Pitavastatin Calcium in Pharmaceutical Dosage Forms
1.Chemicals and reagents
Pitavastatin calcium was from Micro Laboratories. HPLC-grade Acetonitrile and methanol was purchased from Merck, India. Highpurity water was prepared using Millipore purification system. Other chemicals and reagents were of AR grade Pitava 1 and Flovas 1mg were obtained commercially.
2.Instrumentation and chromatographic conditions
HPLC analysis was performed on a Shimadzu LC-10ATVP pump, SPD-M10 AVP with PDA detector. Separation was achieved on the phenomenex C18 (250 x 4.60); 5µ particle size column at room temperature with the mobile phase constituted by 0.5% acetic acid: acetonitrile (35:65) at the flow rate of 1 ml/min. The mobile phase was filtered through 0.45µm nylon filter (Millipore, USA) and degassed by sonication prior to use. The detection was performed at 245 nm. The Standard and sample was introduced through an injector valve with a 20 µl, sample loop. Data acquisition was performed using CLASS-VP software by the measurement of peak areas.
3.Preparation of sample solution
Twenty tablets of Pitavastatin Calcium(CAS NO: 147526-32-7) and Flovas containing 1 mg of Pitavastatin calcium were weighed to get the average weight and then powdered. An amount of powder equivalent to 1 mg of Pitavastatin calcium was transferred to a 100 ml volumetric flask with 50 ml mobile phase and shaken for 10 min, followed by making up to volume with mobile phase. This solution was filtered using 0.2 µ membrane filter. From this 1 ml were pipetted out and transferred to 10 ml volumetric flask, 1 ml of internal standard solution (µg/ml) was added to each and made up to the volume to get the concentration of 1 µg/ml of Pitavastatin calcium.
4.Preparation of standard solution
Standard stock solution of pitavastatin calcium(CAS NO: 147526-32-7) and paracetamol (1000 µg/ml) was prepared in mobile phase containing 0.5% Acetic acid: Acetonitrile 35:65 (%, v/v). Working standard solutions for the calibration curve were prepared by dilution of the above stock solution in a range of 1-5 µg/ml with mobile phase. To each dilution a fixed concentration of 1 µg/ml of internal standard paracetamol was added.
5.Method development and choice of internal standard
A variety of mobile phases and internal standards were investigated in the development of an HPLC method suitable for analysis of Pitavastatin Calcium in the tablet formulations. Finally, the condition adopted was 0.5% acetic acid: acetonitrile 35:65 (%, v/v), at the flow rate of 1 ml/min. Paracetamol was selected as the suitable internal standard for this method.
6.Method validation
The method was validated for the parameters like specificity, range and linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy, and precision based on ICH/CPMP guidelines
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