Abstract
Aims: A new gradient RP-HPLC method was developed for the separation and determination of process related impurities in Palbociclib.
 Methodology: The chromatographic separation was achieved on a Inert sustain swift (C18) column using a mobile phase comprising of perchloric acid and acetonitrile in a gradient mode at a flow rate of 1 mL/min. over a runtime of 50 minutes. All the eluants were monitored at 230 nm. The optimized method was validated as per ICH guidelines for various parameters.
 Results: The linearity of the method was proposed in the range of LOQ to 250 % for the drug and its impurities by subjecting the data obtained to statistical analysis using correlation coefficient model (r > 0.99). The method also gave acceptable recovery of all the four impurities at each level and was found to be accurate. The % RSD obtained in the method precision and intermediate precision were less than 2% depicting the precision of the method. The LOD and LOQ values were calculated based on the signal to noise ratio and are indicating the sensitivity of the method. The specificity of the method was checked in the presence of process related impurities and also degradants generated by exposing to a variety of forced degradation conditions.
 Conclusion: The proposed RP-HPLC method for the determination of process related impurities of Palbociclib could be routinely used in the quality control testing.
Highlights
The proposed RP-HPLC method for the determination of process related impurities of Palbociclib could be routinely used in the quality control testing
The impurities in the drug substance [13] were identified based on the retention time (RT) and relative retention time (RRT) observed from the spike study
Limit of Detection (LOD) and Limit of Quantification (LOQ) were determined by measuring the magnitude of analytical background by blank samples and calculating the signal-to-noise ratio (S/N) for each compound by injecting a series of solutions until S/N ratio obtained as 3 for LOD and 10 for LOQ
Summary
Palbociclib (Fig. 1) is a piperazine pyridopyrimidine derivative and second generation cyclin-dependent kinase inhibitor [1]. Approved for the treatment of hormone receptorpositive and human epidermal growth factor receptor type 2 (HER2)-negative breast cancer in combination with aromatase inhibitors like letrazole as initial endocrine-based therapy or following fluvestrant as endocrine therapy in patients with disease progression. Palbociclib was the first Cyclin-Dependant Kinase 4 and Cyclin-Dependant Kinase 6 [2-5] inhibitor. It is a pale yellow colour solid with a molecular weight of 447.53 g/mol. N hydrochloric acid and insoluble in water.
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