IP 2010
- spectrophotometer set at 240 nm,
injection volume. 20 /ll.
Time Mobile phase A Mobile phase B
(in min.) (per cen v/v) (per cent v/v)
o 65 35
15 65 35
30 20 80
40 20 80
45 65 35
50 65 35
Inject reference solution (b). The test is not valid unless the
relative standard deviation for replicate injections is not more
than 5.0 per cent. The relative retention time with reference to
sildenafil for N-oxide is about 0.29 and for chlorosulphonyl is
about 1.6.
Inject the test solution and reference solution (b). In the
chromatogram obtained with test solution the area ofthe peak
due to N-oxide impurity is not more than 1.67 times the area of
the principal peak in the chromatogram obtained with reference
solution (b) (0.5 per cent), the area of peak due to
chlorosulphonyl is not more than 0.67 times the area of the
principal peak in the chromatogram obtained with reference
solution (b) (0.2 per cent). The area of any other secondary
peak is not more than the area of the principal peak in the
chromatogram obtained with reference solution (b) (0.3 per
cent). The sum of areas of all the secondary peaks is not more
than 3.3 times the area ofthe principal peale in the chromatogram
obtained with reference solution (b) (1.0 per cent). Ignore any
peak corresponding to citric acid.
Heavy Metals (2.3.13). 1.0 g complies with the limit test for
heavy metals, Method B (20 ppm).
Sulphated ash (2.3.18). Not more than 0.1 per cent.
Loss on drying (2.4.19). Not more than 1.0 per cent, determined
on 1.0 g by drying in oven at 105° for 3 hours.
Assay. Determine by liquid chromatography (2.4.14).
NOTE-Use freshly prepared solution.
Solvent mixture. 30 volumes of water and 70 volumes of
acetonitrile.
Test solution. Dissolve 50 mg of the substance under
examination in 50.0 ml ofthe solvent mixture. Dilute 5.0 ml of
this solution to 50.0 ml with the solvent mixture.
Reference solution. A 0.1 per cent w/v solution of sildenafil
citrate RS in the solvent mixture. Dilute 5.0 ml ofthis solution
to 50.0 ml with the solvent mixture.
Chromatographic system
- a stainless steel column 25 cm x 4.6 mm, packed with
octadecylsilane bonded to porous silica (5 /lm) (such as
Hypersil ODS CI8),
2101
SILDENAFIL TABLETS
mobile phase: a mixture of50 volumes ofa buffer solution
prepared by dissolving 3.85 g of ammonium acetate in
1000 ml of water, adjusted to pH 7.5 with ammonia
solution and 50 volumes of acetonitrile,
- flow rate. 1 ml per minute,
spectrophotometer set at 240 nm,
- injection volume. 20 /ll.
Inject the reference solution. The test is not valid unless the
theoretical plates is not less than 2000, the tailing factor is not
more than 2.0 and the relative standard deviation for replicate
injections is not more than 2.0 per cent.
Inject the test solution and the reference solution.
Calculate the content ofC2sH3sN6011S.
Storage. Store protected from light and moisture.
SildenafIl Tablets
Sildenafil Citrate Tablets
Sildenafil Tablets contain not less than 90.0 per cent and not
more than 110.0 per cent of the stated amount of sildenafil
citrate, C2sH3SN6011 S.
Usual Strengths. 25 mg; 50 mg; 100 mg.
Identification
In the Assay, the principal peak in the chromatogram obtained
with the test solution corresponds to the peak in the
chromatogram obtained with the reference solution.
Tests
Dissolution (2.5.2).
Apparatus No.1,
Medium. 900 ml of O. 01 M Hydrochloric acid,
Speed and time. 100 rpm and 30 minutes.
Withdraw a suitable volume ofthe medium and filter. Measure
the absorbance of the filtered solution, suitably diluted with
the medium if necessary, at the maximum at about 294 nm
(2.4.7). Calculate the content of C2sH3SN60 IIS in the medium
from the absorbance obtained from a solution of known
concentration of sildenafil citrate RS in the same medium.
D. Not less than 70 per cent of the stated amount of
C2sH3SN6011 S.
Related substances. Determine by liquid chromatography
(2.4.14)
Solvent mixture. 50 volumes ofmobile phase A and 50 volumes
of methanol.
Test solution. Weigh and powder 20 tablets. Disperse a quantity
ofpowder containing about 50 mg of sildenafil with 35 ml of
SILDENAFIL TABLETS IP 2010

the solvent mixture, sonicate for 20 minutes and dilute to 50 ml Test solution.N'Ieigh and powder 20 tablets. Disperse a quantity
with the solvent mixture, filter. ofpowder containing about 50 mg of sildenafil with 35 mlof
the solvent mixture, sonicate for 20 minutes and dilute to 50.0
Reference solution (a). A 0.028 per cent w/v solution of
ml with the solvent mixture, filter.
sildenafil citrate RS in the solvent mixture.
Reference solution. A 0.14 per cent w/v solution of sildenajil
Reference solution (b). Dilute 5.0 ml ofreference solution (a)
citrate RS in the solvent mixture.
to 100 ml with the solvent mixture.
Chromatographic system
Chromatographic system
a stainless steel column 25 cm x 4.6 rom, packed with
a stainless steel column 25 cm x 4.6 rom, packed with
silica (5 Ilm) (Such as Zorbax Eclipse XDB C18),
octadecylsilane chemically bonded to porous silica (5
- mobile phase: a mixture of 30 volumes of solution
Ilm) (Such as Zorbax Eclipse XDB C 18),
containing 3.85 g of ammonium acetate and 1.0 ml of
- column temperature. 40°,
triethylamine in 1000 ml of water, adjusted to pH 5.5
mobile phase: A. a solution containing 3.85 g of
with acetic acid and 70 volumes of methanol,
ammonium acetate and 1.0 ml of triethylamine in 1000
flow rate. 1 ml per minute,
of water, adjusted to pH 5.5 with acetic acid,
spectrophotometer set at 294 nm,
B. methanol,
injection volume. 20 Ill.
a linear gradiept programme using the conditions given
below, Inject the reference solution. The test is not valid unless the
flow rate. 1 ml per minute, theoretical plates is not less than 2000, the tailing factor is not
spectrophotometer set at 294 nm, more than 2.0 and the relative standard deviation for replicate
injection volume. 10 Ill. injections is not more than 5.0 per cent.
Time Mobile Phase A Mobile Phase B Inject the reference solution the test solution.
(in min.) (per cent lv/v) (per cent lv/v)
Calculate the content of C2sH3sN60 I IS in the tablet.
o 47 53
Storage. Store protected from moisture.
20 47 53
Labelling. The label states the strength in terms of the
35 10 90 equivalent amount of sildenafil.
45 . 10 90
50 47 53
ill 47 53
Silver Nitrate
Inject reference solution (b). The test is not valid unless the
relative standard deviation for replicate injections is not more Mol. Wt. 169.9
than 5.0 per cent. Silver Nitrate contains not less than 99.0 per cent and not
Inject reference solution (b) and the test solution. In the . more than 100.5 per cent ofAgN03.
chromatogram obtained with the test solution, the area of any Category. Local anti-infective.
secondary peak is not more than 0.8 times the area of the
principal peak in the chromatogram obtained with reference Description. Colourless crystals or a white, crystalline powder.
solution (b) (0.8 per cent), the area of peak cOlTesponding to
Identification
N-oxide impurity at relative retention time 0.54 is not more
than the area of the principal peak in the chromatogram A. Gives the reactions of silver salts (2.3.1).
obtained with reference solution (b) (1.0 per cent) and the sum
B. 10 mg gives reaction A ofnitrates (2.3.1).
of areas of all the secondary peaks is not more than 2.0 times
the area of the peak in the chromatogram obtained with
Tests
reference solution (b) (2.0 per cent). Ignore the peak due to
citric acid at retention time about 2.4 minutes. Appearance of solution. A4.0 per cent w/v solution (solution
A) is clear (2.4.1), and colourless (2.4.1).
Other tests. Comply with the tests stated under Tablets.
Acidity or alkalinity. To 2 ml of solution A add 0.1 mlof
Assay. Detennine by liquid chromatography (2.4.14).
bromocresol green solution; the solution is blue. To 2 ml of
Solvent mixture. 50 volumes ofmobile phase and 50 volumes this solution add 0.1 ml ofphenol red solution; the solution is
of methanol. yellow.

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