scholarly journals Development and Validation of Modern UHPLC-DAD Analytical Method for Simultaneous Determination of Repaglinide and Metformin in Pharmaceutical Dosage Forms

2020 ◽  
Vol 32 (12) ◽  
pp. 3127-3134
Keyword(s):  
Simultaneous Determination ◽  
Metformin Hydrochloride ◽  
Forced Degradation ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
System Suitability ◽  
Forced Degradation Studies ◽  
Development And Validation ◽  
Isocratic Mode

For the simultaneous determination of repaglinide and metformin hydrochloride in bulk, an effective and simple UHPLC method was developed and validated and applied to marketed repaglinide and metformin products. The mobile phase used for chromatographic runs consisted of 30 mM phosphate buffer (pH 3.7) and acetonitrile (20:80, v/v) separation was implemented using isocratic mode on an Agilent Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm) column. Drug peaks were well separated and a 232 nm DAD detector observed them. The method was linear for repaglinide and metformin at the concentration range of 20-100 μg/mL, respectively. The method has been validated with respect to system suitability, specificity, accuracy, precision, robustness and ruggedness according to ICH guidelines. Repaglinide and metformin forced degradation studies were conducted for under acidic, base, neutral (peroxide), thermal and photo conditions.

scholarly journals LC-MS/MS CHARACTERIZATION OF FORCED DEGRADATION PRODUCTS OF TUCATINIB, A NOVEL TYROSINE KINASE INHIBITOR: DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD

2022 ◽  
pp. 58-66
Author(s):  
S. K. REEHANA ◽  
K. SUJANA
Keyword(s):  
Kinase Inhibitor ◽  
Degradation Products ◽  
Degradation Pathway ◽  
Hplc Method ◽  
Forced Degradation ◽  
Ich Guidelines ◽  
System Suitability ◽  
Forced Degradation Studies ◽  
Development And Validation

Objective: The current study focused on the development, validation, and characterization of forced degradation products using LC-MS/MS. Methods: A simple, selective, validated and well-defined isocratic HPLC methodology for the quantitative determination of Tucatinib at a wavelength of 239 nm. An isocratic elution of samples was performed on an Inertsil ODS (250x4.6 mm, 5m) column with a mobile phase of 70:30v/v Acetonitrile and formic acid (0.1%) delivered at a flow rate of 1.0 ml/min. MS/MS was used to characterize degradation products formed in the forced degradation study. The validation and characterization of forced degradation products were performed in accordance with ICH guidelines. Results: Over the concentration range of 5-100μg/ml, a good linear response was obtained. Tucatinib's LOD and LOQ were determined to be 0.05 and 0.5, respectively. According to standard guidelines, the method was quantitatively evaluated in terms of system suitability, linearity, precision, accuracy, and robustness, and the results were found to be within acceptable limits. The drug was degraded under acidic, alkaline, and reduction conditions in forced degradation studies. Conclusion: The method was found to be applicable for routine tucatinib analysis. Because no LC-MS/MS method for estimating tucatinib and its degradation products has been reported in the literature. There is a need to develop a method for studying the entire tucatinib degradation pathway.

scholarly journals Novel LC Method Development and Validation for Simultaneous Determination of Montelukast and Doxofylline in Bulk and Pharmaceutical Dosage Forms

2013 ◽  
Vol 2013 ◽  
pp. 1-7
Author(s):  
Gadapa Nirupa ◽  
A. Siva Kumar ◽  
Upendra M. Tripathi
Keyword(s):  
Simultaneous Determination ◽  
Method Development ◽  
Dosage Forms ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Pharmaceutical Dosage Form ◽  
Pharmaceutical Dosage Forms ◽  
Ich Guidelines ◽  
Development And Validation

A novel rapid HPLC method was developed for simultaneous determination of montelukast and doxofylline in bulk and pharmaceutical dosage forms. Development of an analytical method for simultaneous estimation of drugs requires a lot of efforts and of course it is a challenging task. The method was developed by using C18 (150 mm×4.6 mm, 5 μm) column; mobile phase consisting of methanol and phosphate buffer at pH 4.5; the flow rate of 1.0 mL/min and ultraviolet detection at 280 nm. Both drugs were sufficiently resolved having retention time of 4.7 min and 1.9 min for montelukast and doxofylline, respectively. The method was validated as per ICH Guidelines for various parameters like precision, linearity, accuracy, ruggedness, and robustness. The validated method was applied to the commercially available pharmaceutical dosage form and obtained the desired result.

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 Development and validation of a novel stability indicating HPLC method for the separation and determination of darolutamide and its impurities in pharmaceutical formulations

2021 ◽  
Vol 104 (4) ◽  
pp. 57-68
Author(s):  
V.G. Kamani ◽  
◽  
M. Sujatha ◽  
G.B. Daddala ◽  
◽  
...  
Keyword(s):  
Ammonium Acetate ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Forced Degradation ◽  
Degradation Study ◽  
Stability Indicating ◽  
System Suitability ◽  
Development And Validation ◽  
First Time

This study reports for the first time about a stability indicating RP-HPLC method for analysis of darolutamide and its impurities 1, 2, and 3 in bulk and formulations. The separation was achieved on Phenomenex column with Luna C18 (250 mm × 4.6 mm, 5 μm) as stationary phase, and 50 mM ammonium acetate: methanol solution 15:80 (v/v) at pH 5.2 as mobile phase at 1.0 mL/min flow rate. UV detection was carried at wavelength of 239 nm. In these conditions the retention time of darolutamide and its impurities 1, 2, and 3 was 7.05, 8.90, 4.63 and 5.95 min, respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability, and robustness. Forced degradation study was done through exposure of the analyte to five different stress conditions and the % degradation was small in all degradation condition. The proposed method can separate and estimate the drug and its impurities in pharmaceutical formulations. Hence, the developed method was suitable for the quantification of darolutamide and can separate and analyse impurities 1, 2, and 3

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.

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 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 Development and Validation of a New HPLC-UV Method for the Simultaneous Determination of Triclabendazole and Ivermectin B1a in a Pharmaceutical Formulation

2010 ◽  
Vol 93 (6) ◽  
pp. 1868-1873 ◽  
Author(s):  
Maher Shurbaji ◽  
Mohamad H Abu Al Rub ◽  
Munib M Saket ◽  
Ali M Qaisi ◽  
Maher L Salim ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Analytical Method ◽  
Significant Variation ◽  
Rp Hplc ◽  
System Suitability ◽  
Experimental Parameters ◽  
Development And Validation ◽  
Interday Precision ◽  
Peak Purity

Abstract A rapid, simple, and sensitive RP-HPLC analytical method was developed for the simultaneous determination of triclabendazole and ivermectin in combination using a C18 RP column. The mobile phase was acetonitrilemethanolwateracetic acid (56 36 7.5 0.5, v/v/v/v) at a pH of 4.35 and flow rate of 1.0 mL/min. A 245 nm UV detection wavelength was used. Complete validation, including linearity, accuracy, recovery, LOD, LOQ, precision, robustness, stability, and peak purity, was performed. The calibration curve was linear over the range 50.09150.26 g/mL for triclabendazole with r = 0.9999 and 27.0181.02 g/mL for ivermectin with r = 0.9999. Calculated LOD and LOQ for triclabendazole were 0.03 and 0.08 g/mL, respectively, and for ivermectin 0.07 and 0.20 g/mL, respectively. The intraday precision obtained was 98.71 with RSD of 0.87 for triclabendazole and 100.79 with RSD 0.73 for ivermectin. The interday precision obtained was 99.51 with RSD of 0.35 for triclabendazole and 100.55 with RSD of 0.59 for ivermectin. Robustness was also studied, and there was no significant variation of the system suitability of the analytical method with small changes in experimental parameters.

scholarly journals Simultaneous determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation using spectrophotometric technique (Simultaneous Equation Method)

2015 ◽  
Vol 1 (1) ◽  
pp. 45
Author(s):  
Bhadresh V Savaj ◽  
Hasumati A. Raj ◽  
Rajanit V Sojitra ◽  
Paras Virani
Keyword(s):  
Simultaneous Determination ◽  
Simultaneous Equation ◽  
Equation Method ◽  
Propranolol Hydrochloride ◽  
Data Manipulation ◽  
Ich Guidelines ◽  
Quality Control Testing ◽  
Minimal Data ◽  
Development And Validation

A new spectrophotometric method was developed for simultaneous determination of compounds with interfering spectra in binary mixtures without previous separation, showing significant advantages over the conventional methods regarding minimal data manipulation and applicability. The proposed method was applied for the determination of Propranolol hydrochloride and Hydrochlorothiazide in Tablets formulation, for determination of sampling wavelength, 10 ?g/ml of each of PRO and HCT were scanned in 200-400 nm range and sampling wavelengths were 289 nm for PRO and 270 nm for HCT are selected for development and validation of simultaneous equation method. For this method linearity observed in the range of 10-50 ?g/ml for PRP and 5-25 ?g/ml for HCT, and in their pharmaceutical formulation with mean percentage recoveries 100.13 0.86 and 100.07 0.58, respectively. The method was validated according to ICH guidelines and can be applied for routine quality control testing.

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