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Abstract
With the objective of developing an advanced method for rapid separations with shorter runtime, a simple, precise, accurate stability-indicating isocratic reverse phase ultra-performance liquid chromatographic (RP-UPLC) method coupled with a photodiode array detector was developed for the quantitative determination of Gemcitibine hydrochloride and its three impurities (GEM) in drug substance. The determination was completed for an active pharmaceutical ingredient in the presence of degradation products and its process-related impurities. The method was optimized by using the samples generated from forced degradation studies. Good resolution between the peaks for impurities formed during synthesis, degradation products, and the analyte was achieved on a Waters Acquity UPLC HSS T3 (2.1 × 100 mm, 1.8 µm) column using mobile phase containing a mixture of buffer and methanol in the ratio of 90:10. The eluted compounds were monitored at 210 nm. The runtime was only 5.0 min, within which Gemcitabine, its three impurities, and degradation products were well separated. The degradation samples were assayed against the qualified reference standard and the mass balance in each case was more than 99%. The newly developed method was validated as per ICH guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision, and robustness. Forced degradation studies were also performed to demonstrate the stability indicating power of the developed UPLC method.
ACKNOWLEDGMENT
The authors wish to thank the management of Dr. Reddy's group for supporting this work. Authors wish to acknowledge the Process research group for providing the samples for our research.
