Tuesday, February 12, 2013

Assay Method (O)



 Assay Method of
 Ofloxacin Tablet

Buffer
Add 1 ml triethylamine in 500 ml of water and adjust the PH  3.0 ( ±0.05) with dilute phosphoric acid.
Ratio   
Accetonitrile : Buffer º 35 : 65
Diluents
Methanol  and  Water
Standard 
Weight and transfer about 50 mg working standard of Ofloxacin in a 100 ml volumetric flask. Add 70 ml of 0.1 M
Hydrochloric acid and shake for 20 minutes and dilute with 0.1M Hydrochloric acid up to the mark and mix well. Take
5 ml solution in a 50 ml volumetric flask and make volume up to the mark with 0.05 M Hydrochloric acid and mix
well. Filter this  solution with 0.45 m membrane filter before injection.
Sample 
Take the weight of 20 tablets & determine the average weight. Crush the tablets into fine powder. Take an amount of powder sample equivalent to  50 mg Ofloxacin in a 100 ml volumetric flask. Add 70 ml 0.1M Hydrochloric acid and shake for 30 minutes and  dilute  with 0.1 M Hydrochloric acid up to the mark and mix well & sonicate for 20 minutes . Filter the solution by whatman filter paper and take 5 ml filtrate solution in a 50 ml volumetric flask and make volume up to the mark with 0.05 M Hydrochloric acid and mix well. Finally filter this solution with 0.45 m  membrane filter before injection.
Condition
Waters Spherisorb 10 mm ODS1  4.6 ´ 250mm./ 40°C  / UV at 294 nm / 10 minutes.

Assay Method of
  Olmesartan Medoxomil INN Tablet


Mobile Phase
Mix the Methanol and 0.05% o-Phosphoric Acid in the proportion of 60: 40. Filter and degas for 10 minutes.
Diluents
Methanol
Standard 
Weigh accurately about 100 mg Olmesartan Medoxomil WS and transfer it in a 100 ml volumetric flask. Add 50ml of Methanol. Shake for 10 min. Then add sufficient Methanol to make 100 ml. Mix and filter this solution with 0.45mm membrane filter before injection.
Sample 
Take 20 tablets, weigh and determine the Average weight. Then crush these tablets into fine powder using mortar and pastle. Take accurately weight of the Tablet powdered sample containing about 100mg Olmesartan Medoxomil and transfer in a 100 ml volumetric flask. Add 60ml of Methanol. Shake for 20 min and add sufficient diluent to make 100 ml. Mix well and degassed for 10 minutes. Then filter the solution with whatman filter paper. Filter this resultant solution with 0.45 mm membrane filter before injection.
Condition
XTerraÒ PR18 5µm. 4.6 × 250 mm / 270 nm / 1ml per minute / 20 microliter /10 minutes / 6 minutes (Approx.)

Assay Method of
 Omeprazole Capsule

Standard
Take 50 mg of working standard of Omeprazole in a 100 ml volumetric flask. add 60 ml of methanol and shake for 30 minutes. Adjust the volume 100 ml with methanol. Take 1 ml of the solution in a 50 ml volumetric flask. Make the volume up to the mark (50ml) with methanol. Take the absorbance at 302 nm.   (Concentration =0.001%). Use methanol as blank.
Sample
Take 50 mg powder sample equivalent to 50 mg of Omeprazole in a100 ml volumetric flask. Add 60 ml of methanol and shake for 30 minutes. Adjust the volume 100 ml with methanol. Filter the solution by Whatman filter paper. Take 1 ml of the filtrate in a 50 ml volumetric flask. Make the volume up to the mark (50 ml ) with methanol . Take the absdrobance at 302 nm.. (Concentration = 0.001%).Use methanol as blank.

Assay Method of 
 Ondansetron Tablet

Buffer
Take 3.12 gm of NaH2PO4 in a 1000 ml volumetric flask. Add 750 ml distilled water and dissolve by stirring. Adjust the pH 5.4 by NaOH. Finally make the volume 1000 ml by water.
Ratio   
Accetonitrile : Buffer º 85 : 15
Diluents
Accetonitrile : Buffer º 85 : 15
Standard 
                                    Take 12.47 mg of Ondansetron Hydrochloride Working Standard equivalent to 10 mg of Ondansetron in a 100-ml volumetric flask. Add 60 ml of mobile phase and shake for15 minutes and make up the volume 100 ml with the mobile phase. Dilute 10 ml of this solution to 50 ml by the same solvent. Filter this solution with 0.45m syringe filters before injection.
Sample 
Take an accurately weight of powdered sample equivalent to 10 mg of Ondansetron in a 100-ml volumetric flask. Add
mobile phase and shake for15 minutes (Sonicate 5 minutes) and make up the volume 100 mlwith the mobile phase.
Dilute 10 ml of this solution to 50 ml by the same solvent. Filter this solution with 0.45m syringe filters before
injection.
Condition
Waters Spherisorb 5 mm CN 4.6 ´ 250mm./ UV at 216 nm / 20 minutes.

Assay Method of
 Ondansetron Solution

Standard
Take 20 mg of Ondansetron Equivalent to Ondansetron Hydrochloride working standard in a 250 ml volumetric flask. Add 180 ml of distilled water. Shake for 30 minutes. Add 0.1 M HCl to make volume 250 ml. Take 10 ml of the solution in a 100 ml volumetric flask. Make the volume up to mark (100 ml) with 0.1 M HCl. Measure the absorbance at 310 nm taking 0.1 M HCl as blank. (Concentration = 0.008 mg/ml)
Sample
Take 25 ml Anset solution equivalent to 20 mg of Ondansetron in a 250 ml volumetric flask. Add 180 ml of 0.1 M HCl, add shake for 30 minutes. Add 0.1 M HCl to make volume 250 ml. Take 10 ml of this solution in a 100 ml volumetric flask. Make the volume up to mark (100 ml) with 0.1 M HCl. Measure the absorbance at 310 nm taking 0.1 M HCl as blank. (Concentration = 0.008 mg/ml)

Assay Method of
 Ornidazole Tablet

Standard
Take powdered sample equivalent to about 50 mg of Ornidazole in a 100ml volumetric flask. Add 60ml of methanol. Shake for 20minutes. Add methanol to make volume 100ml. Filter the solution. Dilute 1 ml of the filtrate to 50 ml with same solvent.
Sample
Dissolve about 50 mg of Ornidazole WS in solvent and dilute to 100ml. Dilute 1 ml of the solution to 50 ml with same solvent.Measure the absorbance of both sample & standard solution at 311 nm using solvent as blank.

Assay Method of
 Oxyphenonium Tablet

Method - 01
Sample
Take powdered sample equivalent to about 100 mg of Oxyphenonium Bromide add 50 ml of water. Acidify with 2M Nitric acid. Titrate with 0.1M Silver Nitrate soluyion VS & determine the end point potentiometrically .Each ml of 0.1M Silver Nitrate º 42.84 mg of Oxyphenonium Bromide
       
% of content = Required volume of 0.1 M Silver Nitrate VS x F x 42.84 x 100 / Weight of Sample                                                                   

Assay Method of
 Oxyphenonium Tablet
Method - 02
Standard
Dissolve about 25 mg of Oxyphenonium Bromide WS in water and dilute to 250 ml.
Sample
Take powdered sample equivalent to about 25 mg of Oxyphenonium Bromide in a 250 ml volumetric flask, add 200 ml of water and shake for 20 minutes, then volume to 250 ml with water and mix and filter the solution.
System
Take 5 ml each of sample and standard preparation in two 250 ml separating funnel. Add 5 ml of borate buffer and 5 ml of bromothymol blue solution to each preparation. Extract each with 25 ml of chloroform. Reject first 5 ml of the chloroform layer. Measure the absorbance of the chloroform layer at 405 nm taking chloroform as blank.

 Assay Method of
 Oxytocin Injection

Buffer
Take 19.50 g Sodium dihydrogen Orthophosphate( NaH2PO4 ) in 500 ml volumetric flask & dissolve with water make up to 500 ml.
Mobile phase-A 
Buffer ( 20 % ) :   Water ( 80 % )
Mobile phase-B

Buffer ( 20 % ) :  Water ( 30 % )  :   Acetonitrile ( 50 % )
Ratio 
Mix fifty parts of  Mobile phase-A with fifty parts of  Mobile phase-B.
Diluents

Standard  
Weight and transfer about 10 mg working standard of Oxytocin (Potency  approximately 500 IU/mg) in a 100 ml  volumetric flask. Add 75 ml of water and shake for 10 minutes and dilute with water up to the mark and mix well. Dilute 5 ml of  this solution 50 ml volumetric flask  & mix well. Filter this solution with 0.45 m membrane filter before injection.

Sample 
Take an amount of sample concentration 5 IU/ ml & filter this solution with 0.45 m membrane filter before injection.
Condition
Waters Sphreisorb  ODS2 , 5 m   4.6 mm x 150 mm./  25°C / UV at 210 nm / 20 minutes.

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