Development and Validation of Bioanalytical Method for the Determination of Cobicistat from Human Plasma

We aimed to investigate the performance of the development method for sitagliptin quantification analysis in human plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS) using liquid-liquid extraction (LLE) and Nebivolol as internal standard (IS). The parameters of this presented validation method are selectivity, the lower limit of quantification (LLOQ), linearity, accuracy, precision with five different concentration (LLOQ, Low QC, Medium QC, High QC, Upper Limit Of Quantification (ULOQ)), Integrity of dilution, matrix effect, and test for stability. Based on this study, the multiple reaction monitoring (MRM) transitions were m/z 408,23 → 127,02 for Sitagliptin and m/z 406,25 → 151,06 for IS Nebivolol. The selectivity test obtained % interference of sitagliptin and IS nebivolol by (0.00 - 0.38) % and (0.04 - 0.24) %, respectively. LLOQ test obtained a concentration value of 10.32 ng/mL and % RSD (n = 5) of 5.27 %. When the Sitagliptin concentration ranged from 1 to 1000 ng/mL, the method showed strong linearity with a coefficient of correlation of 0.9991. Accuracy test obtained % differentiation of (-12.58 - 7.77) % and precision test obtained % RSD of (1.62 - 5.32) %. The dilution integrity test obtained % differentiation at 4 and 2 times dilution was -9.20 % and -9.16 %. Matrix effect and stability data were in line with the stipulated European Medicines Agency (EMA) guidelines for validating the bioanalytical method.

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Development and Validation of an Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry method with Liquid-Liquid Extraction for The Quantification of Sitagliptin in Human plasma using Nebivolol as Internal Standard

Rochaeny

Irawan

Saputro

et al. 2022

RJPT

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Development and validation of UPLC method for simultaneous estimation of Darunavir, Cobicistat, Emtricitabine and Tenofovir alafenamide in bulk drug and pharmaceutical dosage form

Dadi

Gummadi

2023

RJPT

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The main objective of the present study was to develop and validate a multicomponent analysis of Darunavir, Cobicistat, Emtricitabine and Tenofovir alafenamide in bulk drug and pharmaceutical dosage form by ultra-performance liquid chromatography (UPLC). The drugs were separated using HSS C18 (100mm × 2.1mm, 1.8µ particle size) column with mobile phase consisting of potassium dihydrogen phosphate, pH adjusted to 5.4 and acetonitrile in the composition of 60:40 %v/v operated in isocratic mode at a flow rate of 0.3 ml/min. The column temperature maintained at 30˚C and detection wavelength used was 260 nm. The retention time for Darunavir was found to be 1.04min, for Cobicistat it was 1.82 min, for Emtricitabine it was 2.28 min and for Tenofovir it was found to be 1.39min. The developed method was validated in accordance to the ICH guidelines. The method obeyed Beer’s law in the concentration range of 50 µg/ml- 300µg/ml for Darunavir, 7.5 µg/ml – 45 µg/ml for Cobicistat, 25µg/ml - 150µg/ml for Emtricitabine and 0.625 µg/ml – 3.75µg/ml for Tenofovir alafenamide, with correlation coefficient of 0.999. The % relative standard deviation for all the drugs was found to be less than two indicating the method to be precise. The mean % recovery was found to be within the limits for all the drugs indicating that the method to be accurate. The method was also found to be specific, robust and stable. From the forced degradation studies, it was concluded that the drugs were found to be stable when exposed to different stress conditions as the net degradation was found within the acceptance criteria. The developed method for the multicomponent analysis of Darunavir, Cobicistat, Emtricitabine and Tenofovir alafenamide using UPLC can be used for quality control and routine analysis in bulk drug and pharmaceutical dosage form.

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Development and Validation of Bioanalytical Method for the Determination of Cobicistat from Human Plasma

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Development and Validation of an Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry method with Liquid-Liquid Extraction for The Quantification of Sitagliptin in Human plasma using Nebivolol as Internal Standard

Development and Validation of an Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry method with Liquid-Liquid Extraction for The Quantification of Sitagliptin in Human plasma using Nebivolol as Internal Standard

Development and validation of UPLC method for simultaneous estimation of Darunavir, Cobicistat, Emtricitabine and Tenofovir alafenamide in bulk drug and pharmaceutical dosage form

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