Development of a simple and stability-indicating RP-HPLC method for determining olanzapine and related impurities generated in the preparative process

The Analyst ◽  
2011 ◽  
Vol 136 (15) ◽  
pp. 3149 ◽  
Author(s):  
Daoping Cui ◽  
Yueqing Li ◽  
Mingming Lian ◽  
Feng Yang ◽  
Qingwei Meng
Keyword(s):  
Hplc Method ◽  
Stability Indicating ◽  
Related Impurities ◽  
Rp Hplc ◽  
Preparative Process

scholarly journals A VALIDATED STABILITY INDICATING RP-HPLC METHOD FOR ESTIMATION OF TOLFENAMIC ACID IN PRESENCE OF ITS PHARMACOPOEIAL IMPURITIES

2019 ◽  
pp. 264-270
Author(s):  
ADISON FERNANDES ◽  
SANJAY PAI P. N.
Keyword(s):  
Oxidative Stress ◽  
Correlation Coefficient ◽  
Flow Rate ◽  
Hplc Method ◽  
Tolfenamic Acid ◽  
Stress Conditions ◽  
Forced Degradation ◽  
Stability Indicating ◽  
Related Impurities ◽  
Rp Hplc

Objective: The proposed research work was conducted to develop a single reverse-phase high-performance chromatography (RP-HPLC) method capable of separating two Pharmacopoeial related impurities as well as degradation product of Tolfenamic acid (TA). The drug was subjected to various stress conditions recommended under ICH Q1A (R2) guidelines. Methods: The desired separation of two Pharmacopoeial impurities and one degradant generated under oxidative stress was carried out using Sunfire ODS C-18 (250 x 4.6 mm, 5 µm) column maintained at 40 °C. Isocratic elution was carried out using acetonitrile and ammonium dihydrogen orthophosphate buffer (10 mmol, pH 2.5) in the ratio of 80:20 v/v. The detection was carried out at 205 nm using flow rate of 1 ml/min. The developed method was validated as per ICH Q2 (R1) guidelines for specificity, linearity, accuracy, precision, Limit of detection (LOD), Limit of Quantification (LOQ) and robustness. Results: Linearity response of TA was found at a concentration range of 10-100µg/ml, with a correlation coefficient of 0.9987. The Pharmacopoeial impurity A and impurity B showed linearity results at concentration of 0.1-1µg/ml, with correlation coefficient of 0.9984 for Impurity A and 0.9989 for Impurity B. The % recovery during accuracy studies for TA and the two impurities were within the acceptance range of 95-105%. LOD and LOQ for TA were found to be 4.561µg/ml and 133.771µg/ml respectively. For impurity A, LOD and LOQ were found to be 0.035 µg/ml and 0.106 µg/ml and for Impurity B, LOD and LOQ were 0.042 µg/ml and 0.128 µg/ml. With slight variation of organic phase in mobile phase and flow rate the method exhibited good robustness. Under forced degradation studies the drug was found stable under hydrolytic, photolytic and thermal stress conditions, but was found susceptible for degradation under oxidative stress with appearance of a degradant peak. From on the RRT values of Pharmacopoeial impurities and the formed degradant it was inferred that the developed method is selective for the drug in the presence of impurities or degradants. Conclusion: The developed stability-indicating method is found to be simple, rapid, accurate, precise and robust as compared to other proposed methods while determining TA in presence of its Pharmacopoeial impurities and degradation products. Hence the developed method can be used for analysis of stability samples of TA in presence of its related impurities.

scholarly journals Stability Indicating RP-HPLC Method for the Analysis of Dacomitinib and its Related Impurities in Bulk and Oral Solid Dosage Formulations

2021 ◽  
pp. 187-199
Author(s):  
Venu Kamani ◽  
M. Sujatha ◽  
G. S. N. Koteswara Rao ◽  
N. Vinod Kumar
Keyword(s):  
Mobile Phase ◽  
Degradation Products ◽  
Small Cell Lung Carcinoma ◽  
Sodium Perchlorate ◽  
Growth Factor Receptor ◽  
Hplc Method ◽  
Cell Lung Carcinoma ◽  
Stability Indicating ◽  
Related Impurities ◽  
Rp Hplc

Dacomitinib is an epidermal growth factor receptor inhibitor prescribed for the treatment of metastatic non small-cell lung carcinoma. There are no reported significant official of HPLC methods that resolve the impurities and degradation products generated during stability studies. Therefore, an isocratic RP-HPLC-UV method was developed for the determination of Dacomitinib in the presence of its related impurities and degradation products. The separation of Dacomitinib, impurity 1 and 2 was achieved on Agilent ZORBAX Eclipse (250×4.6 mm; 5 µ id) column as stationary phase, 0.1M sodium perchlorate at pH 5.6, acetonitrile as mobile phase in the ratio of 20:80 (V/V) at a flow rate of 1.0 mL/min in isocratic condition as mobile phase and UV detection was carried at 253 nm. In the optimised conditions, well resolved and retained peaks were observed at a retention time of 5.8 min, 4.0 min and 7.7 min for Dacomitinib, impurity 1 and 2 respectively. In the developed method, a very sensitive detection limit of 0.06 and 0.025 µg/mL was observed for impunity 1 and 2 respectively. The calibration was observed to be within the concentration range of 20 – 200 µg/mL for Dacomitinib and 0.2 – 2 µg/mL for impurity 1 and 2. The proposed method was used to investigate the effective separation of impurities along with degradation compounds formed under different degradative conditions and confirms that the method is stability indicating. Hence it can be concluded that the method was found to be simple, sensitive, specific, accurate, linear, precise, rugged, robust, and useful for estimation and characterizing the stability of Dacomitinib, impurity 1 and 2.

scholarly journals DEVELOPMENT AND VALIDATION OF A STABILITY INDICATING RELATED SUBSTANCES OF TRANDOLAPRIL BY RP-HPLC AND ITS DEGRADATION

2021 ◽  
pp. 115-121
Author(s):  
CHALLA SUDHEER REDDY ◽  
B. TIRUMALESWARA RAO
Keyword(s):  
Quantitative Methods ◽  
Gradient Elution ◽  
Hplc Method ◽  
Allowable Limit ◽  
Stability Indicating ◽  
Pharmaceutical Ingredients ◽  
Related Impurities ◽  
Related Substances ◽  
Rp Hplc ◽  
Test Concentration

Objective: A validated stability-indicating RP-HPLC method for Trandolapril was developed by separating its related impurities. Methods: By using Waters HPLC e-2695 quaternary pump with a PDA detector of 2998 instrument the chromatographic separation of Trandolapril and its related impurities was achieved on the column of Agilent eclipse C18 (150x4.6 mm, 3.5 µ) using gradient elution with a buffer containing 0.1percent formic acid and acetonitrile as a mobile phase with a flow rate of 1 ml/min at ambient temperature. A detector wavelength of 213 nm utilizing the PDA detector were given in the instrumental settings. The linearity was studied between the concentration range of 4-60 µg/ml of Trandolapril and 0.5-7.5 µg/ml of imp-E, imp-A, imp-B and 0.7-10.5 µg/ml of imp-D were injected with a run time of 17 min. Validation of the proposed method was carried out according to an International Conference on Harmonization (ICH) guidelines. Results: LOD and LOQ for the Trandolapril and its impurities were established with respect to test concentration. The plotted calibration curves were linear with a regression coefficient of R2>0.999, indicates that the linearity was with in the limit. As a part of method validation the parameters like specificity, linearity, accuracy, ruggedness, robustness were determined and the results were found to be within the allowable limit. Conclusion: The method developed was found to be applicable to routine analysis and to be used for the measurement of active pharmaceutical ingredients (i. e, Trandolapril and its related impurities). Since, there is no HPLC method reported in the literature for the estimation of Trandolapril and its related impurities, there is a need to develop quantitative methods under different conditions to achieve improvement in specificity, selecivity etc.

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