditions, and the method is specific for the estimation of SIM and EZE in the presence of degradation products. The described method was linear over the range of 180 and 380 g/mL for SIM and EZE, respectively. The mean recoveries were 99.17 and 100.43 for SIM and EZE, respectively. The intermediate precision data were obtained under different experimental conditions, and the calculated value of the coefficient of variation was found to be less than the critical value. The proposed method can be useful in the quality control of bulk manufacturing and pharmaceutical dosage forms.

scholarly journals Analysis of some pharmaceuticals in the presence of their synthetic impurities by applying hybrid micelle liquid chromatography

2020 ◽  
Vol 18 (1) ◽  
pp. 377-390
Author(s):  
Dina El Sherbiny ◽  
Mary E. K. Wahba
Keyword(s):  
Liquid Chromatography ◽  
Sodium Dodecyl Sulfate ◽  
Phosphoric Acid ◽  
Mobile Phase ◽  
Sodium Dodecyl ◽  
Uv Detection ◽  
Stability Indicating ◽  
Photolytic Degradation ◽  
Amino Phenol ◽  
The Stability

AbstractA stability-indicating hybrid micelle liquid chromatography accompanied by UV detection was developed for the simultaneous analysis of either paracetamol (PCA) or pseudoephedrine hydrochloride (PSU) with their synthetic impurities. Mixture I contains PCA with p-amino phenol and p-nitro phenol, while mixture II involves the estimation of PSU with benzaldehyde and benzoic acid. Both mixtures were separated using a C18 column that was thermostatically maintained at 40°C and operating under a flow rate of 1.5 mL/min, applying UV detection at 240 nm for mixture I and 220 nm for mixture II. In both cases, the mobile phase consisted of 0.1 M sodium dodecyl sulfate, acetonitrile, and triethylamine (90:10:0.3, v/v/v) and adjusted to pH 4 (mixture I) or pH 3.7 (mixture II) using 2.0 M O-phosphoric acid. The proposed method was validated and successfully applied to assay different pharmaceuticals containing PCA or PSU. Moreover, the stability-indicating nature of the proposed method was proved through applying photolytic degradation procedures for PCA.

scholarly journals Studies on Paliperidone in OROS Tablets: Extraction Procedure and Chromatographic Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Fábio Barbosa ◽  
Luciano Mantovani ◽  
Cássia V. Garcia ◽  
Andreas S. L. Mendez
Keyword(s):  
Oral Delivery ◽  
Degradation Products ◽  
Extraction Procedure ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Phase System ◽  
Stability Indicating ◽  
Ultrasonic Bath ◽  
The Stability ◽  
Liquid Chromatographic

A stability-indicating liquid chromatographic (LC) method was studied for the determination of paliperidone in osmotic-controlled release oral delivery system (OROS) tablets. A tablet extraction procedure was developed by testing the efficiency of solvents (water, HCl, NaOH, acetonitrile, methanol) and techniques (ultrasonic bath, magnetic stirrer), and evaluating the release of the drug with respect to time. A forced degradation study was conducted to demonstrate the stability-indicating power of the method. Chromatographic separation was achieved using an isocratic elution in a reversed-phase system with a mobile phase prepared from a mixture of phosphate buffer and acetonitrile. The use of an ultrasonic bath demonstrated paliperidone release from OROS tablets in a total time of 60 min. Verifying the efficiency of the chromatographic procedure, the theoretical plates (N=12634.21) and tailing factor (tf=1.31) were constant during repeated injections. The retention time of paliperidone was 4.8 min, and the method was validated within the concentration range of 10–50 μg mL-1 (r=0.9999). Adequate reproducibility (RSD% = 0.30–0.59), interday precision (RSD%=1.81), and accuracy were obtained. The proposed method was successfully applied to paliperidone determination in the presence of degradation products, and an efficient extraction procedure from the OROS tablets was developed.

scholarly journals Development of a Stability-Indicating High-Performance Liquid Chromatographic Method for the Simultaneous Determination of Alprazolam and Sertraline in Combined Dosage Forms

2008 ◽  
Vol 91 (6) ◽  
pp. 1344-1353 ◽  
Author(s):  
Ashutosh Pathak ◽  
Sadhana J Rajput
Keyword(s):  
High Performance ◽  
Chromatographic Method ◽  
Degradation Products ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Dosage Forms ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Abstract The objective of the current study was to develop a validated stability-indicating high-performance liquid chromatographic method for alprazolam and sertraline in combined dosage forms. The method was validated by subjecting the drugs to forced decomposition under hydrolysis, oxidation, photolysis, and thermal stress conditions prescribed by the International Conference on Harmonization. The drugs were successfully separated from major and minor degradation products on a reversed-phase C18 column by using 75 mM potassium dihydrogen phosphate buffer (pH 4.3)acetonitrilemethanol (50 45 5, v/v/v) as the mobile phase with determination at 227 nm. The flow rate was 0.9 mL/min. The method was validated with respect to linearity, precision, accuracy, system suitability, and robustness. The responses were linear over the ranges of 180 and 5200 g/mL for alprazolam and sertraline, respectively. The recoveries of both drugs from a mixture of degradation products were in the range of 97101. The utility of the procedure was verified by its application to marketed formulations that were subjected to accelerated stability studies. The method distinctly separated the drugs and degradation products, even in actual samples. The products formed in marketed tablets were similar to those formed during stress studies.

A new stability indicating chiral RP-HPLC method for determination of degradation products in Meclizine Hydrochloride

2020 ◽  
Vol 16 ◽  
Author(s):  
Bryan Gowramma ◽  
Ramachandran Senthil Kumar ◽  
Kaviarasan Lakshmanan ◽  
Rajagopal Kalirajan ◽  
Subramanian Nainar Meyyanathan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Stress Conditions ◽  
Main Peak ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Degradation Behaviour ◽  
Stability Indicating

Background: An enantiomeric separation of stability-indicating high-performance liquid chromatographic method was developed and validated for the analysis of Meclizine enantiomers. The degradation behaviour of Meclizine Hydrochloride was investigated under different stress conditions recommended by International Conference on Harmonization (ICH). Experiment: Enantiomeric resolution of the drug and complete separation from its degradation products were successfully achieved on a Phenomenex® lux cellulose 1 C18 (250 mm × 4.6 mm i.d, 5 µm particle size) column, using UV detector at a wavelength of 230 nm, with mobile phase consisting of acetonitrile, 20mM ammonium bicarbonate at the ratio of 75:25 (v/v), and a flow rate of 1 mL/min. The drug was subjected to alkaline, acidic, neutral, oxidative and photolytic conditions in order to mimic stress conditions. Result: The degradation products were well resolved from main peak and proving the stability-indicating power of the method. The developed method provided linear responses within the concentration range 1-5 µg/mL, and regression analysis showed a correlation coefficient value (r2) of 0.999. The HPLC method was validated as per ICH guidelines with respect to specificity, precision, linearity and robustness. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.25 µg/mL and 1.00 µg/mL respectively. Conclusion: The method provides good sensitivity and excellent precision and reproducibility. The method was highly selective, where degradation products and co formulated compounds did not interfere. The proposed method was successfully applied in pharmaceutical preparations.

scholarly journals Development of Stability Indicating RP-HPLC Method for Ertapenem in Bulk Drug and Pharmaceutical Dosage Form

2017 ◽  
Vol 16 (1) ◽  
pp. 21-28
Author(s):  
Ruchi Jain ◽  
Nilesh Jain ◽  
Deepak Kumar Jain ◽  
Avineesh Singh ◽  
Surendra Kumar Jain
Keyword(s):  
Dosage Form ◽  
Degradation Products ◽  
Hplc Method ◽  
Stress Conditions ◽  
Assay Method ◽  
Main Peak ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Bulk Drug

A simple, inexpensive, rapid and novel stability indicating isocratic HPLC method has been developed and validated for quantitative analysis of ertapenem sodium in the bulk drug and in pharmaceutical dosage form. An isocratic separation of ertapenem sodium was achieved on Hypersil BDS C18 column (4.6 x 250 mm, 5 ? particle size) as the stationary phase with a flow rate of 1.2 ml/min and using a UV detector to monitor the eluate at 298 nm. The mobile phase consisted of acetonitrile : water (60:40v/v) and pH adjusted 2.9 by othophosphoric acid enabled separation of the drug from its degradation products. The method was validated for linearity, accuracy (recovery), precision, specificity and robustness. The linearity of the method was satisfactory over the range 2-10 ?g/ml (correlation coefficient 0.999). Recovery of ertapenem sodium from the pharmaceutical dosage form ranged from 99.97 to 103.7%. Ertapenem sodium was subjected to stress conditions [hydrolysis (acid, base), oxidation, photolysis and thermal degradation] and the samples were analyzed by this method. The forceddegradation study with ertapenem sodium showed that it was degraded under basic condition. The drug was stable under the other stress conditions investigated. Ertapenem sodium was found to be less stable in solution state, whereas it was comparatively much stable in solid state. The degradation products were well resolved from main peak. The forced degradation study prove the stability indicating power of the method and therefore, the validated method may be useful for routine analysis of ertapenem sodium as bulk drug, in respective dosage forms, for dissolution studies and as stability indicating assay method in pharmaceutical laboratories and industries.Dhaka Univ. J. Pharm. Sci. 16(1): 21-28, 2017 (June)

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

Sign in / Sign up

Export Citation Format

Share Document