Chiral Chromatography Studies of Chemical Behavior of Cinacalcet on Polysaccharide Chiral Reversed-Phase HPLC Stationary Phases

2012 ◽  
Vol 95 (6) ◽  
pp. 1639-1643 ◽  
Author(s):  
Michal Douša ◽  
Jiřiacute; Břicháč

Abstract A rapid HPLC method for the analytical resolution of cinacalcet enantiomers was developed. Four chiral columns (two amylose and two cellulose type) were evaluated in RP systems. Excellent enantioseparation with a resolution of more than 6 was achieved on Chiralpak AY (amylose 5-chloro-2-methylphenylcarbamate chiral stationary phase) using 10 mM triethylamine (pH 8.0)–acetonitrile (40 + 60, v/v) mobile phase. Validation of the HPLC method, including linearity, LOD, LOQ, precision, accuracy, and selectivity, was performed according to the International Conference on Harmonization guidelines. The method was successfully applied for the determination of (S)-cinacalcet in enantiopure active pharmaceutical ingredient (R)-cinacalcet.

2013 ◽  
Vol 5 (19) ◽  
pp. 5010 ◽  
Author(s):  
Marco Ciulu ◽  
Roberta Farre ◽  
Ignazio Floris ◽  
Valeria M. Nurchi ◽  
Angelo Panzanelli ◽  
...  

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.


1998 ◽  
Vol 11 (3) ◽  
pp. 167-171 ◽  
Author(s):  
Shabana I. Khan ◽  
David C. Limburg ◽  
Iklas A. Khan ◽  
John S. Williamson

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.


2010 ◽  
Vol 93 (4) ◽  
pp. 1077-1085 ◽  
Author(s):  
Nafiz O Can ◽  
Goksel Arli

Abstract Development and validation of an RP-HPLC method for determination of levetiracetam in pharmaceutical tablets is described. The separation and quantification of levetiracetam and caffeine (internal standard) were performed using a single analytical procedure with two different types of stationary phases, conventional Phenomenex Gemini C18 (100 4.6 mm, 5 m) and Merck Chromolith Performance RP18e (100 4.6 mm, macropore size 2 mm, micropore size 13 nm) monolithic silica. Five-microliter aliquots of samples were injected into the system and eluted using wateracetonitrile (90 + 10, v/v) mobile phase pumped at the rate of 1 mL/min. The analyte peaks were detected at 200 nm using a diode array detector with adequate resolution. Validation studies were performed using the method recommended by the International Conference on Harmonization, the U.S. Pharmacopeia, and AOAC INTERNATIONAL, which includes accuracy, precision, range, limits, robustness, and system suitability parameters. Levetiracetam and caffeine were detected in about 7 min using the conventional column, whereas less than 5 min was required when the monolithic column was used. Calibration plots had r values close to unity in the range of 0.88.0 g/mL. Assay of levetiracetam in a tablet formulation was demonstrated as an application to real samples.


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