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

Abstract

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.

Development and validation of a stability indicating isocratic HPLC method for gemcitabine with application to drug release from poly lactic-co-glycolic acid nanoparticles and enzymatic degradation studies

“…reported 12 ng/ml and 37.5 ng/ml for LOD and LOQ based on calibration curve (an external standard method) [24]. The accuracy and precision were established across the linear range and met ICH requirements, within 2% for all tested concentrations, similar to other published reports [9,10,22–26]. Moreover, the robustness studies were carried out at different conditions of injection volume, flow rate, temperature, various percentage of organic content in the mobile phase and buffer pH.…”

“…[24] The accuracy and precision were established across the linear range and met ICH requirements, within 2% for all tested concentrations, similar to other published reports. [9,10,[22][23][24][25][26] Moreover, the robustness studies were carried out at different conditions of injection volume, flow rate, temperature, various percentage of organic content in the mobile phase and buffer pH. The system suitability was found to meet pre-established criteria at all the conditions and the % RSD in peak area was less than 2.0% for all conditions tested.…”

“…Very few HPLC methods deal with the determination of gemcitabine in the presence of degradation products from forced degradation studies, and those that do are time‐consuming, with complicated mobile phases and gradient elution leading to base line shifting [9,10]. To date, digestive enzymatic degradation studies of gemcitabine have not been reported.…”

“…Very few HPLC methods deal with the determination of gemcitabine in the presence of degradation products from forced degradation studies, and those that do are timeconsuming, with complicated mobile phases and gradient elution leading to base line shifting. [9,10] To date, digestive enzymatic degradation studies of gemcitabine have not been reported. Thus in this study, a simple analytical method was developed, which provides rapid quantification accurately and precisely to characterize and assess the performance of a pharmaceutical delivery systems of gemcitabine.…”

Stability-Indicating HPLC Determination of Gemcitabine in Pharmaceutical Formulations

“…Although several HPLC [ 14 – 22 ] and LC-MS/MS [ 23 – 28 ] methods have been reported for estimation of drug and its metabolites in biological fluids, these methods [ 23 – 28 ] are complicated, costly, and time consuming in comparison to a simple HPLC-UV method. A few stability indicating that HPLC methods [ 3 , 11 , 12 ] have been reported, which provides variable level of degradation of gemcitabine. Jansen et al [ 3 ] reported the separation and identification of degraded product of gemcitabine in acidic stress condition.…”