Assay Method of
Pantoprazole Sodium / Solution
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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
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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