Assay Method of
Magnesium Hydroxide Tablet
Sample
|
Take a volume of test solution equivalent to 20 mg of
magnesium hydroxide in a 250 ml conical flask. Add 100 ml of water and 10 ml
of triethanolamine and stir. Add 5 ml of Ammonium - ammonium chloride buffer
TS & 3 drops of eriochrome black indicator solution. Cool the solution
between 3° & 4°C by immersion of
the flask in an ice bath. Then remove & titrate with 0.05 M Na2EDTA VS
until a blue color produced. Each ml of 0.05 M Na2EDTA VS º
2.916 mg of Magnesium Hydroxide.
% of Mg(OH)2
= No. of ml of 0.05 M Na2EDTA
VS x F x 2.916 x 100 / Amount of Mg(OH)2
taken
|
Indicator
|
Dissolve 200 mg of eriochrome black T in a mixture of 15
ml of triethanolamine and 5 ml of dehydrated alcohol & mix.
|
Assay Method of
Mebendazole Syrup
Standard
|
10 mcg /ml of Mebendazole RS in 0.1N Methanolic Hydrochloric acid TS. (
0.001 % conc. )
|
Sample
|
Take suspension
equivalent to 100 mg of
Mebendazole in 100 ml volumetric flask. Add 60 ml of 0.1N Methanolic
Hydrochloric acid. and shake for 15 minutes. Make volume up to 100 ml
with 0.1N Methanolic Hydrochloric acid
. Filter.Dilute 1 ml of the filtrate to 100 ml with 0.1N Methanolic Hydrochloric acid .Measure
the absorbance of the resulting solution at the maximum at 247 nm., taking
0.1N Methanolic Hydrochloric acid as reagent blank.
|
Assay Method of
Mebeverine
Hydrochloride Tablet
Sample
|
Weigh and powder 20 tablets. Heat a quantity of powder equivalent to 500 mg of Mebeverine hydrochloride with 100 ml of 0.1M
hydrochloric acid for 10 minutes on water bath , shaking occasionally. Cool ,
add sufficient 0.1M hydrochloric acid to produce 250 ml . Mix and filter. To 10 ml of the filtrate
add sufficient 0.1M hydrochloric acid to produce 100 ml and dilute 15 ml of
the resulting solution to 100 ml with the same solvent. Measure the
absorbance of the solution at 263 nm . Calculate the content of Mebeverine
Hydrochloride taking 263 as the value of A (1%, 1cm ) at the maximum at 263
nm .
|
Calcula.
|
% of content
= Absorbance of sample x
100 / conc. in g /100 ml x 263
|
Assay Method of
Mebeverine
Hydrochloride SR Capsule
Standard
|
Accurately weigh and transfer about 75 mg of working
standard of Mebeverine Hydrochloride into 100 ml volumetric flask. Add 70 ml
of 0.1 M HCl and shake. Adjust the volume up to the mark with the same
solvent. Dilute 1 ml of this solution to 50 ml volumetric flask with 0.1 M
HCl.
|
Sample
|
Take 20 Capsules & determine the average content
weight. Powder the pellets & transfer powdered sample equivalent to 75 mg
of Mebeverine hydrochloride into a 100 ml volumetric flask. Add 70 ml of 0.1
M HCl and shake for 30 minutes. Adjust the volume up to the mark with the
same solvent. Filter the solution. Take 1 ml of the filtrate into a 50 ml
volumetric flask. Make the volume up to the mark with 0.1 M HCl & mix
well.
|
Calcula.
|
Measure the absorbance of both Standard and sample
solution in a UV-Visible Spectrophotometer having 1 cm cell at a wavelength
of 263 nm using 0.1 M HCl as blank solution.
|
Assay Method of
Meclozine Hydrochloride Tablet
Buffer
|
Weigh about 3.45 gm of Monobasic
Sodium Phosphate in 500 ml of water, and adjust pH to 4.0 with dilute
Phosphoric acid.
|
Ratio
|
Buffer: Methanol = 20: 80
|
Diluents
|
Methanol and
Water
|
Standard
|
Accurately
weigh and transfer about 62.5 mg of Meclozine Hydrochloride Working Standard
in a 100-ml volumetric flask. Add 50 ml of methanol and shake for 10 minutes
and make up the volume with the water. Take 10 ml of this solution into a 50
ml volumetric flask and make up the volume with water Filter this solution
with 0.45m membrane filters before injection.
|
Sample
|
Weigh
and powder 20 tablets. Take powder-containing equivalent to 62.5 mg of
Meclozine Hydrochloride in a 100-ml volumetric flask. Add 50 ml of methanol
and shake for 10 minutes and make up the volume with the water. Filter this
solution with the whatman filter paper. From the filtrate take 10 ml of
solution into a 50 ml volumetric flask and make up the volume with water
Finally filter this solution with 0.45m
membrane filters before injection.
|
Condition
|
Waters
Spherisorb 10 mm C8 4.6 ´
250mm./ 40°C / UV at
230 nm / 15 minutes.
|
Assay Method of
Mecobalamin Tablet
M. Phase
|
Methanol: Water = 35: 65
|
Ratio
|
Buffer : Acetonitrile = 60 : 40
|
Diluents
|
Take 200 ml Methanol in 500ml volumetric flask and made volume
with water.
|
Standard
|
Accurately
weigh and transfer about 15 mg Mecobalamin INN Working Standard in 50ml Amber Volumetric
flask. Add 30 ml Diluents and shake for 10 minutes and make the volume up
to mark &mix well & Dilute
5ml to 50 ml with Diluents within 5 minutes.. Filter this solution with 0.25m
membrane filters before injection within 5 minutes.
|
Sample
|
Take
powder-containing equivalent to 3 mg of Mecobalamin in a 100 ml Amber volumetric flask. Add 70
ml of diluents & shake for 10 minutes. Dilute with Diluents up to the mark
& filter with Whitman filter paper within 5 minutes. Filter This solution
with 0.25 m membrane filter before injection within 5minutes.
|
Condition
|
Waters
Spherisorb 10 mm ODS1 4.6 ´
250mm./ 40º C / UV at 266 nm / 15 minutes.
|
Gradient Program
Serial No
|
Time
(minutes)
|
Flow
|
%of A Pump
(Solvent- Methanol)
|
% of B Pump
(Solvent- Water)
|
1
|
1.0
|
35.0 %
|
65.0%
|
|
2
|
8.00
|
1.0
|
35.0 %
|
65.0 %
|
3
|
8.01
|
1.0
|
70.0 %
|
30.0 %
|
4
|
14.00
|
1.0
|
70.0 %
|
30.0 %
|
5
|
14.01
|
1.0
|
35.0 %
|
65.0%
|
6
|
20.00
|
1.0
|
35.0 %
|
65.0 %
|
Assay Method of
Mecobalamin Injection
M. Phase
|
Methanol: Water = 65: 35
|
Diluents
|
Distilled Water.
|
Standard
|
Accurately weigh and transfer about 12.5 mg
Mecobalamin INN Working Standard in 25-ml Amber Volumetric flask.
Add Diluents and shake for 15 minutes and make the
volume up to mark & mix well. Filter this solution with 0.25m
membrane
filters before injection.
|
Sample
|
Take 10
ml Injection in an amber Biker. Filter this solution with 0.25m
membrane filters before injection.
|
Condition
|
Waters Spherisorb 10 mm
ODS1
4.6 ´
250mm./ 40º C / at 550 nm / 7 minutes / Inject. 100 ml.
|
Assay Method of
Mefenamic Acid / Tablet + Suspension
Standard
|
Take 50 mg of Mefenamic Acid working standard in a 100 ml
volumetric flask. Add 70 ml of diluent. Shake for 15 minutes. Add diluent to
make volume 100 ml. Take 2 ml of the solution in a 50 ml volumetric flask.
Make the volume up to mark (50 ml) with same diluent. Measure the absorbance
at 350 nm taking above diluent as blank.
|
Sample
|
Weigh and powder 20 tablets. Take a quantity of the
powder containing 50 mg of Mefenamic Acid in a 100 ml volumetric flask. Add
70 ml of diluent. Shake for 15 minutes. Add diluent to make volume 100 ml.
Filter the solution. Take 2 ml of filtered solution in a 50 ml volumetric
flask. Make the volume up to mark (50 ml) with same diluent. Measure the
absorbance at 350 nm taking above diluent as blank.
|
Assay Method of
Meropenem Injection
Buffer
|
Take 1 ml triethylamine into a
1000 ml flask add 950 ml water then adjust pH 5.0 with phosphoric acid then
volume 1000 ml with water.
|
M. Phase
|
Methanol: Buffer pH – 5.0 = 25:
75
|
Diluents
|
Only Buffer pH – 5.0
|
Standard
|
Accurately weigh and transfer about 25 mg Meropenem for
injection ( with sodium carbonate buffer ) USP Working
Standard in 50 ml Volumetric flask.Add Diluents and shake
for 10 minutes and make the volume up to mark & mix well.
Filter this solution with 0.45mmembrane
filters before injection.
|
Sample
|
Same as standard preparation.
|
Condition
|
Waters Spherisorb 10 mm
ODS1
4.6 ´ 250mm./
at 300 nm / 10 minutes / Inject. 20 ml.
|
Assay Method of
Methyl Dopa Tablet
Glycin Buffer
|
Mix 42 g of sodium hydrogen carbonate and 50 g of
potassium hydrogen carbonate with 180 ml of water and add a solution
containing 37.5 g of glycine and 15 ml of 13.5M ammonia in 180 ml of water.
Dilute to 500 ml with water and stir until solution is complete.
|
Standard
|
Dissolve a 0.1 g of anhydrous methyldopa WS completely in
sufficient 0.05M sulphuric acid to produce 100 ml and filter. To 5 ml of the
filtrate add 2 ml of iron(II) sulphate-citrate solution, 8 ml of glycine
buffer solution and sufficient water to produce 100 ml.
|
Sample
|
Dissolve a quantity of the powder containing the
equivalent of 0.1 g of anhydrous methyldopa as completely as possible in sufficient
0.05M sulphuric acid to produce 100 ml and filter. To 5 ml of the filtrate
add 2 ml of iron(II) sulphate-citrate solution, 8 ml of glycine buffer
solution and sufficient water to produce 100 ml. Measure the absorbance of
the resulting solution at the maximum at 545 nm using
|
Blank
|
Dilute 2 ml of iron(II) sulphate-citrate solution, 8 ml
of glycine buffer solution to 100 ml with water.
|
Assay Method of
Methyl Ergonovine Maleate Tablet
.
Sample
|
Weigh & powder 20 tablets . Dissolve a quantity of
powder equivalent to 2 mg of Methyl Ergometrine Maleate in 50 ml of a 1 % w/v solution of tartaric acid. Mix
and filter . To 3 ml add 6 ml of dimethylaminobenzaldehyde solution , mix,
cool in running water for five minutes, add sufficient
dimethylaminobenzaldehyde solution to produce 10 ml ( Solution A ). At the
same time prepare two similar solutions, one with Methyl Ergometrine Maleate
RS (Solution B ) and the other without
the substance being examined. ( Solution C ) .
Measure the absorbance
of Solution A & B at 590 nm, using solution C as the blank,
|
Assay Method of
Methyl Ergonovine Maleate
Injection
.
Standard
|
Dissolve 25 mg of Methyl Ergonovine Maleate in 50 ml of water . Dilute
4 ml to 50 ml with water .
|
Sample
|
Dilute a quantity of
sample equivalent to 2 mg of Methyl Ergonovine Maleate ( 10 ml ) in 50
ml of water. Mix . To 3 ml add 6 ml of
dimethylaminobenzaldehyde solution ( # solution ) , mix, cool in running
water for five minutes, add sufficient di-methylaminobenzaldehyde solution to
produce 10 ml ( Solution A ). At the same time prepare two similar solutions,
one with Methyl Ergonovine Maleate WS (Solution B ) and the other
without the substance being examined.
( Solution C ) .Measure the absorbance
of Solution A & B at 590 nm, using solution C as the blank,
|
# solution
|
Dissolve 0.125 mg of 4-Dimethyl benzaldehyde in a cooled
mixture of 35 ml water and 65 ml of sulphuric acid. Add 0.1ml of 5 % w/v
solution of iron (III) chloride
hexahydrate .Allow to stand for 24
hours, protect from light , before use. Discard the solution if any yellow
colour appears.
|
Assay Method of
Metoclopramide HCl Syrup
Reagent
|
01. 1 % w/v Sodium Nitrite 02. 5 % w/v of Ammonium Suphamate 03. 0.5 % w/v solution of N-(2-naphthyl) ethylenediamine
dihydrochloride in 1M Hydrochloric acid and All reagents should be freshly prepared
.
|
System
|
Protect the solutions from light . Dilute a quantity of
sample solution containing 10 mg of Anhydrous Metoclopramide HCl to 100 ml with water. To 5 ml of this
solution add 5 ml of M hydrochloric acid , mix . Add 5ml of sodium nitrite
solution , mix and allow to stand for 20 minutes . Add 5 ml of
Ammonium sulphamate solution , mix and allow to stand for 25 minutes.
Add 5 ml of N-(2-naphthyl)
ethylenediamine dihydrochloride solution
, mix and dilute with water to 100 ml . Allow to stand for 5
minutes.Measure the absorbance of the resulting solution at the maximum at
534 nm , using water in the reference cell. Calculate the content of Metoclopramide Hydrochloride from the absorbance obtained by repeating the procedure using 5
ml of 0.01 % w/v solution of Metoclopramide Hydrochloride RS in place of the
solution being examined.
|
Assay Method of
Metformin Hydrochloride Tablet
.
Sample
|
Shake a quantity of the powder containing 0.1 g of Metformin
Hydrochloride with 70 ml of water for 15 minutes, dilute to 100 ml with water
and filter, discarding the first 20 ml. Dilute 10 ml of the filtrate to 100
ml with water and dilute 10 ml of the resulting solution to 100 ml with
water. Measure the absorbance of the resulting solution at the maximum at 232
nm using water as blank.
|
Calculation
|
% of Metformin
Hydrochloride = Absorbance of Sample ´ 100
/ Conc. Of spl. ´ 798
|
Assay
Method of
Metronidazole Tablet
.
Sample
|
Take powder equivalent to 50 mg of metronidazole in a 100ml volumetric
flask. Add 60 ml of 0.1M hydrochloric acid.
Shake for 15 minutes. Make the volume up to 100ml with 0.1M
hydrochloric acid. Mix and filter. Dilute 1 ml of the filtrate to 50 ml with
0.1M hydrochloric acid. Measure the absorbance of the resulting solution at
277 nm using 0.1M hydrochloric acid as blank.
|
Calculation
|
% of Metronidazole = Absorbance of Sample ´ 100
/ Conc. Of spl. ´ 375
|
Assay Method of
Metronidazole Suspension
.
Sample
|
Take suspension
equivalent to 100 mg of metronidazole
in a 250 ml separating funnel. Rinse the pipette with 10 ml of water.
Extract two times each with 40 ml of chloroform. Collect the extracts in a
400 ml beaker and evaporate the extracts to dryness on a water bath. Dissolve
the residue in 30 ml of anhydrous glacial acetic acid. Titrate with 0.1N
perchloric acid VS using naptholbenzein solution as indicator.1 ml of 0. 1N
perchloric acid VS equivalent to
17.12 mg of metronidazole.
|
Calculation
|
% of content
= No. of ml of 0.1N perchloric
acid VS x F x 17.12 x 100 / 100 mg
|
Assay Method of
Miconazole / Gel
or Miconazole Nitrate +
Hydrocortisone Cream
Buffer
|
For 1 liter buffer take about 6 gm of Ammonium Acetate in
the mixer of 550 ml distilled water & 450 ml methanol, then shake for 5
minutes for properly dissolve finally filter & sonicate this buffer
solution.
|
Ratio
|
Buffer 45 % : Acetonitrile 55 %
|
Diluents
|
Methanol
|
Standard
|
Dissolve about 25 mg of Hydrocortisone ( 1 mg
Hydrocortisone ≡ 1.116 mg Hydrocortisone Acetate ) WS & 50 mg of
Miconazole Nitrate WS in a 50 ml volumetric flask then add 35 ml methanol and
shake for 25 minutes and dilute with methanol up to mark 50 ml and mix well
finally filter this solution with 0.20 micron membrane filter before
injection.
|
Sample
|
Take about 2.5 gm of sample cream equivalent to 25 mg of
Hydrocortisone & 50 mg of Miconazole Nitrate in a 50 ml volumetric flask
then add 35 ml methanol and shake for 25 minutes and dilute with methanol up
to mark 50 ml and mix well, filter this solution with whattman filter paper
& finally filter this solution with 0.20 micron membrane filter before
injection.
|
Condition
|
Waters Spherisorb 5 mm
ODS2 4.6 ´ 250mm./ 50°C / UV at 235 nm 3 minutes for Hydrocortisone
& 7 minutes for Miconazole Nitrate ( Approximately)
|
Assay Method of
Midazolam Tablet
.
System
|
Take standard & sample as concentration = 0.001%
Solvent = 0.1 M HCl
Wave Length = 258 nm
|
Assay Method of
Mizolastine Tablet
Buffer
|
Transfer accurately weighed about 1.70 gm of
potassium Dihydrogen orthophosphate (KH2PO4) in 450 ml purified
water, mix well. Adjust PH to 3.5 ±
0.05 with orthophosphoric acid and dilute to 500 ml with distilled water.
Filter
through a 0.45mm
membrane filter.
|
Ratio
|
Buffer : Acetonitrile in the proportion of 70 : 30
|
Standard
|
Weigh
accurately about 10mg Mizolastine WS and transfer in a 25ml volumetric flask.
Add 15 ml of mobile phase. Shake for 25min. Then add same diluent to make 25
ml. Mix and filter this solution with 0.45mm membrane filter before
injection.
|
Sample
|
Take 20 tablets in a mortar and finely crushes
with passel. Take accurately weight of the Tablet powdered sample
containing about 10mg Mizolastine and transfer in
a 25 ml volumetric flask. Add 15ml of
mobile phase. Shake for
25min and add same diluent to make 25 ml. Mix and
filter with whatman filter paper. Filter this resultant solution
with 0.45 mm membrane filter before
injection .
|
Condition
|
ODS1 , 5 m 4.6 x 250 mm / UV at
212 nm/10 minutes
|
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