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SULFASALAZINE
IDENTIFICATION
Examine by infrared absorption spectrophotometry
(2.2.24), comparing with the spectrum obtained with
sulfasalazine CRS. Examine the substances prepared as
discs.
TESTS
Related substances. Examine by liquid chromatography
(2.2.29).
Test solution. Dissolve 25.0 mg of the substance to be
examined in dilute ammonia R3 and dilute to 25.0 ml with
the same solvent.
Reference solution (a). Dilute 1.0 ml of the test solution to
100.0 ml with dilute ammonia R3.
Reference solution (b). Dissolve 1.0 mg of sulfasalazine
derivative for resolution CRS in 10.0 ml of reference
solution (a). Dilute 1.0 ml of this solution to 10.0 ml with
reference solution (a).
The chromatographic procedure may be carried out using :
a stainless steel column 0.25 m long and 4.6 mm in
internal diameter, packed with octadecylsilyl silica gel
for chromatography R (5 m),
as mobile phase at a flow rate of 1 ml/min :
Mobile phase A. In a 1000 ml volumetric flask dissolve
1.13 g of sodium dihydrogen phosphate R and 2.5 g of
sodium acetate R in 900 ml of water R. Adjust to pH 4.8
with glacial acetic acid R and adjust the volume to
1000 ml with water R,
Mobile phase B. Mix 1 volume of mobile phase A with
4 volumes of methanol R,
Time
(min)
Mobile phase A
(per cent V/V)
Mobile phase B
(per cent V/V)
Comment
0 - 15
60 45
40 55
linear gradient
15 - 25
45
55
isocratic
25 - 60
45 0
55 100
linear gradient
60 - 65
100
isocratic
65 - 67
0 60
100 40
switch to initial
composition
67 - 77
60
40
re-equilibration
Sulfasalazinum
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Sulfasalazine
any peak with an area less than 0.05 times the area of the
principal peak in the chromatogram obtained with reference
solution (a).
Salicylic acid and sulfapyridine. Examine by liquid
chromatography (2.2.29).
Test solution. Dissolve 25.0 mg of the substance to be
examined in dilute ammonia R3 and dilute to 25.0 ml with
the same solvent.
Reference solution (a). Dissolve 5.0 mg of salicylic acid R
and 5.0 mg and sulfapyridine CRS in dilute ammonia R3
and dilute to 10.0 ml with the same solvent.
Reference solution (b). Dilute 2.0 ml of reference solution (a)
to 100.0 ml with dilute ammonia R3.
The chromatographic procedure may be carried out using :
a stainless steel column 0.25 m long and 4.6 mm in
internal diameter, packed with octadecylsilyl silica gel
for chromatography R (5 m),
as mobile phase at a flow rate of 1 ml/min a mixture of
70 volumes of mobile phase A (described in the test for
related substances) and 30 volumes of mobile phase B
(described in the test for related substances),
as detector a spectrophotometer set at 300 nm.
Inject 20 l of reference solution (b). Adjust the sensitivity
of the system so that the height of the principal peaks
in the chromatogram obtained is at least 50 per cent of
the full scale of the recorder. When the chromatogram is
recorded in the prescribed conditions, the retention times
are : salicylic acid about 6 min and sulfapyridine about 7 min.
The test is not valid unless the resolution between the peaks
corresponding to salicylic acid and sulfapyridine is at least 2.
Inject 20 l of the test solution and 20 l of reference
solution (b). Continue the chromatography for 10 min. In
the chromatogram obtained with the test solution the area
of the peak corresponding to salicylic acid is not greater
than 0.5 times the area of the first peak in the chromatogram
obtained with reference solution (b) (0.5 per cent) and the
peak corresponding to sulfapyridine is not greater than
0.5 times the area of the second peak in the chromatogram
obtained with reference solution (b) (0.5 per cent). Disregard
any peak with an area less than 0.05 times the area of the
principal peak in the chromatogram obtained with reference
solution (b).
Chlorides (2.4.4.). To 1.25 g add 50 ml of distilled water R.
Heat at about 70 C for 5 min. Cool and filter. To 20 ml of
the filtrate add 1 ml of nitric acid R, allow to stand for 5 min
and filter to obtain a clear solution. 15 ml of the filtrate
complies with the limit test for chlorides (140 ppm).
Sulphates (2.4.13). To 20 ml of the filtrate prepared for the
test for chlorides add 1 ml of dilute hydrochloric acid R,
allow to stand for 5 min and filter. 15 ml of the filtrate
complies with the limit test for sulphates (400 ppm).
Heavy metals (2.4.8). 2.0 g complies with limit test D for
heavy metals (10 ppm). Prepare the standard using 2 ml of
lead standard solution (10 ppm Pb) R.
Loss on drying (2.2.32). Not more than 1.0 per cent,
determined on 1.000 g by drying in an oven at 100 C to
105 C for 2 h.
Sulphated ash (2.4.14). Not more than 0.5 per cent,
determined on 1.0 g.
ASSAY
Dissolve 0.150 g in 0.1 M sodium hydroxide and dilute
to 100.0 ml with the same solvent. Transfer 5.0 ml of this
solution to a 1000 ml volumetric flask containing about
750 ml of water R. Add 20.0 ml of 0.1 M acetic acid and
General Notices (1) apply to all monographs and other texts
A. 4,4-[(4-hydroxy-1,3-phenylene)bis(diazenediyl)]bis[N(pyridin-2-yl)benzenesulphonamide],
B. 2-hydroxy-3,5-bis[2-[4-(pyridin-2-ylsulphamoyl)phenyl]diazenyl]benzoic acid,
C. 2-hydroxy-5-[2-[4-(2-iminopyridin-1(2H)yl)phenyl]diazenyl]benzoic acid,
D. 4-[2-(2-hydroxyphenyl)diazenyl]-N-(pyridin-2yl)benzenesulphonamide,
E. 2-hydroxy-4-(pyridin-2-ylsulphamoyl)-5-[2-[4-(pyridin-2ylsulphamoyl)phenyl]diazenyl]biphenyl-3-carboxylic acid,
F. 2-hydroxy-3-[2-[4-(pyridin-2-ylsulphamoyl)phenyl]diazenyl]benzoic acid,
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Sulfathiazole
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