Background
To establish a simple, sensitive, accurate, precise, efficient, economical RP-UPLC method for simultaneous estimation of Doravirine, Lamivudine and Tenofovir disoproxil fumarate in bulk and their combined pharmaceutical formulations. Optimization of Chromatographic separation was achieved on analytical column HSS C18 (100 × 2.1 mm, 1.8 μ) maintained at temperature 30 °C and mobile phase consisting of 0.01 N Potassium dihydrogen orthophosphate buffer (pH-4.8) and acetonitrile in the ratio 60:40 v/v and at a flow rate 0.3 mL/min in isocratic mode. The injection volume was set as 1 µl detection wavelength is 260 nm. The proposed method validation was done as per International Council on Harmonization Q2 (R1) guidelines.
Results
Doravirine, Lamivudine and Tenofovir disoproxil fumarate were eluted at retention times of 1.2, 1.5, and 1.8 min respectively. The proposed method was identified an excellent linearity over concentration range of 12.5–75.0 µg/mL for Doravirine and 37.5–225.0 µg/mL for Lamivudine and 37.5–225.0 µg/mL for Tenofovir disoproxil fumarate. The percentage relative standard deviation for intra-day and inter-day precision of the present method was less than 2% for Doravirine, Lamivudine and Tenofovir disoproxil fumarate. Accuracy of the present method was evaluated by recovery studies which were in the range of 99.62–99.88% for Doravirine and 98.78–99.44% for Lamivudine and 99.67–100.52% for Tenofovir disoproxil fumarate. The limit of detection and limit of quantification were found to be 0.249 µg/mL and 0.756 µg/mL for Doravirine and 0.24 µg/mL and 0.727 µg/mL for Lamivudine and 0.797 µg/mL and 2.966 µg/mL for Tenofovir disoproxil fumarate. Forced degradation studies were carried out under various stress conditions like acid, base, peroxide, thermal, photo and neutral conditions.
Conclusions
The present method makes sure about no degraded impurity peak interference at the retention time of analyte peak hence can be applied for quality control investigation of Doravirine, Lamivudine and Tenofovir disoproxil fumarate in bulk and pharmaceutical formulations.
Background
The present investigation was proposed to develop a simple, sensitive, rapid, accurate, precise stability-indicating RP-UPLC method for simultaneous estimation of sitagliptin and ertugliflozin. Chromatographic separation was performed with Waters Hibar C8 [100×2.1mm, 2μ] column and mobile phase acetonitrile: water (pH 3.5) [50:50%, v/v], pumped at a flow rate 0.2ml/min. The separated analytes were detected with a UV detector at a wavelength of 218nm.
Results
The separation of sitagliptin and ertugliflozin was done at a retention time of 0.859min and 1.570min, respectively. The present method was validated according to the ICH guidelines Q2 R1, and stability-indicating studies were carried out as per ICH guidelines Q1A R2. Intra-day and inter-day precision were found to be within acceptable limits. The linearity of the proposed method was in the concentration range of 25–125μg/ml and 3.75–22.5μg/ml for sitagliptin and ertugliflozin, respectively. Limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.5μg/ml and 1.53μg/ml for sitagliptin and 0.13μg/ml and 0.38μg/ml for ertugliflozin, respectively. The recovery of the method was found in between 99.7% and 100.7%.
Conclusion
The proposed method was able to distinguish the analytes from by-products. Hence, the method was successfully implied for stability-indicating studies and for routine examination of sitagliptin and ertugliflozin in pharmaceutical formulation.
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