Prasugrel Dissolution

Sugral Tablet 5 mg. Prasugrel HCl Reference : MS

Dissolution for Prasugrel : Preparation of HCl , 0.1 M. Transfer 34.0 ml concentrated HCl in 6 liter vessel flask containing 1 liter of water and dilute with water to 4000 ml . Dissolution :

Method

:

Dissolution Medium Rotation speed Wave length Temperature Sampling time

: : : : :

USP apparatus II (Paddle method) 0.1 N HCl (500 ml) 75 rpm 240 nm 37oC ± 0.5 oC 30 minutes

Transfers 500 ml of dissolution medium into each of six vessels equilibrate at 37 oC ± 0.5 °C. Place one tablet into each of six vessels and press start rotation. After 30 minutes withdraw the sample. Filter in a HPLC vial through 0.45 micron filter paper using swinage. Mobile Phase. 0.01 M Phosphate Buffer pH 3.0: Dissolve 1.36 gm of monobasic potassium phosphate in about 500 ml of water, and dilute with water to 1000 ml and adjust pH 3.0 ± 0.05 using diluted phosphoric acid. Preparation of Mobile Phase: Prepare a mixture of (Phosphate buffer 0.01 M pH 3.0) and acetonitrile in ratio of (300 : 700). filter and degas mixture. Make adjustment if necessary. Standard Preparation: Weigh and transfer approximately 27.5 mg of Prasugrel Hydrochloride reference standard (equivalent to 25 mg Prasugrel) into 50 ml volumetric flask, add about 30 ml of Acetonitrile. Sonicate for 5 minute, dilute dilute to volume volume with Acetonit Acetonitril rilee and mix well. well. Pipette Pipette out 2 ml of above above soluti solution on into into a 100 ml volume volumetri tricc flask, flask, dilute dilute to volume volume with dissol dissoluti ution on medium medium and mix well. well. Filter Filter in a HPLC HPLC vial vial through 0.45 micron filter paper using swinage. Chromatographic Conditions: Column : Nucleosil 10-100, 4.6 mm x 250 mm, contains 10 µm (L1) or equivalent Wavelength avelen gth : 240 nm Flow rate : 1.2 ml/min. Injection volume : 20 µl

System suitability: Chromatograph the standard preparation, and record the peak areas as directed under procedure. The symmetry factor for Prasugrel is not more than 2.0. The relative standard deviations for five replicate injections of the standard preparation is not more than 2.0 %, if RSD is more than 2 % then inject one more standard and calculate the relative standard deviations for six replicate injections is not more 3.0 %. Procedure: Separately inject equal volume of the standard preparation and the assay preparation into the chromatograph, when column is conditioned, record the chromatograms. The area for the two sample  peaks should be within 3.0 %. Calculation:

C = Concentration of standard C = Weight of standard (mg) x 50

2 100

x 1000 = mcg/ml Factor 

Factor = Potency factor (Correction factor) of reference standard to make anhydrous. Rf = Response factor of standard Rf = Mean peak area of standard Concentration of standard Ps = Peak area of sample Prasugrel mg / tablet = Ps x Rf

500 __ 1 tablet

x

1 x 373.4 1000 409.90

373.4 Conversion factor to convert Prasugrel HCl to Prasugrel. 409.9 % Prasugrel = Prasugrel mg / tablet x 100 of label claim Label claim (5)