scholarly journals A Rapid Stability-Indicating RP-HPLC Method for the Determination of Betaxolol Hydrochloride in Pharmaceutical Tablets

2013 ◽  
Vol 8 ◽  
pp. ACI.S11256 ◽  
Author(s):  
Sylvain Auvity ◽  
Fouad Chiadmi ◽  
Salvatore Cisternino ◽  
Jean-Eudes Fontan ◽  
Joël Schlatter
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

A stability-indicating reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of betaxolol hydrochloride, a drug used in the treatment of hypertension and glaucoma. The desired chromatographic separation was achieved on a Nucleosil C18, 4 μm (150 × 4.6 mm) column, using isocratic elution at a 220 nm detector wavelength. The optimized mobile phase consisted of a 0.02 M potassium dihydrogen phosphate: methanol (40:60, v/v, pH 3.0 adjusted with o-phosphoric acid) as solvent. The flow rate was 1.6 mL/min and the retention time of betaxolol hydrochloride was 1.72 min. The linearity for betaxolol hydrochloride was in the range of 25 to 200 μg/mL. Recovery for betaxolol hydrochloride was calculated as 100.01%-101.35%. The stability-indicating capability was established by forced degradation experiments and the separation of unknown degradation products. The developed RP-HPLC method was validated according to the International Conference on Harmonization (ICH) guidelines. This validated method was applied for the estimation of betaxolol hydrochloride in commercially available tablets.

scholarly journals DEVELOPMENT AND VALIDATION OF STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF β-ACETYLDIGOXIN

2016 ◽  
Vol 9 (1) ◽  
pp. 54
Author(s):  
Megha Sharma ◽  
Neeraj Mahindroo
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Hplc Method ◽  
Stability Study ◽  
Array Detector ◽  
Forced Degradation ◽  
Simple Method ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The objective of the present study was to develop and validate a novel stability indicating reverse phase-high performance liquid chromatography (RP-HPLC) method for determination of β-acetyldigoxin, an active pharmaceutical ingredient (API).Methods: The chromatographic separation was carried out on Agilent Technologies 1200 series HPLC system equipped with photo diode array detector and C-18 (4.6x250 mm, 5 µ) column. The mobile phase consisted of water: acetonitrile (65:35 v/v), delivered at a flow rate of 1.5 ml/min and eluents were monitored at 225 nm.Results: The retention time of β-acetyldigoxin was 9.2 min. The method was found to be linear (R2= 0.9995) in the range of 31.25-500 µg/ml. The accuracy studies showed the mean percent recovery of 101.02%. LOD and LOQ were observed to be 0.289 µg/ml and 0.965 µg/ml, respectively. The method was found to be robust and system suitability testing was also performed. Forced degradation analysis was carried out under acidic, alkaline, oxidative and photolytic stress conditions. Significant degradation was observed under tested conditions, except for oxidative condition. The method was able to separate all the degradation products within runtime of 20 min and was able to determine β-acetyldigoxin unequivocally in presence of degradation products.Conclusion: The novel, economic, rapid and simple method for analysis of β-acetyldigoxin is reported. The developed method is suitable for routine quality control and its determination as API, and in pharmaceutical formulations and stability study samples.

scholarly journals STABILITY INDICATING RP-HPLC METHOD DEVELOPMENT AND VALIDATION FOR THE SIMULTANEOUS DETERMINATION OF VILDAGLIPTIN AND METFORMIN IN PHARMACEUTICAL DOSAGE FORM

2017 ◽  
Vol 9 (3) ◽  
pp. 150
Author(s):  
Ramesh Jayaprakash ◽  
Senthil Kumar Natesan
Keyword(s):  
High Performance ◽  
Method Development ◽  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Rp Hplc

Objective: The present study was aimed to develop a rapid, accurate, linear, sensitive and validate stability-indicating high performance liquid chromatographic [RP-HPLC] method for determination of vildagliptin and metformin in pharmaceutical dosage form.Methods: The chromatographic separation was performed on kromasil-C18 column [4.5 x 250 mm; 5 µm] using a mobile phase consisting of 0.05 mmol potassium dihydrogen phosphate buffer: acetonitrile [80:20 v/v], [pH adjusted to 3.5 using orthophosphoric acid]. The flow rate is 0.9 ml/min and the detection was carried out at 263 nm.Results: The chromatographic condition, the peak retention time of metformin and vildagliptin were found to be 2.215 min and 2.600 min respectively. Stress testing was performed in accordance with an international conference on harmonization [ICH] Q1A R2 guidelines. The method was validated as per ICH Q2 R1 guidelines. The calibration curve was found to be linear in the concentration range of 5-17.5 µg/ml and 50-175 µg/ml for vildagliptin and metformin. The limit of detection and quantification was found to be 0.0182 µg/ml and 0.0553 µg/ml for vildagliptin and 0.4451 µg/ml and 1.3490 µg/ml for metformin respectively.Conclusion: A new sensitive, simple and stability indicating reverse-phase high-performance liquid chromatography [RP-HPLC] method has been developed and validated for the determination of vildagliptin and metformin. The proposed method can be used for routine determination of vildagliptin and metformin.

scholarly journals A Stability Indicating UPLC Method for the Determination of Tramadol Hydrochloride: Application to Pharmaceutical Analysis

2012 ◽  
Vol 2012 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura B. Vinay ◽  
Hosakere D. Revanasiddappa ◽  
Cijo M. Xavier ◽  
Pavagada J. Ramesh ◽  
Madihalli S. Raghu
Keyword(s):  
Limit Of Detection ◽  
Potassium Dihydrogen Phosphate ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Uv Detector ◽  
Limit Of Quantification ◽  
Tramadol Hydrochloride ◽  
Stability Indicating

The use of Ultra Performance Liquid Chromatography (UPLC), with a rapid 5-minute reversed phase isocratic separation on a 1.7 μm reversed-phase packing material to provide rapid ‘‘high throughput’’ support for tramadol hydrochloride (TMH) is demonstrated. A simple, precise and accurate stability-indicating isocratic UPLC method was developed for the determination of TMH in bulk drug and in its tablets. The method was developed using Waters Aquity BEH C18 column (100 mm × 2.1 mm, 1.7 μm) with mobile phase consisting of a mixture of potassium dihydrogen phosphate buffer of pH 2.8 and an equal volume of acetonitrile (60 : 40 v/v). The eluted compound was detected at 226 nm with a UV detector. The standard curve of mean peak area versus concentration showed an excellent linearity over a concentration range 0.5–300 μg mL−1 TMH with regression coefficient (r) value of 0.9999. The limit of detection (S/N =3) was 0.08 μg mL−1 and the limit of quantification (S/N =10) was 0.2 μg mL−1. Forced degradation of the bulk sample was conducted an accordance with the ICH guidelines. Acidic, basic, hydrolytic, oxidative, thermal and photolytic degradation were used to assess the stability indicating power of the method. TMH was found to degrade significantly in acidic, basic and oxidative stress conditions and stable in thermal, hydrolytic and photolytic conditions.

Development and Validation of Stability-Indicating HPLC Method for Roflumilast and Related Substances

2013 ◽  
Vol 781-784 ◽  
pp. 68-71 ◽  
Author(s):  
Fang Tan
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Related Substances ◽  
Limit Of Quantitation

A reversed phase HPLC method was developed and validated for analysis of roflumilast, its related substances and degradation products, using Ecosil C18 column (250×4.6 mm, 5 μm) with a flow rate of 1.0 ml/min and detection wavelength of 215nm. The mobile phase was a mixture of acetonitrile and 0.005mol·L-1ammonium dihydrogen phosphate buffer pH 3.5 in the ratio of 48:52 (v/v). The samples were analyzed using 20 μl injection volume and the column temperature was maintained at 30°C. The limit of detection and limit of quantitation were found to be 2.6 ng/ml and 8ng/ml, respectively. The stability-indicating capability of method was established by forced degradation studies and method demonstrated successful separation of drug, its related substances and degradation products. The method is sensitive, specific, accurate, precise and stability indicating for the quantitation of drug, its related substances and other degradation compounds.

scholarly journals Stability-Indicating RP-HPLC Method for Simultaneous Estimation of Enrofloxacin and Its Degradation Products in Tablet Dosage Forms

2015 ◽  
Vol 2015 ◽  
pp. 1-11 ◽  
Author(s):  
V. Ashok Chakravarthy ◽  
B. B. V. Sailaja ◽  
Avvaru Praveen Kumar
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Forced Degradation ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Tablet Dosage

The present work was the development of a simple, efficient, and reproducible stability-indicating reverse-phase high performance liquid chromatographic (RP-HPLC) method for simultaneous determination enrofloxacin (EFX) and its degradation products including ethylenediamine impurity, desfluoro impurity, ciprofloxacin impurity, chloro impurity, fluoroquinolonic acid impurity, and decarboxylated impurity in tablet dosage forms. The separation of EFX and its degradation products in tablets was carried out on Kromasil C-18(250×4.6 mm, 5 μm) column using 0.1% (v/v) TEA in 10 mM KH2PO4(pH 2.5) buffer and methanol by linear gradient program. Flow rate was 1.0 mL min−1with a column temperature of 35°C and detection wavelength was carried out at 278 nm and 254 nm. The forced degradation studies were performed on EFX tablets under acidic, basic, oxidation, thermal, humidity, and photolytic conditions. The degraded products were well resolved from the main active drug and also from known impurities within 65 minutes. The method was validated in terms of specificity, linearity, LOD, LOQ, accuracy, precision, and robustness as per ICH guidelines. The results obtained from the validation experiments prove that the developed method is a stability-indicating method and suitable for routine analysis.

scholarly journals Stability Indicating RP-HPLC for Quantification Mangiferin in Extract of Three Species Mango Leaves

2020 ◽  
Vol 8 (1) ◽  
pp. 15-20
Author(s):  
Yuni Retnaningtyas ◽  
Nia Kristiningrum ◽  
Hidayah Dwi Renggani ◽  
Indah Purnama Sary
Keyword(s):  
High Performance ◽  
Degradation Products ◽  
Mangifera Indica ◽  
Reversed Phase ◽  
Hplc Method ◽  
Complete Separation ◽  
Forced Degradation ◽  
Rp Hplc ◽  
Mango Leaves ◽  
The Stability

The stability indication of Reversed Phase-High Performance Liquid Chromatography (RP-HPLC) method was validated for quantitative determination of mangiferin on three species mango leaves (Mangifera odorata Griff, Mangifera foetida Lour, and Mangifera indica L.). The samples were extracted by maseration method using methanol and concentrated using rotary evaporator. The method carried out on stationary phase a purospher RP-18 endcapped (25 cm × 4.6 mm i.d., 5 µm) column with a mobile phase consisting of methanol: phosphoric acid 0.1% (v/v) (31:69); flow rate:0.8 mL/min; solvent methanol, detection was carried out at 258 nm. The analytical  performace this measurement is good with the value of linearity (r2=0.998), precision (%RSD=0.649%), and accuration (10.67%). The forced degradation studies were carried out according to the International Conference on Harmonization (ICH) guidelines. The results indicating that the complete separation between degradation products and mangiferin peak occured. The degradation limit of mangiferin 5–20% (according to the guideline of ICH) except in basic condition (100%). The method was succesful applied to determine of the mangiferin in  pakel (Mangifera foetida), kweni (Mangifera indica) and kopyor (Mangifera odorata) extract. The mangiferin content was obtained are pakel (9.95%), kopyor (7.40%) and kweni (Mangifera odorata) (2.49%) respectively.

A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR DETERMINATION OF AZELNIDIPINE AND ITS IMPURITIES IN PHARMACEUTICAL FORMULATION

INDIAN DRUGS ◽  
2020 ◽  
Vol 57 (08) ◽  
pp. 70-76
Author(s):  
Pavani Peddi ◽  
S. L. Tulasi ◽  
N. Usha Rani ◽  
T. Raja Rajeswari
Keyword(s):  
Degradation Products ◽  
Impurity Content ◽  
Hplc Method ◽  
Stability Study ◽  
Forced Degradation ◽  
Uv Detector ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Formulation Analysis

A novel simple, rapid, sensitive and stability-indicating RP-HPLC method was developed and validated for the determination of azelnidipine (ALDP) and its impurities 1 and 2. Resolution of drug, its potential impurities and degradation products were achieved by RP-HPLC on was performed on Prontosil ODS C18 column (250 mm x 4.6 mm, 5µ) using a mobile phase consisting of methanol and 0.1M sodium acetate 40: 60 (v/v) at a flow rate of 1 ml/min and 231 nm of UV detector. Validation of the method was performed along with formulation analysis and forced degradation studies. The calibration curves of ALDP were linear over a concentration range of 50-300 µg/mL. The method was rapid with a retention time of the impurity 2, impurity and ALDP observed at 3.60, 5.15 and 6.90 min, respectively. The method was applied for the impurities determination in drug tablets and for degradation products determination in a stability study of ALDP. The impurity content in the tablets was quantified as 0.1% of total drug. The method can also be used for rapid and accurate quantification of ALDP in its tablets during stability testing.

scholarly journals Development and Validation of a Novel Stability-Indicating RP-HPLC Method for Simultaneous Determination of Tezacaftor and Ivacaftor in Fixed Dose Combination

2020 ◽  
Vol 58 (4) ◽  
pp. 346-354
Author(s):  
Narendra Singh ◽  
Parveen Bansal ◽  
Mukesh Maithani ◽  
Yashpal Chauhan
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Fixed Dose ◽  
Simultaneous Estimation ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

Abstract A simple and precise novel stability-indicating method for the simultaneous estimation of tezacaftor and ivacaftor in combined tablet dosage form was developed and validated using reversed-phase high-performance liquid chromatography (RP-HPLC). The method is being reported for the first time and includes an estimation of degradation products produced post-stress conditions without any extraction or derivatization. The chromatographic separation of the drugs was achieved with a Symmetry Shield RP18 Column (100 Å, 5 μm, 4.6 mm × 250 mm) using a mixture of buffer, methanol and acetonitrile (42:27:31 v/v/v) as mobile phase. The buffer used in mobile phase contained 35 mM potassium dihydrogen phosphate, and its pH was adjusted to 7.0 ± 0.02 with 20% orthophosphoric acid. The instrument was set at flow rate of 1.2 mL min−1 at ambient temperature and the wavelength of UV-visible detector at 275 nm. The developed method could be suitable for the quantitative determination of these drugs in pharmaceutical preparations and also for quality control in bulk manufacturing. Stress testing was performed to prove the specificity. No interference was observed from its stress degradation products. The statistical analysis was done by using F-test and t-test at 95% confidence level.

scholarly journals Stability-Indicating RP-HPLC Method for Assay of Silver Lactate

2011 ◽  
Vol 8 (2) ◽  
pp. 483-490
Author(s):  
V. Srinivasan ◽  
H. Sivaramakrishnan ◽  
B. Karthikeyan
Keyword(s):  
Thermal Stress ◽  
Degradation Products ◽  
Potassium Dihydrogen Phosphate ◽  
Hplc Method ◽  
Stress Conditions ◽  
Base Hydrolysis ◽  
Assay Method ◽  
Dihydrogen Phosphate ◽  
Stability Indicating ◽  
Rp Hplc

A simple, economic and time-efficient stability-indicating, reverse-phase high-performance liquid chromatographic (RP-HPLC) method has been developed for analysis of silver lactate in the presence of degradation products generated by decomposition. When silver lactate was subjected to acid hydrolysis, base hydrolysis, oxidative, photolytic, humidity and thermal stress, degradation was observed during base hydrolysis, oxidation, humidity and thermal stress. The drug was found to be stable to other stress conditions. Successful chromatographic condition of the drug from the degradation products formed under stress conditions was achieved on a phenomenex Gemini column with potassium dihydrogen phosphate buffer, pH adjusted to 2.2 with orthophosphoric acid, as mobile phase. The method was validated for linearity, precision, specificity and robustness and can be used for quality-control during manufacture and assessment of the stability of samples of silver lactate. To the best of our knowledge, a validated stability-indicating LC assay method for silver lactate based on lactic acid is reported for the first time.

scholarly journals A Rapid Reversed-Phase HPLC Method for Analysis of Trans-Resveratrol in PLGA Nanoparticulate Formulation

2014 ◽  
Vol 2014 ◽  
pp. 1-6 ◽  
Author(s):  
Gurinder Singh ◽  
Roopa S. Pai
Keyword(s):  
High Performance ◽  
Linear Regression Analysis ◽  
Potassium Dihydrogen Phosphate ◽  
Plga Nanoparticles ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Relative Standard ◽  
New Formulation

A rapid reversed-phase high performance liquid chromatography (RP-HPLC) method was developed for the determination of trans-resveratrol (t-RVT) in PLGA nanoparticle formulation. A new formulation of t-RVT loaded PLGA nanoparticles (NPs) with potential stealth properties was prepared by nanoprecipitation method in our laboratory. The desired chromatographic separation was achieved on a Phenomenex C18 column under isocratic conditions using UV detection at 306 nm. The optimized mobile phase consisted of a mixture of methanol: 10 mM potassium dihydrogen phosphate buffer (pH 6.8): acetonitrile (63 : 30 : 7, v/v/v) at a flow rate of 1 mL/min. The linear regression analysis for the calibration curves showed a good linear correlation over the concentration range of 0.025–2.0 μg/ml, with determination coefficients, R2, exceeding 0.9997. The method was shown to be specific, precise at the intraday and interday levels, as reflected by the relative standard deviation (RSD) values, lower than 5.0%, and accurate with bias not exceeding 15% and percentage recovery was found to be in the range between 94.5 and 101.2. The limits of detection and quantification were 0.002 and 0.007 μg/ml, respectively. The method was successfully applied for the determination of t-RVT encapsulation efficiency.

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