Tuesday, February 12, 2013

Assay Method (P)



Assay Method of
  Pantoprazole Sodium / Solution

Standard
Dissolve about 50 mg of Pantoprazole Sodium WS in 60 ml of methanol and dilute to 100 ml with same solvent. Dilute 2 ml of the filtrate to 50 ml with methanol.
Sample
Shake a quantity of powder containing 50 mg of Pantoprazole Sodium (1mg of Pantoprazole is equivalent to 1.058mg of Pantoprazole Sodium) with 60 ml of methanol for 20 minutes, add sufficient methanol to produce 100 ml and filter. Dilute 2 ml of the filtrate to 50 ml with methanol. Measure the absorbance of sample and standard solution at 289 nm using methanol as blank.
                           
  Assay Method of
   Paracetamol Tablet & Suppository
                             .
Sample 
Weigh 10 suppositories and cut into small pieces. To a quantity containing 75 mg of Paracetamol add 25 ml of 0.1 M
Sodium Hydroxide and 75 ml of water. warm if necessary to dissolve & mix. Cool in ice and filter. Dilute 1 ml of the
filtrate to 100 ml with a mixture of 9 ml of 0.1 M Sodium Hydroxide and water. Mix. Measure the absorbance of the
resulting solution at 257 nm, using 0.01 M Sodium Hydroxide as blank.
Calculation
 % of Paracetamol =  Absorbance of Sample ´ 100 / Conc.in g / 100 ml  ´ 715                                              
                                      
Assay Method of
  Paracetamol Syrup & Suspension
                             .
Sample 
Accurately transfer 3 ml of syrup/suspension equivalent to 72 mg of Paracetamol into 100 ml amber volumetric flask. Add 70 ml of 0.01 M NaOH & shake for 15 minutes and then up to the mark 100 ml with 0.01 M NaOH .Take 1 ml of the solution in a 100 ml volumetric flask. Make the volume up  to mark (100 ml) with 0.01 M NaOH  and mix well. Measure the absorbance at 257 nm taking 0.01 M NaOH as blank. Calculate the content of Paracetamol taking 715 as the value of A (1%, 1 cm) at the maximum at 257 nm. (Concentration of Sample 0.00072%).
Calculation
 % of Paracetamol =  Absorbance of Sample ´ 100 / 0.00072 ´ 715                                              
          
Assay Method of
 Paracetamol + Caffeine Tablet

Buffer
Transfer accurately weighed about 0.82 g of anhydrous sodium acetate to a 1000 ml volumetric flask and dissolved in water than add 20 ml of Tetrahydrofuran and mix well and dilute with water to volume  and mix well. Adjust pH 4.5 glacial acetic acid  and than filter  and digas.
M. Phase
Mobile Phase B: Aceonitrile & Mobile Phase C: Buffer pH 4.5
Solvent
Buffer pH 4.5 : Acetonitrile = 95 : 5
Standard 
Transfer about 10.0 mg of Caffeine WS and 77.0 mg of Paracetamol WS to a 50 ml volumetric flask and add 10 ml of solvent than shake and sonicate, if necessary to dissolve. Dilute with solvent to volume, mix and filter. Take 5 ml of this filtrated solution to a 50 ml volumetric flask and dilute with solvent up to the mark. Filter this solution with 0.45 µ membrane filter before injection.
Sample 
Shake a quantity of the powdered sample containing about 10.0 mg of Caffeine WS and 77.0 mg of Paracetamol WS to a 50 ml volumetric flask and add 10 ml of solvent than shake and sonicate, if necessary. Dilute with solvent to volume, mix and filter. Take 5 ml of this filtrated solution to a 50 ml volumetric flask and dilute with solvent up to the mark. Filter this solution with 0.45 µ membrane filter before injection.
Condition
Waters Sphreisorb  ODS2 , 5 m   4.6 mm x 250 mm / UV at 278 nm / 15 minutes.
Paracetamol           : 5.0 minutes & Caffeine       : 13.0 minutes (Approximately)

Gradient Program

Time
Flow
% A
% B
% C
% D
-
1.00
0.00
10.0
90.0
0.00
8.00
1.00
0.00
2.5
97.5
0.00
10.00
1.00
0.00
10.00
90.0
0.00
15.00
1.00
0.00
10.00
90.0
0.00

Assay Method of 
 Pefloxacin Mesylate Tablet & Solution

Standard
Dissolve about 50 mg of Pefloxacin Mesylate WS in 60 ml of 0.1M Hydrochloric acid and dilute to 100 ml with same solvent. Dilute 1 ml of the filtrate to 100 ml with 0.1M Hydrochloric acid. Measure the absorbance of sample and standard solution at 276 nm using 0.1M Hydrochloric acid as blank.
Sample
Shake a quantity of powder containing 50 mg of Pefloxacin Mesylate (1mg of Pefloxacin is equivalent to 1.288 mg of Pefloxacin Mesylate) with 60 ml of 0.1M Hydrochloric acid for 20 minutes, add sufficient 0.1M Hydrochloric acid to produce 100 ml and filter. Dilute 1 ml of the filtrate to 100 ml with 0.1M Hydrochloric acid.

Assay Method of
 Pheniramine Maleate Injection

Buffer
Take 2.528 gm Sodium Heptanesulphonate & 300 ml of Distilled water in a Plastic vat and adjust the pH to 2.5 with Phosphoric Acid then finally make the volume 500 ml with Distilled water.
Ratio   
Buffer ( 90% ) : Acetonitrile ( 10% )    
Solvent
Mobile Phase.
Standard 
22.75 mg Pheniramine Maleate ---→ 25 ml amber flask. shake for 15 minutes
Sample 
Take 1 ml Injection equivalent to 22.75 mg of Pheniramine Maleate ---→ 25 ml amber flask. shake for 5 minutes
Condition
Waters Spherisorb 10 mm ODS1 4.6 x 250 mm / UV at 264 nm / 1.0 ml/min / 20 ml / 3 minutes / 35 minutes.

Assay Method of 
 Phenobarbital Tablet

Buffer
Take 6.6 gm of Sodium trihydrate acetate and 3.5 ml glacial acetic acid  in a 1000 ml volumetric flask. Add 750 ml distilled water and dissolve by stirring. Adjust the pH 4.5±0.1 by glacial acetic acid. Finally make the volume 1000 ml by water.
Ratio   
Buffer ( 60% ) : Methanol ( 40% )    
Standard 
Take 40 mg of Phenobarbital Working Standard in a 50-ml volumetric flask. Add 30 ml of mobile phase and shake for 10 minutes and make up the volume 50 ml with the mobile phase.. Filter this solution with 0.2m syringe filters before injection.
Sample 
Take an accurately weight of powdered sample (not be crashed) equivalent to 40 mg of Phenobarbital in 50-ml volumetric flask. Add mobile phase and shake for 30 minutes and make up the volume 50 ml with the mobile phase. Filter this solution with 0.2m syringe filters before injection.
Condition
Waters Spherisorb 10 mm ODS1 4.6 x 250 mm / UV at 254 nm / 12 minutes

Assay Method of
 Pioglitazone Tablet

Buffer

Weigh about 1.15g of Di-ammonium hydrogen orthophosphate and 1.36 g Potassium di-hydrogen orthophosphate in 1000ml of water, add 1 ml of triethylamine and adjust pH to 5.0 with dilute phosphoric acid.
Ratio   
Buffer: Acetonitrile = 45 : 55
Diluents
Acetonitrile: Water = 60:40
Standard 
Accurately weigh and transfer Pioglitazone Hydrochloride working standard equivalent to about 20mg of Pioglitazone (1 mg Pioglitazone is equivalent to 1.1023 mg Pioglitazone Hydrochloride) in a 100ml volumetric flask. Add 70 ml of Diluent and shake for 25 minutes and make up the volume with diluent. Filter this solution with 0.45 m membrane filter before injection
Sample 
Accurately weigh and transfer sample equivalent to about 20mg of Pioglitazone in a 100ml volumetric flask. Add 70 ml of Diluent and shake for 25 minutes and make up the volume with diluent and then filter. Filter the filtrate with 0.45 m membrane filter before injection
Condition
Waters Spherisorb 5 mm C18 Column 4.6 ´ 250mm./ 30º C / UV at 220 nm / 12 minutes.

Assay Method of 
 Pioglitazone + Metformin Hydrochloride Tablet

Buffer

Weigh about 1.15g of Di- ammonium   hydrogen Orthophosphate and 1.36 g Potassium di-hydrogen orthophosphate in
 1000ml of water, add 1 ml of triethylamine and adjust pH to 5.0 with dilute Phosphoric acid.
Ratio   
Buffer : Acetonitrile = 50 : 50
Diluents
Methanol 
Standard 
Accurately weigh and transfer about 25.0 mg pioglitazone equivalent of pioglitazone HCl of Working Standard in a 50-ml volumetric flask. Add 30 ml  Methanol and shake for 10 minutes and make up the volume with Methanol. From these solution 10 ml was taken in a 100 ml volumetric flask containing 166.66 mg Metformin HCl of Working Standard and add 70 ml Methanol & shake well. Finally make up the volume 100 ml. by the same solvent Filter this solution with 0.45 m membrane filters before injection.
Sample 
Weigh and powder 20 tablets. Take powder-containing equivalent to 5 mg of Pioglitazone & 166.66 mg Metformin HCl in a 100-ml volumetric flask. Add 70 ml of diluents and shake for 25 minutes and make up the volume with diluents. Filter this solution with 0.45m membrane filters before injection.
Condition
Waters Spherisorb 5 mm ODS2 4.6 ´ 250mm./ 40º C / UV at 260 nm & 225 nm / 12 minutes.
3.50 min for Metformin HCl & 6.50 min. for Pioglitazone Hydrochloride (approx.)
                                               
Gradient Program

Time
Flow Rate
A (%)
B (%)
Detection
0.01
1.0 ml
50
50
260 nm
6.00
1.0 ml
50
50
260 nm
6.01
1.0 ml
50
50
225 nm
12.00
1.0 ml
5
50
225 nm









Assay Method of  
Piracetam Tablet

Buffer
Mix 500 mg K2HPO4 with 450 ml of distilled water adjusts pH 6.0 with phosphoric acid then filter through a 0.45-micron membrane filter and degas.
Ratio
10 % Acetonitrile: 90 % Phosphate Buffer pH 6.0
Solvent
Distilled Water
Standard 
Dissolve about 50mg of Piracetam WS in 100 ml volumetric flask then add 70 ml water and shake 20 minutes then up to mark 100 ml with water. Filter this solution with 0.45 m membrane filter before injection.
Sample 
Take sample powder about 50mg of Piracetam in 100 ml volumetric flask then add 70 ml water and shake 10 minutes and sonicate for 5 minutes then up to mark 100 ml with water. Filter this solution with Whattman filter paper then 0.45 m membrane filter before injection.
Condition
Waters Spherisorb 5 mm ODS2 Analytical Column (4.0 x 250 mm)./ 40 C/ UV at 205 nm / 4 minutes approx.

Assay Method of
 Pizotifen Malate Tablet

Buffer
Mix 1.5 ml of Triethylamine with 450 ml of water adjust pH 3.5 with phosphoric acid then filter through a 0.45-micron membrane filter and degas.
Ratio
Acetonitrile 60 % : Triethylamine Buffer pH 3.5  40 %.
Solvent
Mobile Phase
Standard 
Dissolve about 20mg of Pizotifen Malate WS in 100 ml volumetric flask then add 70 ml mobile phase and shake 10 minutes then up to mark 100 ml with mobile phase. Filter this solution with 0.45 m membrane filter before injection.
Sample 
Take sample powder about 20mg of Pizotifen Malate in 100 ml volumetric flask then add 70 ml mobile phase and shake 10 minutes then up to mark 100 ml with mobile phase. Filter this solution with Whattman filter paper then 0.45 m membrane filter before injection.
Condition
XTerra RP18  5µm Column (4.6 mmx 25cm)./ 40 C/ UV at 215 nm / 7 minutes

Assay Method of
 Pramoxine Hydrochloride

Solvent
Ethanol
Standard 
10 mg ---® 100 ml ---® take 10 ml ---® 50 ml (Shake – 10 minutes)
Sample 
Same as Standard. Take absorbance at 226 nanometer.

Assay Method of
 Prasugrel Hydrochloride Tablet

Buffer
Dissolve 2.0 gm of  Di ammonium hydrogen Orthophosphate and 1.0 gm of Tetra n – butyl ammonium hydrogen sulphate into 1000 ml volumetric flask & add 950 ml distilled water, adjust the pH 4.0 ± 0.05 with Ortho Phosphoric Acid &  make volume with distilled water up to 1000 ml. Filter through 0.45 m membrane filter and degasses.
Ratio   
Phosphate Buffer pH 4.0 ( 40 % ) : Acetonitrile ( 60 % )
Solvent
Mobile Phase
Standard 
Take about 20 mg of Prasugrel HCl WS into 100 ml volumetric flask. Add 70 ml of diluents & shake for 15 minutes
and then up to the mark  100 ml with mobile phase and mix well. Filter this solution with 0.45 m membrane filter before injection.
Sample 
Same as Standard.
Condition
Water Spherisorb , 10 mm ODS1 4.6 x 250 mm / 400 C/ UV at 210 nm / 7 mins appros / 20 µl / 1 ml per minute

Assay Method of
 Prednisolone Sodium Phosphate Solution

Buffer
Dissolve 6.8 gm of Potashium Di hydrogen Phosphate ( KH2PO4 )into 1000 ml volumetric flask & add 950 ml distilled water, adjust the pH 3.0 ± 0.05 with Ortho Phosphoric Acid &  make volume with distilled water up to 1000 ml. Filter through 0.45 m membrane filter and degasses.
Ratio   
Phosphate Buffer pH 3.0 ( 70 % ) : Acetonitrile ( 30 % )
Standard 
 Accurately weigh and transfer about 6.72 mg of working standard of Prednisolone Sodium Phosphate equivalent to  5mg  of Prednisolone into 100 ml amber volumetric flask. Add 70 ml of distilled water & shake for 10 minutes and then up to the mark  100 ml with distilled water and mix well. Filter this solution with 0.45 m membrane filter before injection.
Sample 
 Accurately transfer 5 ml of sample oral solution equivalent to 5 mg of Prednisolone into 100 ml amber volumetric flask. Add 70 ml of distilled water & shake for 10 minutes and then up to the mark  100 ml with distilled water and mix well. Filter this solution with 0.45 m membrane filter before injection.
Condition
XTerra  RP18 , 5 mm 4.6 x 250 mm / 400 C/ UV at 247 nm/10 minutes
                                              
Assay Method of
 Prednisolone Sodium Phosphate Tablet

Standard
Take about 10 mg of Prednisolone working standard in a 100 ml volumetric flask. Add 70 ml of distilled water & shake for 25 minutes. Then  make volume 100 ml with distilled water. Take 8 ml of the solution in a 50 ml volumetric flask. Make the volume up  to mark ( 50 ml ) with distilled water. Measure the absorbance at 246 nm taking distilled water as blank.
Sample
Weight & take the average weight of 20 tablets. Crush the tablets into powder. Take a quantity of  the powder containing equivalent to 10 mg of Prednisolone in a 100 ml volumetric flask. Add 70 ml of distilled water & shake for 25 minutes. Then  make volume 100 ml with distilled water & sonicate for 5 minutes. Take 8 ml of the solution in a 50 ml volumetric flask. Make the volume up  to mark (50 ml ) with distilled water. Measure the absorbance at 246 nm taking distilled water as blank.

Assay Method of
 Pregabalin Capsule

Buffer
Dissolve 1.2 gm of  Potashium Dihydrogen Phosphate into 1000 ml volumetric flask & add  950 ml distilled water, adjust the pH 6.9 ± 0.05 with 5M NaOH & make   volume with distilled water up to 1000 ml. Filter through 0.45 m membrane filter and   degasses.
Ratio   
Buffer ( 70% ) : Acetonitrile ( 30% )    
Diluent  
Buffer ( 70% ) : Acetonitrile ( 30% )
Standard 
Accurately weigh and transfer about 100 mg of working standard of Pregabalin into 50 ml volumetric flask. Add 30 ml of diluent & shake for 30 minutes and then up to the mark  50 ml with diluent and mix well. Filter this solution with 0.45 m membrane filter before injection.
Sample 
Take powder equivalent to 100 mg of Pregabalin into 50 ml  volumetric flask. Add 30 ml of diluent & shake for 30 minutes and then up to the mark  50 ml with diluent and mix well. Filter this solution by Whattman filter paper and finally  with 0.45 m membrane filter before injection.
Condition
C8 10 mm 4.6 x 250 mm / UV at 210 nm / 7 minutes
       
Assay Method of
 Primaquin Phosphate Tablet

Standard
Dissolve about 50 mg of Primaquin Phosphate WS in 60 ml of 0.1M Hydrochloric acid and dilute to 100 ml with same solvent. Dilute 1 ml of the filtrate to 50 ml with 0.1M Hydrochloric acid.
Sample
Shake a quantity of powder containing 50 mg of Primaquin Phosphate (1mg Primaquin is equivalent to 1.756mg Primaquin Phosphate) with 60 ml of 0.1M Hydrochloric acid for 20 minutes, add sufficient 0.1M Hydrochloric acid to produce 100 ml and filter. Dilute 1 ml of the filtrate to 50 ml with 0.1M Hydrochloric acid. Measure the absorbance of sample and standard solution at 284 nm using 0.1M Hydrochloric acid as blank.
         
 Assay Method of
   Prochlorperazine Maleate Tablet
                             .
Sample 
To a quantity of powder containing 10 mg of Prochlorperazine Maleate add 30 ml of absolute ethanol and 
1 ml of 25 % w/v ammonia solution, mix. Shake for 30 minutes; add sufficient absolute alcohol to produce 
50 ml. Mix and filter. Dilute 1 ml of the filtrate to 25 ml with absolute ethanol.
Measure the absorbance of the solution at 258 nm using ethanol as blank.
Calculation
 % of Prochlorperazine Maleate =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 620                                               

Assay Method of
   Prochlorperazine Mesilate Injection
                             .
Sample 
Carry out the following procedure protected from light. To a quantity containing 12.5 mg of Prochlorperazine Mesilate add sufficient absolute ethanol containing 0.01 % v/v of 13.5 M
ammonia to produce 100 ml. Dilute 5 ml of the solution to 100 ml with the ammoniacal ethanol.
Calculate the content of Prochlorperazine Mesilate  taking 635 as the value of A (1% , 1cm )
 at the maximum at 258 nm .
Calculation
 % of Prochlorperazine Mesilate  =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 635                                              

Assay Method of
 Prochlorperazine Mesilate Solution

Solvent
Water
Standard 
5 mg ----® 100 ml. Shake – 15 minutes.
Sample 
Same as standard. wavelength 307 nm

Assay Method of
 Procyclidine HCl  Tablet

Reagent
Bromocresol purple solution : Dissolve 250 mg of  bromocresol purple in dilute glacial acetic acid ( 1 in 50 ) to make 1000 ml
Standard
Tranfer about 25 mg of Procyclidine Hydrochloride WS in  a 100 ml volumetric flask.  Add water to volume and mix. Dilute 10 ml of this solution to 100 ml with bromocresol purple solution and mix.Conc . of standard preparation 0.0025 %
Sample
Weigh and powder 20 tablets. To a quantity of powder equivalent to  2.5  mg of Procyclidine HCl , add 10 ml of water, mix. Dilute with bromocresol purple solution to 100 ml. Mix. Allow to settle the undissolved particles. Use the supernatant liquid as directed in the procedure.
Procedure 
Transfer 5.0 ml each of the standard and  the sample preparation to individual 60 ml separators. Transfer 0.5 ml of water and 4.5 ml of bromocresol purple solution  to a third separator to provide the blank.  Extract each solution with 20 ml of chloroform and filter each extract , discarding the first 5 ml of the filtrate. Concomitantly determine the absorbance of  each filtrate in a 1 cm cell at the wave length of maximum absorbance  at about 405 nm  , against the blank.
Calculate the quantity ,in mg , of procyclidine HCl in the portion of the tablet taken by the formula :
                                                               
                                                                                0.1C (Au / As ),
in which C is the concentration , in mcg per ml , of Procyclidine RS  and Au and As are the absorbances of the solutions from the sample preparation and standard preparation  , respectively .

 Assay Method of
 Promethazine Hydrochloride Tablet & Injection
                             .
Sample 
Triturate a quantity of the powder containing 50 mg of Promethazine Hydrochloride with 10 ml of 2M hydrochloric
 acid and add 200 ml of water. Shake for 15 minutes, add sufficient water to produce 500 ml and centrifuge about 
50 ml of the mixture. To 5 ml of the clear, supernatant liquid add 10 ml of 0.1M hydrochloric acid and sufficient 
water to produce 100 ml.

Measure the absorbance of the resulting solution at the maximum at 249 nm using 0.01M hydrochloric acid as blank.
Calculation
 % of Promethazine Hydrochloride =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 910                                               

Assay Method of 
 Promethazine Hydrochloride Syrup
                             .
Reagent
Palladium (II) Chloride reagent :
Dissolve, with gentle heating 0.100 g of Palladium (II) chloride in 50 ml water and 1 ml conc. of Hydrochloric
 acid. Cool and dilute to 100 ml with water. 
Blank
To 5 ml of palladium chloride add water to make the volume 25 ml and mix.
Calculate the content of  Promethazine HCl taking 110 as the value of A (1% , 1cm ) at the maximum at 472 
nm .
System
Dilute 10 ml sample to 50 ml with water. Take 5 ml of the resulting solution in a 25 ml of volumetric flask.
 Add  5 ml of Palladium chloride  and water to make the volume. Mix. Measure the absorbance at 472 nm 
Conc. 0.004 %
Calculation  
% of Promethazine HCl  = Absorbance   x 100 / conc. in gm per 100 ml x  110

Assay Method of
   Propranolol Hydrochloride Tablet
                             .
Sample 
Weigh and powder 20 tablets. Shake a quantity of powder containing 20 mg of Propranolol Hydrochloride
 with 20 ml of water for 10 minutes.  Add 50 ml of methanol, shake for further 10 minutes, add sufficient 
methanol to produce 100 ml. Mix and filter. Dilute 10 ml of the filtrate to 50 ml with methanol and
 measure the absorbance of the resulting solution at 290 nm.Calculate the content of Propranolol 
Hydrochloride taking 206 as the value of A (1%, 1 cm) at 290 nm.
Calculation
 % of Propranolol Hydrochloride =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 206                                               

Assay Method of
   Pseudoephedrine Hydrochloride Tablet

Sample
Take the weigh of   20 tablets & determine the average weight. Then crush them into fine powder. Take powdered sample equivalent to 30 mg of Pseudoephedrine Hydrochloride and dissolve in a mixture of 30 ml Glacial Acetic Acid and 10 ml of Mercuric Acetate solution which is previously neutralized. Titrate with 0.1 N Perchloric acid and determine the end point potentiometrically using crystal violet as an indicator. 1 ml 0.1N Perchloric acid VS ≡ 20.17 mg of Pseudoephedrine Hydrochloride

Assay Method of
   Pseudoephidrine HCl +  Loratadine Tablet

Buffer

Dissolve 1.750 gm of Di Potassium dihydrogen orthophosphate with 950 ml  distilled water into 1000ml volumetric flask, adjust the pH 5.5 ± 0.05 with dilute Phosphoric Acid  & make volume with distilled water up to 1000  ml.         
Ratio   
Methanol : Buffer = Time Programming
Diluents
Methanol 
Standard 
Take 5 mg of Loratadine WS & 120 mg Pseudoephidrine HCl in a 50 ml volumetric flask. Add 30 ml of methanol & Shake for 10 minutes & make volume up to the mark with  Solvent.  Filter this solution with 0.45 m membrane filter before injection.
Sample 
Weigh & take the average weight of 20 tablets. Crush the tablets into powder. Take a quantity of the powder containing equivalent to 5 mg of Loratadine WS & 120 mg  Pseudoephidrine  HCl in a 50 ml volumetric flask. Add 30 ml of methanol & Shake for 10 minutes & make volume up to the mark with  Solvent. Filter this solution with 0.45 m membrane filter before injection.
Condition
XTerraÒ RP18 5mm 4.6 ´ 250mm./ 40º C / UV at 258 nm / 15 minutes.
4 minutes for Pseudoephedrine HCl & 9 minutes for Loratadine (approx.)
Gradient Program
Time
Flow Rate
A (%)
B (%)
0.00
1.2
40
60
10.00
1.2
100
0
10.01
1.2
40
60
15.00
1.2
40
60




Assay Method of
 Pseudoephedrine Hydrochloride  + Loratadine Tablet

Buffer

Dissolve 1.750 gm of Di Potassium dihydrogen orthophosphate with 950 ml  distilled water into 1000 ml volumetric flask, adjust the pH 5.5 ± 0.05 with dilute Phosphoric Acid  & make volume with distilled water up to 1000  ml.         
Ratio   
Mobile Phase   A :   Methanol
Mobile Phase   C :   Buffer pH 5.5
Standard 
Take 10 mg of Loratadine WS & 240 mg Pseudoephidrine HCl in a 50 ml volumetric flask. Add 30 ml of methanol & Shake for 10 minutes & make volume up to the mark with Solvent.  Filter this solution with 0.45 m membrane filter before injection.
Sample 
Weigh & take the average weight of 20 tablets. Crush the tablets into powder. Take a quantity of the powder containing equivalent to 10 mg of Loratadine WS & 240 mg Pseudoephidrine  HCl in a 50 ml volumetric flask. Add 30 ml of methanol & Shake for 10 minutes & make volume up to the mark with Solvent. Filter this solution with 0.45 mm membrane filter before injection.
Condition
m Bondapack 125A° 5mm  3.9 x 300  mm Analytical Column / UV at 258 nm / 15 minutes
Pseudoephedrine HCl  : 2.5 minutes & Loratadine  : 9 minutes (approximately)
                                                                    
Gradient Program
Time
Flow Rate
A (%)
B (%)
C (%)
D (%)
0.00
1.2
40
0
60
0
10.00
1.2
100
0
0
0
10.01
1.2
40
0
60
0
15.00
1.2
40
0
60
0

                        
Assay Method of
 Pyrazinamide Tablet
                             .
Sample 
To a quantity of the powder containing 0.1 g of Pyrazinamide add 200 ml of water, allow to stand for 10 minutes, swirling occasionally, mix with the aid of ultrasound for 10 minutes and dilute to 500 ml with water. Filter and discard the first 20 ml of filtrate. Dilute 5 ml of the filtrate to 100 ml with water.Measure the absorbance of the solution at 268 nm using water as blank.
Calculation
 % of Pyrazinamide =  Absorbance of Sample ´ 100 / Conc. Of spl. ´ 650                                              

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