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REPORT:
2. ASSAY OF ASPIRIN
REPORT:
AIM: To perform the assay of calcium gluconate and repeat its percentage purity.
APPARATUS: Conical flask, pipette, measuring cylinder.
CHEMICALS: Disodium edetate, calcium gluconate, warm water, magnesium sulphate,
strong ammonia, mordant black-II.
PRINCIPLE: Calcium gluconate is used as calcium replenisher. Chemically it is calcium Dgluconate mono hydrate. Estimation of calcium gluconate is done by disodium edetate.
PROCEDURE:
Standardization of disodium edetate:
0.125gms of granulated zinc was accurately weighed and dissolved in few ml of HCl.To this
0.2ml of bromine water was added.solution was gently boiled to remove excess of
bromine.Solution was cooled and NaOH was added until solution becomes neutral.dilute to
250ml Ammonia buffer of PH 10 was added until the precipitate was just dissolved, 5ml
excess was added.Then a mixture of mordant black-II and NaCl was added as indicator and
was titrated with 0.05M disodium edetate until the green colour appears.
ASSAY: Drug equivalent to 0.5gms was taken and dissolved in 50ml of warm water. The
solution was cooled and 5ml of 0.05M MgSO 4 and 10ml of NH3 was added. The resultant
mixture was then titrated with 0.5M EDTA using mordant black-II as indicator.
Each ml of 0.05M EDTA 0.02242gms of calcium gluconate.
6. ASSAY OF METRONIDAZOLE
20 tablets were weighed, powdered and a quantity equivalent of 0.2gms was taken.
Solution is extracted with 6 quantities each of 10ml of hot acetone and cool.
50ml of acetic anhydride was added.
0.1ml of anhydrous glacial acetic acid was added and 1% solution of brilliant green
which acts as indicator, and titrated against 0.1N perchloric acid.
Each ml of HClO4 0.01712gms of metronidazole.
7. ASSAY OF METFORMIN
20 tablets were weighed and powdered and 0.1gm was taken and dissolved in 70ml of
From this 1, 2, 3, 4, 5ml was taken, to each 2ml of ninhydrin, 1.5ml of 0.1N HCl, 2ml
ASSAY:
20 tablets were weighed and quantity equivalent to 100mg was dissolved in 100ml of
0.1N HCl.
From this 3 ml was taken, 1.5N HCl, ninhydrin, 2ml methanol were added and heated
9. ASSAY OF FUROSEMIDE
From the above solution, 1ml was diluted with 200ml of methanol which gives
10ppm.
From the above 2, 4, 6, 8and 10ml were pipetted and make up to 10ml with methanol
To the aliquots of drug 2 ml of 3.5M HCl was added and 10ml of NaNO2was added.
The solutions were kept for 5min and allow to diazotization reaction to go to
completion.
The resulting solutions are coupled with aniline by adding 7ml of 10% aniline
ASSAY:
10 tablets were taken , weight of drug equivalent to 0.05gms was taken and dissolved
in 50ml CH3OH
1ml of above solution was taken and diluted to 10ml with methanol
From the resulting solution any volume ranging from 2-10ml was pipetted out and
CHEMICALS: MBTH reagent, distilled water, cephadroxil pure drug and ceric ammonium
nitrate.
PRINCIPLE: MBTH3 methyl, 2-benzo thiazolinone hydrazine was originally introduced
for aldehydes, and later extended to a variety of organic compounds like phenol, aryl amines
and different N and S heterocyclic compounds. Cephadroxil is an antibiotic which belongs to
the category of cephalosporins which act by disrupting the cell wall. Cephodroxil consists of
phenol group which interacts with MBTH and gives coloured solution which is observed
under U.V. With phenols under reaction conditions MBTH loses two electrons and one proton
to form the electrophilic intermediate, which has been identified as the active coupling
species that undergoes electrophilic substitution with phenols and other groups to form
coloured products.
PROCEDURE:
For calibration curve: 10 mg of pure drug was weighed and dissolved in 10ml of water.
From the above solution 0.1, 0.2, 0.3, 0.4 and 0.5 ml are taken and to these solutions 2ml of
MBTH solution was taken and to these solutions 2ml of MBTH solution was added and 2ml
of Ce(IV) solution was added and volume was made up to 1oml with distilled water which
produces concentration of 10, 20, 30, 40 and 50 g/ml. The absorbance was noted at 410nm.
add 1ml MBTH and 2ml cerric ammonium nitrate and made up to 10ml with water.
Blue colour develops due to complex formed. The concentrations are 4, 5, 6, 7, 8
g/ml.
The absorbance was measured at 580nm and curve was plotted.
ASSAY:
1000g/ml
From this 0.5ml was taken and add 1ml MBTH, 2ml cerric ammonium nitrate. Make
up to 10ml with water and absorbance was noted.
phenyl)-,-dihydroxy-5(1-methylethyl)-3-phenyl-4-[phenyl
amino
carbonyl]-1h-
PROCEDURE:
Preparation of stock solutions: stock standard solution of 0.5 mg/ml was prepared by
dissolving the appropriate weight of AVS in 100ml volumetric flask, 5ml of methanol was
added the volume was then diluted to the mark with distilled water. 0.01M MBTH solution
was prepared with doubled distilled water and 1% Ce (SO 4)2 solution was prepared with
sulphuric acid of 0.369M, medium. Freshly prepared solutions were always used.
Procedure for calibration curve: Aliquots of standard AVS solution (0.1-1.0ml, 0.5mg/ml)
were transferred into a series of 25ml calibrated volumetric flask. Then 1ml of MBTH
solution was added and kept a side for 3 min. after that, 1 ml of Ce(SO 4)2 solution was added.
The volume was made up to mark with distilled water mix well and note the absorbance at
566nm as function of time between 0-20min against reagent blank treated similarly.
ASSAY: 20 tablets containing AVS were weighed and pulverized. An amount of the powder
equivalent to 25mg of the cited drug was dissolved in a 25ml of CH 3OHand mixed for about
5min and filtered. The methanol was evaporated to about 5ml. the remaining portion of
solution was diluted to 50ml with double distilled water to achieve a concentration of
0.5mg/ml.Then to this above solution 1ml of MBTH was added and kept aside for 3min. after
that 1ml of Ce(SO4)2was added and the volume was made up to mark (25ml) with double
distilled water. Mix well and absorbance was noted at 566nm.
20 tablets were weighed and the drug equivalent to 100mg was taken and dissolved in
AIM: To estimate the amount of Ranitidine HCl pure drug and tablets, distilled water.
APPARATUS: UV- visible spectrophotometer, volumetric flask, pipette, measuring cylinder
etc.
PRINCIPLE: Ranitidine HCl is chemically N, N dimethyl-5-[2-(1-methyl amine-2nitrovinyl)-ethylthiomethyl] furfuryl amine hydrochloride. It is a H 2-receptor antagonist and
is widely used in short term treatment of duodenal ulcer and in the management of hyper
secretory conditions.
This method is based on the condensation of RNH with PDAB to form a red coloured
product. The absorbance of coloured product measured is a quantitative measure of
concentration of RNH. The absorbance was measured at 503nm.
Procedure for preparation of standard solutions:
PDAB solution of 0.025N was prepared in 2N HCl. Ranitidine HCl stock solution containing
1000g/ml RNH was prepared by dissolving 100mg of pure drug in water and diluting to the
mark in a 100ml calibrated flask.
Procedure for calibration curve:
Aliquots containing 50-350g/ml RNH were transferred into a series of 10ml standard flask
by means of a micro burette. To each flask 3ml of 0.025N PDAB was added and kept a side
for 20min for colour development. It was then diluted up to the mark with distilled water. The
absorbance was measured against reagent blank at 503nm. The graph of PDAB-RNH
condensation product and corresponding reagent blank was plotted by taking concentration
Vs absorbance.
ASSAY: Three tablets were taken and ground into a fine powder. Powder equivalent to
168mg of RNH was weighed into a 100ml calibrated flask, 60 ml of water was added and
shaken well and filtered. First 10ml portion of the filtrate was discarded. A suitable aliquot
was taken and add 3ml of 0.025N P-Dimethyl amino benzaldehyde was added and kept aside
for 20 min for colour development. It was then diluted up to the mark with distilled water.
The absorbance was measured against the reagent blank at 503nm.