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Sample
|
Take average weight of 20 tablet and crush in a mortar to
achieve fine powder. Take equivalent amount of tablet powder containing 150
mg of Ursodeoxycholic Acid in 50 ml Ethanol R into 250ml titration vessel,
previously neutralized to 0.2 ml of phenolphthalein solution R. Add 50 ml of
Distilled Water and Titrate with 0.1M Sodium Hydroxide VS until a pink color
is obtained.
Each ml
of 0.1M Sodium Hydroxide VS is equivalent to 39.26 mg of Ursodeoxycholic
Acid.
|
Buffer
|
Dissolve about 3.854 g of Ammonium Acetate in 900 ml
water. Adjust pH to 5.0±0.05 with dilute acetic acid and
dilute to 1000 ml with water.
|
Ratio
|
Mix 50 volume of Buffer with 50 volume of methanol and
filter through a 0.45-micron membrane filter and degas.
|
Standard
|
Dissolve about 25.0 mg of valdicoxib WS in 50 ml of
methanol and dilute to 100 ml with water. Dilute 5 ml to 50 ml with mobile
phase. Filter this solution with 0.45 m
membrane filter before injection.
|
Sample
|
Shake a quantity of the powdered sample containing about
25.0 mg of Valdicoxib in 50 ml of methanol for 30 minutes, dilute to 100 ml
with water and then filter. Dilute 5 ml of filtrate to 50 ml with mobile
phase. Filter this solution with 0.45 m
membrane filter before injection.
|
Condition
|
C18 Column (4.6 mmx 25cm) & 10µm (ODS1)./ UV at 245
nm
|
Sample
|
Weigh
& take the average weight of 20 tablets. Crush the tablets into fine
powder. Take a quantity of the powder containing equivalent to 58 mg of
Valproic acid into a 200 ml volumetric flask. Add accurately 100 ml of
ethanol 96%. Shake for 20 minutes & filter. Take 50 ml of filtrate
solution in 100 ml conical flask & add 1 ml of 1% Phenaphaline solution
as indicator. Titrate with 0.1M Sodium hydroxide VS to a pink color end
point. Perform blank titration for necessary correction.
Each ml of 0.1M Sodium hydroxide VS º 14.42 mg of Valproic
Acid
|
Sample
|
Weigh
& take the average weight of 20 tablets. Crush the tablets into fine
powder. Take a quantity of the powder containing equivalent to 66.8 mg of
Sodium valproate into a 100 ml glass vessel. Add 60 ml of glacial acetic acid
& shake for 20 minutes. Titrate with 0.1M Perchloric Acid vs using crystal violet solution as indicator.
Perform blank titration for necessary correction.
Each ml
of 0.1M Perchloric Acid VS º
16.62 mg of Sodium valproate.
|
Sample
|
Shake a quantity of the powder containing 100 mg of
Verapamil Hydrochloride
with 150 ml of 0.1 M hydrochloric acid for 10 minutes; add sufficient 0.1 M hydrochloric acid to produce 200 ml and filter. Dilute 10 ml of the filtrate to 100 ml with water.Measure the absorbance of the resulting solution at the maximum at 278 nm using 0.1 M hydrochloric acid as blank. |
Calculation
|
% of Verapamil
Hydrochloride=Absorbance of Sample´100/Conc. Of spl.´118
|
Solvent
|
Chloroform
|
Standard
|
50 mg
----® 100 ml ----®
take 5 ml ----® 50 ml (Shake 20 minutes)
|
Sample
|
Same as
standard. Take absorbance at 336 nm.
|
Sample
|
Take 35 ml of Nid Syrup equivalent to about 70 mg of
Elemental Zinc (35ml) in a 250 ml conical flask. Add 100 ml distilled water
& mix well. Then add 5 ml of Ammonia - Ammonium Chloride buffer TS and
using 0.1 ml of Erio-Chrome Black TS as
indicator. Titrate immediately with 0.05M Na2EDTA VS. At the end point
the solution become violet to deep blue. Each ml of 0.05M Na2EDTA VS is
equivalent to 3.269 mg of elemental Zinc.
% of Zinc = Required
Vol. Of VS x Constant x F x 100 / Weight of Elemental Zinc in sample Solution
|
Buffer
|
Take 1.25 gm Di-Sodium hydrogen
orthophosphate & 0.125 gm Potassium di-hydrogen orthophosphate in 500ml
of water & adjust the PH to 4.0 with dilute phosphoric acid. Filter through 0.45 m
membrane filter and Degasses.
|
Ratio
|
Methanol : Buffer = 60 : 40
|
Diluents
|
Methanol
|
Standard
|
Accurately
weigh and transfer about 20 mg Tamsulosin HCl Working Standard in a 100-ml
Volumetric flask. Add Diluents and shake for10 minutes and make the volume up
to mark & mix well. Transfer 4 ml of this solution in a 100 ml volumetric
flask and add diluents up to the mark
(100 ml) & mix well. Filter this solution with 0.45m
membrane filters before injection
|
Sample
|
Weigh
and powder 20 tablets. Take powder-containing equivalent to 0.4 mg of
Tamsulosin HCl in a 50-ml volumetric flask. Add Diluents (Methanol HPLC
grade) and shake for 30 minutes & degasses for 10 minutes and make the
volume up to mark & mix well. Filter the solution through whatman filter paper no.1 and half
of Filter this solution with 0.45m membrane filters before injection
|
Condition
|
Waters
Spherisorb 10.0 mm ODS2 4.6 ´
250mm./ UV at 225 nm / 15 minutes.
|
Buffer
pH 3.5
|
Dissolve 3.4 gm Potassium Dihydrogen Phosphate in 1000 mL
of water. Add 1.0 mL of Triethylamine and adjust
pH to 3.5 with dilute ortho Phosphoric acid.
|
Ratio
|
Buffer 60 % : Acetonitryl 40 %
|
Diluents
|
Methanol
|
Standard
|
Weigh accurately about 50 mg Telmisartan WS and transfer
it in a 100 ml volumetric flask. Add 50 ml 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 50 mg
Telmisartan 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
|
Luna C18 5µm. 4.6 × 250mm. / 230 nm / 1ml per minute / 20
mL / 25 minutes / 19 minutes (Approx.)
|
Sample
|
Take powdered sample equivalent to 90 mg of Tenoxicam and
dissolve in a mixture of 70 ml Glacial Acetic Acid and 5 ml of Formic Acid
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 ≡ 33.74 mg
of Tenoxicam
|
Solvent
|
Methanol
|
Standard
|
50 mg
---® 100 ml ---®
take 1 ml ---® 50 ml ---®
take 5 ml ---® 50 ml
|
Sample
|
Same as Standard. Take
absorbance at 223 nanometer.
|
Sample
|
Weigh and powder 20 capsules. Take powder equivalent to 50 mg of Tetracycline Hydrochloride in 100 ml volumetric flask. Add 60 ml of
0.1N Hydrochloric acid and shake for
20 minutes. Make the volume up to 100 ml with the same solvent . Mix and
filter. Dilute 1 ml of the filtrate to 50 ml with 0.1N Hydrochloric acid . Measure absorbance
at 274 nm , taking 0.1N Hydrochloric acid
as Blank .
% of content
= Absorbance x 100 / conc. in g /100 ml x 387
|
Buffer
|
Add 1 ml triethylamine in 500
ml of water and adjust the PH
3.0( ±0.05) with dilute phosphoric acid.
|
Ratio
|
Acetonitrile : Buffer in the proportion of 70 : 30
|
Diluents
|
Acetonitrile : Buffer in the proportion of 70 : 30
|
Standard
|
Accurately weigh and transfer about 25 mg of Tiemoniun
methylsulphate working standard
in a 100 ml volumetric flask .Add 70 ml diluents and shake for 10
minutes and make the volume up to the mark with the same solvent. Filter this
solution with 0.20 m membrane filter before injection.
|
Sample
|
Weigh and make fine powder of 20 tablets. Take an accurately weighed
portion of powder equivalent to 25 mg of Tiemoniun methylsulphate in a 100 ml volumetric
flask. Add 70 ml of diluents and shake for 10 minutes . Adjust the volume to100 ml with the same solvent .Then
degassed it for 15 minutes. Filter the solution by Whatman filter paper. Further
filter this solution with 0.20 m membrane filter before
injection.
|
Condition
|
XTerra®
RP18 ,5 mm 4.6 ´ 250mm./ UV at 235 nm /
8 minutes
|
Solvent
|
water
|
Standard
|
50 mg
---® 100 ml ---®
take 5 ml ---® 100 ml (Shake 20 minutes)
|
Sample
|
Same as Standard. Take
absorbance at 235 nanometer.
|
Buffer
|
Dissolve 6.8 gm Monobasic potassium phosphate[ KH 2 PO4 ]in 500 ml of water and make
up to 1000 ml with water. Adjust pH
of this solution to 7.5 ± 0.1with potassium hydroxide.
|
Ratio
|
Accetonitrile
: Buffer º 50
: 50
|
Diluents
|
Accetonitrile : Buffer º 20 : 80
|
Standard
|
Weight and transfer about 25 mg working standard
of Tizanidine in a 100 ml volumetric
flask. Add 70 ml of solvent and
shake for 20 minutes and dilute with solvent up to the mark and mix well.
Take 5 ml solution in a 50 ml volumetric flask and dilute with solvent 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 25 mg Tizanidine in a 100 ml volumetric
flask. Add 70 ml solvent and shake for 30 minutes and dilute
with solvent up to the mark and mix well. Filter the solution by
whatman filter paper and take 5 ml solution in a 50 ml volumetric flask and
dilute with solvent and mix well. Finally filter this solution with 0.45 m membrane filter before injection.
|
Condition
|
XTerra RP18 ,
5 mm 4.6 ´
250mm./ 40°C / UV at
230 nm / 8 minutes.
|
Buffer
|
Transfer 1.36 gm of Sodium acetate trihydrate to a 1000
ml volumetric flask add about 200 ml of distilled water and shake until
dissolution is complete and volume up to 1000 ml with distilled water .
|
Ratio
|
Mix buffer solution and acetonitrile (70 : 30 ) filter through 0.45 m membrane filter and degasses.
|
Diluents
|
Mobile Phase
|
Standard
|
Weight and transfer about 50 mg working standard of
Theophylline in a 50 ml volumetric
flask. Add 30 ml of Mobile Phase and shake for 20 minutes and dilute
with Mobile Phase up to the mark and
mix well. Take 5 ml solution in a 50 ml volumetric flask and up to the mark
with Mobile Phase 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 Theophylline in a
50 ml volumetric flask. Add 30 ml Mobile Phase and shake for 30 minutes
and dilute with Mobile Phase up to the mark and mix
well. Filter the solution by whatman filter paper and take 5 ml filtrate
solution in a 50 ml volumetric flask and up to the mark with Mobile Phase and
mix well. Finally filter this solution with 0.45 m membrane filter before injection.
|
Condition
|
Waters Sphreisorb ODS1 , 10 m 250 x 4.6 mm./ 40°C / UV at 280 nm / Theophylline = 3.5 minutes.
|
Sample
|
Dissolve powdered sample equivalent to 100 mg Tolperiaone
Hydrochloride in previously neutralized mixture of 60 ml glacial acetic acid
and acetic anhydride (40 ml + 20 ml) using crystal violet solution as
indicator. Titrate with 0.1 M perchloric acid and determine the end
point.Each ml of 0.1M perchloric acid VS is equivalent to 28.183 mg of
Tolperiaone Hydrochloride.% of content =
V x F x 28.183 x 100 / W
|
Sample
|
Weigh 20 Suppositories and then cut in to small pieces.
Take about 1.4 gm sample equivalent to 100 mg Tramadol Hydrochloride in a
warm mixture of 25 ml Glacial Acetic Acid, 10 ml Acetic Anhydride and
carryout non aqueous titration, determining the end point Potentiometrically.
Perform a reagent blank use Crystal violet indicator if necessary.
Each ml
of 0.1 M Perchloric acid VS is equivalent to 29.98 mg of Tramadol
Hydrochloride
|
Solvent
|
Water
|
Standard
|
50 mg
----® 100 ml ----®
take 10 ml ----® 50 ml (Shake 15 minutes)
|
Sample
|
Same as
standard. Take absorbance at 272 nm.
|
Buffer
|
Take 6.805 gm & Potassium Dihydrogen Phosphate in
a 1000ml volumetric flask and adjust the volume with Distilled water &
adjust the pH 4.5 with Phosphoric Acid.
|
Ratio
|
ACN : Buffer = 40: 60
|
Standard
|
Accurately weigh and transfer about 25 mg of
working standard of Trimetazidine.Dihydrochloride into 50 ml volumetric flask Add 35 ml of Methanol & shake for 20 minutes and dilute with Methanol up to the mark and
then sonicate for 20
minutes Take 2 ml of the solution in a 50 ml volumetric flask. Volume
up to mark with Methanol .Filter this solution with 0.25 m
membrane filter before injection.
|
Sample
|
Weigh of 10 tablets and make it powder. Take powder-containing equivalent
to 25 mg of Trimetazidine Dihydrochloride in a 50-ml volumetric flask. Add 35 ml of
Methanol & shake for 20 minutes. Dilute with Methanol up to the mark then Sonicate this Solution for 20 minutes & filter with Whitman filter
paper .Take 2 ml of the solution in a 50 ml volumetric flask. Make the
volume up to mark with Methanol.
Filter this solution with 0.25 mm
membrane filter before injection.
|
Condition
|
Waters Spherisorb 10 mm
ODS1 4.6 ´
250mm./ 40º C / UV at 210 nm / 10 minutes.
|
