scholarly journals Method Development and Validation for the Determination of Indiquinoline Tartrate, a Novel Kappa Opioid Agonist, and its Related Substances by High-Performance Liquid Chromatography

2012 ◽  
Vol 50 (4) ◽  
pp. 343-348 ◽  
Author(s):  
C. Sun ◽  
Y. Shen ◽  
D. Sun ◽  
T. Hang ◽  
J. Tu
Author(s):  
O. S. S. Chandana ◽  
D. Sathis Kumar ◽  
R. Ravichandra Babu

Objective: Our main objective is to develop an accurate and precise RP-HPLC method for the determination of Eprosartan Mesylate and its impurities. Methods: A Develosil ODS UG-5; (150 × 4.6) mm; 5 µm column was used for the Separation of drugs by a mobile phase consisting of Buffer and Acetonitrile mixture in the gradient proportion. The flow rate maintained was 0.8 ml/min and the wavelength used for detection was 235 nm.Results: The linearity was observed in the range of 0.025-50µg/ml of spiked impurities in Eprosartan Mesylate, impurity 1 and impurity 2 with a correlation coefficient of 0.99927, 0.99910 and 0.99934 respectively. The mean percentage recoveries for LOQ, 50%, 80%, 100%, 150% and 200% accuracy were found to be 101.5±1.51, 107.0±1.7, 104.6±0.4, 102.8±0.36, 101.7±0.26 and 101.3±0.15 respectively for impurities in Eprosartan Mesylate, impurity 1 and impurity 2. Linearity, accuracy, precision and robustness parameters for the suggested method were estimated for validation.Conclusion: The developed method is uncomplicated, accurate, sensitive and precise for the determination of related substances in the Eprosartan Mesylate. The satisfying % recoveries and low % RSD Values confirmed the suitability of the developed method for the usual analysis of Eprosartan mesylate in pharmaceuticals.


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.


2011 ◽  
Vol 8 (3) ◽  
pp. 1444-1450 ◽  
Author(s):  
K. Ashok Kumar ◽  
S. Ramachandra Shetty ◽  
Laxmi Narasu

A simple, precise and accurate high-performance thin-layer chromatographic method has been established for the determination of rutin in the stem extract ofHibiscus micranthusLinn. A flavonoid fraction of methanolic extract of the stem powder was used for the experimental work. Separation was performed on silica gel 60 F254HPTLC plates withn-butanol: acetic acid: water: ammonia 3:1:1:1(v/v), as mobile phase. The determination was carried out using the densitometric absorbance mode at 286 nm. Rutin response was linear over the range 50–400 ng/μL. The concentration of rutin in the flavanoidal fraction was found to be 9.93%. The HPTLC method was evaluated in terms of sensitivity, accuracy, precision and reproducibility.


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