scholarly journals Ultra performance liquid chromatographic method for simultaneous quantitation of degradation products of telmisartan and hydrochlorothiazide in combination dosage form

2020 ◽  
Vol 11 (2) ◽  
pp. 2070-2082
Author(s):  
Narasimha Reddy G P ◽  
Sreenivasulu Reddy T ◽  
Sidda Reddy K ◽  
Shashi Kumar K N
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Drug Product ◽  
Wave Length ◽  
Stability Study ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating

This work is intended to thrive a stability indicating Ultra performance liquid method for the estimation of (TLM) and (HCTZ) and degradation products pharmaceutical dosage forms. Separation was carried out on Zorbax Eclipse XDB C-18(50 x 2.1 mm, 1.7 ) column using a gradient method. Mobile phase A is 10mM KH2PO4 having 1% (v/v) of and mobile phase B is used in this work. 0.5 / minute is the flow of rate and at 271nm noticed wave length is monitored. Method development trails were carried out on six different columns. For specificity, limit of quantification, limit of detection, linearity, accuracy, method precision, robustness and stability this method is validated. Correlation coefficient of the impurities is more than 0.99. Stability indicating method confirmed that there were no interference of all impurities of TLM and HCTZ. Hence, developed LC method was stability indicating and well applied for drug product stability study as well as to quality monitoring.

scholarly journals LC-MS characterization of acid degradation products of metoclopramide: Development and validation of a stability-indicating RP-HPLC method

2020 ◽  
Vol 11 (1) ◽  
pp. 781-789
Author(s):  
Sriram Valavala ◽  
Nareshvarma Seelam ◽  
Subbaiah Tondepu ◽  
Suresh Kandagatla
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Hplc Technique

The present study aims to develop a simple, accurate and specific stability-indicating RP-HPLC technique for the analysis of metoclopramide in the presence of its stress degradation products and characterization of degradation compounds by LC-MS/MS analysis. As per ICH Q1A-R2 guidelines, the drug was exposed to acid hydrolytic stress condition. Three degradation products were formed for MCP in acid hydrolysis. The liquid chromatography was processed on a Luna C18-(2) 100A,250×4.6mm 5micron column using an isocratic mobile phase consisting of 0.1% formic acid in water-acetonitrile (20:80, v/v) by adjusting the mobile phase at 1 ml/min flow rate with wavelength detection at 273 nm. The developed procedure was applied to LC-MS/MS (liquid chromatography-tandem mass spectrometry) for the characterization of all the degradant components. Total new three degradation compounds were recognized and identified by LC-MS/MS. The developed RP-HPLC technique was validated as per the ICH Q2-R1 guidelines. Limit of detection and limit of quantification values of MCP were evaluated from the linearity graph and were found to be 5.23 µg/ml and 17.44 µg/ml. Accuracy study was established at 80.0, 100.0 and 120.0 µg/ml concentration levels and the findings were found in the range of 98.4% - 101.8%. The linearity of the technique was assessed over the drug concentration range of 50.0 µg/ml to 250.0 µg/ml and the regression equation, slope and correlation coefficient values were found to be y = 10618x + 1623.2, 10618 and 0.9996 respectively. The developed technique was uninterruptedly applied for the quantification of metoclopramide inactive pharmaceuticals.

METHOD DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC AND STABILITY INDICATING RP-HPLC METHODS FOR SIMULTANEOUS ESTIMATION OF MOXIFLOXACIN HYDROCHLORIDE AND KETOROLAC TROMETHAMINE IN BULK AND OPTHALMIC DOSAGE FORMS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (04) ◽  
pp. 38-46
Author(s):  
H Parimi ◽  
C Bolla ◽  
B. M. Gandhi ◽  
B. R Vatchavai ◽  
S. S Kamatham ◽  
...  
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Dosage Forms ◽  
Simultaneous Estimation ◽  
Uv Spectrophotometry ◽  
Ketorolac Tromethamine ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Rp Hplc

The main objective of the present work was to develop a simple, precise, accurate and reproducible UV-Spectrophotometric and stability indicating RP-HPLC methods for simultaneous estimation of moxifloxacin HCl (MOX) and ketorolac tromethamine (KET) in bulk and ophthalmic dosage forms. UV Spectrophotometry was carried out by simultaneous equation method using distilled water : acetonitrile (50:50 V/V) as solvent. The wavelengths were found to be 295 nm for MOX and 322 nm for KET. The isobestic point was found to be 308 nm. The linearity range is 2-10 μg/mL for both MOX and KET with correlation co-efficient >0.99. The separation of these two drugs using RP-HPLC was achieved on a SHISHEDO C18, 250×4.6 mm, 5 micron size column with a mobile phase consisting of acetonitrile and acetate buffer (45:55 V/V) at pH 4.0 at a flow rate of 1 mL/min and UV detection at 308 nm. The retention times were observed to be 2.418 and 3.827 minutes for MOX and KET, respectively. Linearity was found to be 10-50 μg/mL for both MOX and KET, respectively. The two developed methods were successfully validated for accuracy, precision, linearity, limit of detection, limit of quantification and robustness. The two developed methods were validated according to ICH guidelines and were found to be with in the limits. The stress testing of the drugs individually was carried out under acidic, alkaline, oxidation, photo-stability and thermal degradation conditions and its degradation products were studied. These two methods could be used for simultaneous estimation of MOX and KET in bulk and ophthalmic dosage forms.

scholarly journals METHOD DEVELOPMENT AND VALIDATION OF NORETHINDRONE ACE-TATE ASSAY AND ITS RELATED IMPURITIES IN API AND PHARMACEUTICAL FORMULATION WITH ORTOGONAL DETECTOR TECHNQUES

2017 ◽  
Vol 9 (12) ◽  
pp. 110
Author(s):  
J. Satish ◽  
P. Radhakrishnanand ◽  
K. Surendra Babu
Keyword(s):  
Method Development ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Water Solution ◽  
Pharmaceutical Formulation ◽  
Acetonitrile Solution ◽  
Reverse Phase ◽  
Limit Of Quantification ◽  
Stability Indicating ◽  
Organic Impurities

Objective: To develop and validate a sensitive and stability indicating gradient reverse phase ultra-high performance(UHPLC-PDA) liquid chromatography with photodiode array(PDA) and mass spectroscopy (MS) of Norethindrone Acetate (NA) assay and organic impurities (OI) in active pharmaceutical Ingredient(API) and Pharmaceutical Formulation (PF).Methods: The chromatographic conditions were optimized using Zorbax SB-C18 analytical UHPLC column with the dimensions (100 x 2.1) mm and 1.8 μm particle sizes. The mobile phase consisted of water (solution A) and acetonitrile (solution B) with gradient elution as mentioned time (min)/% Solution B: Initial/40,0.2/40, 9.2/55,12.0/55,12.2/90,15.5/90, 15.8/40 and 18.0/40. The flow rate was at the rate of 0.4 ml/min and the detection wavelengths were 254 nm and 210 nm. The column was kept at 40 °C and the injection volume was 5 μL. Stability of NA sample in different conditions was investigated by exposing the drug to stress study utilizing acid, base, oxidation, thermal, Humidity and photolytic.Results: There was no interference from excipients, impurities or degradation products at the retention time of NA about 9.1 min indicating the specificity of the method.The drug showed good stability under oxidation, thermal, humidity and photolytic conditions, but significant degradation was observed under acid and base conditions. The procedure was validated for specificity, linearity, accuracy, precision and robustness. The degradation products were well resolved from NA and its impurities. The obtained LOD (Limit of detection) values are 0.001% to 0.015% and LOQ (Limit of quantification) values are 0.003% to 0.05% of impurities.Conclusion: A sensitive, rapid, specific and stability indicating gradient Reverse Phase UHPLC-PDA-PDA with MS (Orthogonal detectors) method for the determination of NA for the assay and organic impurities was successfully developed. The developed method was validated to be specific, linear, accurate, precise and robust. The peak purity and LC-MS test results confirmed that the NA peak was homogenous in all stress samples and the mass balance was found to be more than 99%, thus proving the stability indicating power of the method

Development and Validation of a Stability-Indicating HPTLC Method for the Estimation of Eszopiclone in Pharmaceutical Dosage Forms

2021 ◽  
Vol 11 (3) ◽  
pp. 219-223
Author(s):  
Vidhya K. Bhusari ◽  
Sunil R. Dhaneshwar
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Limit Of Quantitation ◽  
Stress Degradation ◽  
Bulk Drug ◽  
Hptlc Method

Objective: A simple, sensitive, selective, precise repeatable and stability-indicating high-performance thin layer chromatographic method was developed and validated for Eszopiclone in bulk drug and in formulation. Method: Silica gel 60 F-254, TLC precoated aluminium plates was used as the stationary phase for analyzing Eszopiclone and its degradation products, using mobile phase consisting toluene: ethyl acetate: methanol (6: 4: 2 v/v/v). Result: This mobile phase gave compact spots for Eszopiclone with Rf value of 0.52 ± 0.02. Eszopiclone was exposed to hydrolysis, oxidation, neutral and photolytic conditions for conducting stress degradation study. The peak of Eszopiclone and the degradation product was well resolved from each other with a significantly different Rf value. Densitometric estimation of Eszopiclone was performed at 304nm. A good linear plot was obtained in the concentration range of 150-300ng/spot. The method was validated for precision, accuracy (recovery) and robustness study. The limit of detection (LOD) and limit of quantitation (LOQ) was found to be 130ng/spot and 150ng/spot, respectively. Conclusion: The developed HPTLC method can separate Eszopiclone from its degradation products, hence stability studies can be performed using this method.

scholarly journals New Stability Indicating Method for Quantification of Impurities in Amlodipine and Valsartan Tablets by Validated HPLC

2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Rama Joga Venkata Eranki ◽  
Gopichand Inti ◽  
Venkatasubramanian Jayaraman ◽  
Sudhakar Rao Vidiyala ◽  
J. SreeRamulu
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Drug Product ◽  
Thermal Studies ◽  
Pharmaceutical Preparations ◽  
Stability Study ◽  
Combination Drug ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Stability Indicating

A stability indicating LC method was developed for simultaneous determination of amlodipine and valsartan in pharmaceutical dosage form. Efficient chromatographic separation was achieved on C8 stationary phase with simple combination of mobile phase-A (70 : 20 : 10 v/v/v of water : acetonitrile : methanol with 2 mL of Octylamine adjusted the pH to 2.50 + 0.05 with orthophosphoric acid) and mobile phase-B (Acetonitrile) delivered in gradient mode. Quantification was carried out using ultraviolet detection at 240 nm at flow rate of 1.0 mL/min with Injection Volume of 100 μL and ambient column temperature. This method was capable to detect both the drug components of Amlodipine and Valsartan in presence of their degradation products (Amlodipine Imp-A and Valsartan Impurity-B) with the detection level of 0.05%. Amlodipine/Valsartan and their combination drug product were exposed to thermal studies, photolytic, hydrolytic and oxidative stress conditions, and samples analysed. Peak homogeneity data of Amlodipine and Valsartan is obtained using PDA detector, demonstrating the specificity. The method shows excellent linearity over range of 0.05–2.0% for Amlodipine; Amlodipine Impurity-A and 0.05–1.0% for Valsartan and Valsartan Impurity-B. The correlation coefficient for Amlodipine and Valsartan are 0.9999. The proposed method was found to be suitable and accurate for quantitative determination and the stability study of Amlodipine and Valsartan in pharmaceutical preparations.

scholarly journals Development and validation of stability indicating RP-HPLC method for the determination of related substances in Raloxifene hydrochloride tablets dosage forms

2019 ◽  
Vol 10 (4) ◽  
pp. 3325-3331
Author(s):  
Babu C ◽  
Suresh Reddy K.V.N ◽  
Shashi Kumar K.N
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Dosage Forms ◽  
Limit Of Quantification ◽  
Intermediate Precision ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Related Substances ◽  
Raloxifene Hcl

This work is intended to thrive a stability-indicating high performance liquid chromatographic method for the analysis of Raloxifene HCl related compounds in pharmaceutical dosage forms. The separation was achieved Inertsil C8 (150 x 4.6 mm ID, 3.5μm)column using a gradient method. Mobile phase A is 0.01M KH2PO4 buffer (pH4.5), and mobile phase B is acetonitrile used in this work. 1.0 mL/ minute is the flow of rate and at 280nm noticed wavelength is monitored. For specificity, the limit of quantification, the limit of detection, linearity, accuracy, method precision, intermediate precision, robustness and stability this method is validated. The six injection impurities of standard solutions at the 4.0 µg/mL conjecture concentration were confirmed experimentally for LOQ values. The correlation coefficient of the impurities is more than 0.99. All impurities meet the criteria for linearity of both the impurities and raloxifene. The RSD recoveries obtained for impurities are not more than 10%. The achievement of this study demonstrated that the method is selective, linear, precise, rugged, robust and stability-indicating for the determination of related substances in raloxifene HCl tablet dosage form.

scholarly journals A Validated New Gradient Stability-Indicating LC Method for the Analysis of Doripenem in Bulk and Injection Formulation

2013 ◽  
Vol 2013 ◽  
pp. 1-9
Author(s):  
Singaram Kathirvel ◽  
Garikapati Devalarao
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Active Pharmaceutical Ingredient ◽  
Hplc Method ◽  
Array Detector ◽  
Limit Of Quantification ◽  
Mobile Phase Flow Rate ◽  
Phase Gradient ◽  
Stability Indicating

A sensitive, precise, specific, linear, and stability-indicating gradient HPLC method was developed for the estimation of doripenem in active pharmaceutical ingredient (API) and in injectable preparations. Chromatographic separation was achieved on C18 stationary phase with a mobile phase gradient consisting of acetonitrile, methanol, and pH 5.2 phosphate buffer. The mobile phase flow rate was 0.8 mL/min, and the eluted compounds were monitored at 210 nm. The method is linear over the range of 0.335 to 76.129 µg/mL. The correlation coefficient was found to be 0.999. The numbers of theoretical plates and tailing factor for doripenem were 53021 and 0.9, respectively. Doripenem was subjected to the International Conference on Harmonization (ICH) prescribed hydrolytic (acid, base, and neutral), oxidative, photolytic, and thermal stress conditions. Among all the above-mentioned conditions, the drug was found to be stable under photolytic degradation. Peak homogeneity data for doripenem in the chromatograms from the stressed samples obtained by use of the photodiode array detector demonstrated the specificity of the method for analysis of doripenem in presence of the degradation products. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, and robustness.

scholarly journals Validated stability-indicating method for estimation of related substances of paroxetine in active pharmaceutical ingredient and its pharmaceutical dosage forms

2020 ◽  
Vol 11 (4) ◽  
pp. 8004-8011
Author(s):  
Surapuraju Pavan Kumar Raju ◽  
Raveendra Reddy J
Keyword(s):  
Mobile Phase ◽  
Method Development ◽  
Degradation Products ◽  
Drug Stability ◽  
Active Pharmaceutical Ingredient ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Stress Studies ◽  
Related Substances ◽  
Stability Indicating Method

Validated stability-indicating analytical method was established for the quantitative determination of paroxetine and its related substances in API and it’s finished product in the presence of degradation products. To prove the stability-indicating nature of the method, stress studies were carried out. The method was developed by using (Waters, symmetry C18, 250×4.6 mm, 5 μm column) employing water:THF: TFA 90:10:1 (v/v/v) as mobile phase-A and mobile phase-B consist of ACN:THF: TFA the proportion of 90:10:1 (v/v/v) in a gradient mode with a flow rate of 1.5 mL/min was chosen. The column and sample cooler were kept at 45°C and 5°C respectively and 285 nm used as detection wavelength. Significant degradation observed in alkaline conditions, whereas no signification decay in drug stability was observed in other decomposition environments. Method development as well as optimisation studies were done by analysing the samples generated in the stress studies and spiked samples. Mass balance was found to be in the range of 90.3 and 100.1%, signifying the method is stability-indicating. All earlier analysis methods for the analysis of paroxetine have not been entirely validated by considering all the degradation products. The established method validated as per ICH Q2 (R1) and considered as linear, specific, accurate, precise, rugged, robust and found to be suitable for the routine and stability analysis of the product.

STABILITY INDICATING UPLC METHOD FOR ESTIMATION OF METFORMIN HYDROCHLORIDE AND NATEGLINIDE SIMULTANEOUSLY IN THE PRESENCE OF STRESS DEGRADATION PRODUCTS

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (05) ◽  
pp. 56-64
Author(s):  
Rani A Prameela ◽  
S. Madhavi ◽  
Rao B. Tirumaleswara ◽  
Sudheer Reddy CH.
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Metformin Hydrochloride ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Column Temperature

A novel Ultra Performance Liquid Chromatography (UPLC) method was developed and validated for the simultaneous determination of antidiabetic drugs metformin hydrochloride and nateglinide. The method was developed using a Waters ACQUITY UPLC SB C18 (100 × 2.1 mm, 1.8 μm) column. The mobile phase consisting of 0.01 % potassium dihydrogen phosphate buffer (pH 5.8): acetonitrile (50: 50 V/V) was used throughout the analysis. The flow rate was 0.3 mL/min, the injection volume was 1.0 μL, column temperature was 30 0C, run time 3 min and detection was carried at 238 nm using a TUV detector. The retention times of metformin hydrochloride and nateglinide were found to be 1.28 1.71 min, respectively. Metformin hydrochloride and nateglinide were found to be linear over the concentration range of 125-750 and 15-90 μg/mL. The limit of detection and the limit of quantification for metformin hydrochloride were found to be 0.22 and 0.68 μg/mL, respectively, and, for nateglinide, 0.02 and 0.6 μg/mL, respectively. Developed method was validated as per ICH guidelines. The specificity of the method was confirmed by forced degradation study. The suggested method is suitable for determination of metformin hydrochloride and nateglinide in bulk and pharmaceutical dosage forms.

scholarly journals Photostability study of amlodipine besylate tablets packed in primary packaging

2021 ◽  
Vol 10 (1) ◽  
pp. 20-28
Author(s):  
Ivana Savić-Gajić ◽  
Ivan Savić ◽  
Predrag Sibinović ◽  
Valentina Marinković
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Coefficient Of Determination ◽  
Amlodipine Besylate ◽  
Limit Of Quantification ◽  
First Order Kinetics ◽  
The Given

In this study, the modified stability-indicating RP-HPLC method was validated for quantitative analysis of amlodipine besylate in the presence of its impurity D (3-ethyl 5-methyl 2-[(2-aminoethoxy)methyl]-4-(2-chlorophenyl)-6-methylpyridine-3,5-dicarboxylate). The method was applied for the determination of an analyte in the tablets and irradiated samples packed in the primary packaging (Alu/PVC/PVDC blister packaging). The efficient chromatographic separation was achieved using a ZORBAX Eclipse XDB-C18 column (4.6×250 mm, 5 mm) with isocratic elution of mobile phase which consisted of acetonitrile:methanol:triethylamine solution (15:35:50, v/v/v) (pH 3.0). The flow rate of the mobile phase was 1 mL min-1, while the detection of amlodipine besylate was carried out at 273 nm. Amlodipine besylate and its impurity D were identified at the retention times of 16.529 min and 2.575 min, respectively. The linearity of the method with the coefficient of determination of 0.999 was confirmed in the concentration range of 10 - 75 µg mL-1 for amlodipine besylate. The limit of detection was 0.2 µg mL-1, while the limit of quantification was 0.66 µg mL-1. After UV and Vis radiation of the tablets packed in the primary packaging, the content of amlodipine besylate was reduced by 22.38% and 19.89%, respectively. The presence of new degradation products was not detected under the given chromatographic conditions. The photodegradation of amlodipine besylate followed pseudo-first-order kinetics. Based on the half-life of amlodipine besylate (38.4 days for UV radiation and 43.3 days for Vis radiation), it was concluded that amlodipine besylate in the tablets has satisfactory photostability after its packing in the Alu/PVC/PVDC blister packaging.

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