scholarly journals A Novel LC-MS/MS Method Development and Validation for Ultra-trace Level Determination of Three Genotoxic Efavirenz Impurities

2020 ◽  
Vol 82 (3) ◽  
Author(s):  
Annapoorna Vadlamani ◽  
K. Ravindhranath
2019 ◽  
Vol 15 (5) ◽  
pp. 591-598 ◽  
Author(s):  
Haitham Alrabiah ◽  
Ahmed Bakheit ◽  
Sabray Attia ◽  
Gamal A.E. Mostafa

Background: Conivaptan inhibits two of vasopressin receptor (vasopressin receptor V1a and V2). Conivaptan is used for the treatment of hyponatremia, and in some instances, for the treatment of the heart failure. Methods: The present study aimed to develop a simple, sensitive, and accurate HPLC with ultraviolet detection for the assay of conivaptan (CON) in mouse plasma using bisoprolol as internal standard (IS). A precipitation procedure was used to extract CON and the IS from the mouse plasma. CON was chromatographically separated using a C18 analytical column at 25°C. The separation was carried out using a mixture of phosphate buffer (50 mM): acetonitrile (60: 40, v/v, pH 4.5) with a flow rate of 1.0 mL/min and detection was performed at 240 nm. Results: The assay was validated according to the US Food and Drug (FDA) guidelines. The method demonstrated linearity over a concentration range of 150 - 2000 ng/mL (correlation coefficient: r 2 = 0.9985). The mean recovery of CON from the mouse plasma was 101.13%. All validation parameters for CON were within the acceptable range. Conclusion: The investigated method has been shown to be suitable for estimating the CON in plasma samples, and this method is sensitive and highly selective, allowing the estimation of its concentrations up to the nano-scale. The suggested method was successfully used in a pharmacokinetic study of CON in mouse plasma.


Author(s):  
Kuntal Mukherjee ◽  
S. T. Narenderan ◽  
B. Babu ◽  
Survi Mishra ◽  
S. N. Meyyanathan

A simple, sensitive and rapid high performance liquid chromatographic method has been developed for the determination of Propofol. The main focus of the method was to determine Propofol in solution form as well as in marketed formulation. Chromatographic separation was achieved on Inertsil ODS-3V column (250mm x 4.6mm; 5µm) with a mobile phase consisting of methanol: water (85:15), with a flow rate of 1.0ml/min (UV detection at 270nm). Linearity was observed over the concentration range of 10-110µg/ml with a regression equation y=88048x + 44524 and having a regression value (R2) of 0.999. The LOD and LOQ values found to be 10ng and 100ng, respectively. No changes found in ruggedness and robustness studies. The percentage of recovery was found to be 95.25% to 101.81%. Validation studies revealed that the method was specific, accurate, precise, reliable, robust, reproducible and suitable for the quantitative analysis in its pharmaceutical formulations.


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