scholarly journals Validation of a Stability-Indicating RP-HPLC Method for Determination of L-Carnitine in Tablets

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Roghaieh Khoshkam ◽  
Minoo Afshar
Keyword(s):  
Hplc Method ◽  
Stability Factor ◽  
Forced Degradation ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Forced Degradation Studies

A rapid and stability-indicating RP-HPLC method was developed for determination of l-carnitine in tablets. The separation was based on a C18 analytical column using a mobile phase which consisted of 0.05 M phosphate buffer (pH = 3): ethanol (99 : 1), including 0.56 mg/mL of sodium 1-heptanesulfonate. Column temperature was set at 50°C and quantitation was achieved by UV detection at 225 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. Among the different stress conditions, the exposure to acidic and basic conditions was found to be an important adverse stability factor. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in l-carnitine concentration range of 84.74–3389.50 µg/mL (r2=0.9997). Precision was evaluated by replicate analysis in which relative standard deviation (RSD) values for areas were found below 2.0%. The recoveries obtained (100.83%–101.54%) ensured the accuracy of the developed method. The expanded uncertainty (3.14%) of the method was also estimated from method validation data. Accordingly, the proposed validated and rapid procedure was proved to be suitable for routine analyzing and stability studies of l-carnitine in tablets.

scholarly journals Validation and Uncertainty Estimation of an Ecofriendly and Stability-Indicating HPLC Method for Determination of Diltiazem in Pharmaceutical Preparations

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Fahimeh Sadeghi ◽  
Latifeh Navidpour ◽  
Sima Bayat ◽  
Minoo Afshar
Keyword(s):  
Degradation Products ◽  
Pharmaceutical Preparations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Solution Ph ◽  
Validation Data ◽  
Column Temperature ◽  
Stability Indicating ◽  
Relative Standard

A green, simple, and stability-indicating RP-HPLC method was developed for the determination of diltiazem in topical preparations. The separation was based on a C18analytical column using a mobile phase consisted of ethanol: phosphoric acid solution (pH = 2.5) (35 : 65, v/v). Column temperature was set at 50°C and quantitation was achieved with UV detection at 240 nm. In forced degradation studies, the drug was subjected to oxidation, hydrolysis, photolysis, and heat. The method was validated for specificity, selectivity, linearity, precision, accuracy, and robustness. The applied procedure was found to be linear in diltiazem concentration range of 0.5–50 μg/mL (r2=0.9996). Precision was evaluated by replicate analysis in which % relative standard deviation (RSD) values for areas were found below 2.0. The recoveries obtained (99.25%–101.66%) ensured the accuracy of the developed method. The degradation products as well as the pharmaceutical excipients were well resolved from the pure drug. The expanded uncertainty (5.63%) of the method was also estimated from method validation data. Accordingly, the proposed validated and sustainable procedure was proved to be suitable for routine analyzing and stability studies of diltiazem in pharmaceutical preparations.

scholarly journals STABILITY INDICATING RP-HPLC ASSAY METHOD FOR ESTIMATION OF DIMETHYL FUMARATE IN BULK AND CAPSULES

2017 ◽  
Vol 9 (5) ◽  
pp. 121 ◽  
Author(s):  
Hemant K. Jain ◽  
Archana A. Gunjal
Keyword(s):  
Dimethyl Fumarate ◽  
Hplc Method ◽  
Assay Method ◽  
Forced Degradation ◽  
Dihydrogen Phosphate ◽  
Column Temperature ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Degradation Studies

Objective: To develop an accurate, simple, precise and specific stability indicating RP-HPLC method for estimation of dimethyl fumarate in bulk and capsules.Methods: An Inertsil ODS (150x4.6 mm, 5µ) column and a mobile phase containing acetonitrile: potassium dihydrogen phosphate buffer pH 6.8 (50:50% v/v) was used for this study. The flow rate was maintained at 1.0 ml/min; column temperature was fixed at 35 °C and UV detection was carried out at 210 nm. The forced degradation studies were performed and method was validated with as per ICH guidelines.Results: The retention time of dimethyl fumarate was found to be 3.3±0.02 min. The value of correlation coefficient between peak area and concentration was found to be 0.9993. The mean percent recovery of dimethyl fumarate in capsules was found in the range of 99.65 to 101.64%. The results of forced degradation studies indicated that the drug was found to be stable in basic, oxidative and thermal conditions while degraded in acidic conditions.Conclusion: It can be conducted from results that the developed HPLC method is simple, accurate, precise and specific. Results of stress testing study revealed that the method is stability indicating. Thus, this method can be used for routine analysis of dimethyl fumarate capsules and check their stability.  

scholarly journals Validation of a Stability-Indicating RP-HPLC Method for the Determination of Entecavir in Tablet Dosage Form

2010 ◽  
Vol 93 (2) ◽  
pp. 523-530 ◽  
Author(s):  
Sérgio Luiz Dalmora ◽  
Maximiliano da Silva Sangoi ◽  
Daniele Rubert Nogueira ◽  
Lucélia Magalhães da Silva
Keyword(s):  
Dosage Form ◽  
Potassium Phosphate ◽  
Hplc Method ◽  
Forced Degradation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 4.6 mm id) maintained at 30C. The mobile phase consisted of acetonitrilewater (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5200 g/mL (r2 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19, with bias lower than 1.81. The LOD and LOQ were 0.39 and 0.5 g/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.

scholarly journals Stability-indicating HPLC-DAD method for the determination of empagliflozin

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Shilpi Pathak ◽  
Pradeep Mishra
Keyword(s):  
Hplc Method ◽  
Coefficient Of Determination ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Forced Degradation Studies ◽  
Tablet Dosage

Abstract Background A stability-indicating RP-HPLC method was developed and validated for the estimation of empagliflozin drug and its tablet dosage form using a DAD detector. The mobile phase consisted of methanol/acetonitrile/0.1%OPA (75:20:5). The peak was observed at 2.54 min using 222.0 nm absorption maxima. Results Calibration curve plot was found within the range of 10–50 µg/mL. The coefficient of determination (R2) was found to be 0.9990. Forced degradation studies were performed for the empagliflozin in various conditions, and the results were calculated as %RSD values and were found to be within the limits. Conclusion The method was validated as per ICH guidelines with respect to all validation parameters.

scholarly journals A Stability Indicating RP-HPLC Method for the Estimation of Gemcitabine HCl in Injectable Dosage forms

2010 ◽  
Vol 7 (s1) ◽  
pp. S239-S244 ◽  
Author(s):  
Shaik Mastanamma ◽  
G. Ramkumar ◽  
D. Anantha Kumar ◽  
J. V. L. N. Seshagiri Rao
Keyword(s):  
Dosage Forms ◽  
Hplc Method ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Gemcitabine Hydrochloride ◽  
Rp Hplc ◽  
Forced Degradation Studies ◽  
The Stability ◽  
Injectable Dosage

A stability indicating RP HPLC method has been developed for the determination of gemcitabine hydrochloride. Chromatography was carried out on an ODS C18column (250×4.6 mm; 5μ) using a mixture of methanol and phosphate buffer (40: 60 v/v ) as the mobile phase at a flow rate of 1.0 mL/min. The detection of the drug was monitored at 270 nm. The retention time of the drug was found to be 2.31 min. The method produced linear responses in the concentration range of 10 to 60 μg/mL of gemcitabine HCl. The method was found to be reproducible for analysis of the drug in injectable dosage forms. The stability of the drug was assessed by forced degradation studies.

scholarly journals Design of experiment-driven stability-indicating RP-HPLC method for the determination of tofacitinib in nanoparticles and skin matrix

2021 ◽  
Vol 7 (1) ◽  
Author(s):  
Srividya Gorantla ◽  
Ranendra N. Saha ◽  
Gautam Singhvi
Keyword(s):  
Hplc Method ◽  
Adhesive Tape ◽  
Forced Degradation ◽  
Widespread Application ◽  
Stability Indicating ◽  
Relative Standard ◽  
Forced Degradation Studies ◽  
Factorial Design Of Experiments ◽  
Us Fda

Abstract Background Tofacitinib—an oral JAK inhibitor—has been recently approved by US FDA to treat moderate to severe RA. The delivery of tofacitinib to specific inflammation site at joint via topical route using nanoformulations helps in managing the potential adverse effects. The objective is to develop and validate a simple, specific, and sensitive stability-indicating HPLC method for quantification of tofacitinib in topical nanoformulations and different matrices (adhesive tape, and skin layers, i.e., stratum corneum, viable epidermis, and dermis). The major objective was to avoid use of instruments like LC–MS/MS and to ensure a widespread application of the method. Result A 32 factorial ‘design of experiments’ was applied to optimize process variables, to understand the effect of variables on peak properties. The calibration curve showed regression coefficient (R2) 0.9999 and linearity in the concentration range of 50 to 15,000 ng/mL, which is suitable for the analysis of conventional dosage forms and nanoformulations. Method validation was performed as per ICH guideline Q2 (R1). The accuracy by recovery studies ranged between 98.09 and 100.82%. The % relative standard deviations in intraday and interday precisions were in the range of 1.16–1.72 and 1.22–1.80%, respectively. Forced degradation studies indicated the specificity of method and showed stability-indicating potential for tofacitinib peak. Conclusion The validated method provides a quantification method of tofacitinib in the presence of formulation excipients, dissolution media, and skin tissues in detail. In addition, the method was successfully utilized for determination of various dermatokinetics profile of tofacitinib.

scholarly journals Stability Indicating RP-HPLC Method for Determination of Valsartan in Pure and Pharmaceutical Formulation

2010 ◽  
Vol 7 (1) ◽  
pp. 246-252 ◽  
Author(s):  
S. K. Patro ◽  
S. K. Kanungo ◽  
V. J. Patro ◽  
N. S. K. Choudhury
Keyword(s):  
Linear Response ◽  
Mobile Phase ◽  
Hplc Method ◽  
Forced Degradation ◽  
Control Analysis ◽  
Solution Stability ◽  
Stability Indicating ◽  
Quality Control Analysis ◽  
Rp Hplc

A simple, rapid and accurate and stability indicating RP-HPLC method was developed for the determination of valsartan in pure and tablet forms. The method showed a linear response for concentrations in the range of 50-175 µg/mL using 0.01 M NH4H2PO4(pH 3.5) buffer: methanol [50:50] as the mobile phase with detection at 210 nm and a flow rate of 1 mL/min and retention time 11.041 min. The method was statistically validated for accuracy, precision, linearity, ruggedness, robustness, forced degradation, solution stability and selectivity. Quantitative and recovery studies of the dosage form were also carried out and analyzed; the % RSD from recovery studies was found to be less than 1. Due to simplicity, rapidity and accuracy of the method, we believe that the method will be useful for routine quality control analysis.

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 Development and validation of a stability indicating RP-HPLC-DAD method for the determination of bromazepam

PLoS ONE ◽  
2021 ◽  
Vol 16 (3) ◽  
pp. e0244951
Author(s):  
Hany W. Darwish ◽  
Nesma A. Ali ◽  
Ibrahim A. Naguib ◽  
Mohamed R. El Ghobashy ◽  
Abdullah M. Al-Hossaini ◽  
...  
Keyword(s):  
Hplc Method ◽  
Array Detector ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Photodiode Array Detector ◽  
Alkaline Conditions ◽  
Development And Validation

A reliable, selective and sensitive stability-indicating RP-HPLC assay was established for the quantitation of bromazepam (BMZ) and one of the degradant and stated potential impurities; 2-(2-amino-5-bromobenzoyl) pyridine (ABP). The assay was accomplished on a C18 column (250 mm × 4.6 mm i.d., 5 μm particle size), and utilizing methanol-water (70: 30, v/v) as the mobile phase, at a flow rate of 1.0 ml min-1. HPLC detection of elute was obtained by a photodiode array detector (DAD) which was set at 230 nm. ICH guidelines were adhered for validation of proposed method regarding specificity, sensitivity, precision, linearity, accuracy, system suitability and robustness. Calibration curves of BMZ and ABP were created in the range of 1–16 μg mL-1 with mean recovery percentage of 100.02 ± 1.245 and 99.74 ± 1.124, and detection limit of 0.20 μg mL-1 and 0.24 μg mL-1 respectively. BMZ stability was inspected under various ICH forced degradation conditions and it was found to be easily degraded in acidic and alkaline conditions. The results revealed the suitability of the described methodology for the quantitation of the impurity (ABP) in a BMZ pure sample. The determination of BMZ in pharmaceutical dosage forms was conducted with the described method and showed mean percentage recovery of 99.39 ± 1.401 and 98.72 ± 1.795 (n = 6), respectively. When comparing the described procedure to a reference HPLC method statistically, no significant differences between the two methods in regard to both accuracy and precision were found.

FORCED DEGRADATION STUDIES OF TIZANIDINE HYDROCHLORIDE AND DEVELOPMENT OF VALIDATED STABILITY-INDICATING RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (4) ◽  
pp. 50-55
Author(s):  
Shahbaz Rathor ◽  
Atul Sherje ◽  
Keyword(s):  
Thermal Degradation ◽  
Hplc Method ◽  
Base Hydrolysis ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Stress Studies ◽  
Stability Indicating Method ◽  
Rp Hplc ◽  
Forced Degradation Studies

Simple and precise stability indicating RP-HPLC method for the quantitative determination of tizanidinehydrochloride (TZN) in pharmaceutical dosage form was developed and validated. The separation was achieved using Atlantis C18 column (250 x 4.6 mm, 5µm) at 25 °C using a mobile phase containing 20mM KH2 PO4 (pH 3.5):methanol in the ratio of 30:70 V/V at 0.8 mL/min flow rate and 315nm detection wavelength. The retention time for TZN was 3.7 min and showed linearity in the 5-40µg/mL range with R2 >0.99. The drug was subjected to acid/ base hydrolysis, oxidative and thermal degradation to establish stability indicating method. The method was validated as per ICHQ2 (R1) guidelines. The method was accurate, precise, and specific for TZN estimation. In stress studies, the drug was found to be stable to acid/alkaline hydrolysis, oxidation, and thermal degradation conditions. Thus, the reported method can be used as a stability-indicating method for quality control and routine analysis of TZN.

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