Phthalylsulfathiazole EUROPEAN PHARMACOPOEIA 8.

Substances precipitated with ammonia. To 10 mL of B. To 1 g add 8.5 mL of dilute sodium hydroxide solution R
solution S add 8 mL of dilute ammonia R1. Any opalescence and boil under a reflux condenser for 30 min. Cool and
in the solution is not more intense than that in a mixture of add 17.5 mL of dilute hydrochloric acid R. Shake vigorously
10 mL of solution S and 8 mL of water R. and filter. Neutralise the filtrate with dilute sodium
Hypophosphorous acid and phosphorous acid. To 5 mL hydroxide solution R. Filter, wash the precipitate with
of solution S add 2 mL of silver nitrate solution R2 and heat water R, recrystallise from water R and dry the crystals at
on a water-bath for 5 min. The solution shows no change in 100-105 °C. The crystals melt (2.2.14) at 200 °C to 203 °C.
appearance. C. To 0.1 g in a test-tube add 3 mL of dilute sulfuric acid R and
Chlorides (2.4.4) : maximum 6 ppm, determined on solution S. 0.5 g of zinc powder R. Fumes are evolved which produce
a black stain on lead acetate paper R.
Sulfates (2.4.13) : maximum 10 ppm, determined on the
preparation to be examined. D. To 0.1 g add 0.5 g of resorcinol R and 0.3 mL of sulfuric
acid R and heat on a water-bath until a homogeneous
Arsenic (2.4.2, Method A) : maximum 0.2 ppm, determined mixture is obtained. Allow to cool. Add 5 mL of
on 7.5 mL of solution S. dilute sodium hydroxide solution R. Dilute 0.1 mL of
Iron (2.4.9) : maximum 6 ppm. this brownish-red mixture to 25 mL with water R. An
intense green fluorescence appears which disappears on
Dilute 3 mL of solution S to 10 mL with water R. acidification.
Heavy metals (2.4.8) : maximum 1 ppm. E. Dissolve about 10 mg of the crystals obtained in
To 20 g add 4 mL of dilute ammonia R1 and dilute to 25 mL identification test B in 200 mL of 0.1 M hydrochloric acid.
with water R. 12 mL of the solution complies with test A. 2 mL of the solution gives the reaction of primary aromatic
Prepare the reference solution using a mixture of 2 mL of amines (2.3.1) with formation of an orange precipitate.
water R and 8 mL of lead standard solution (1 ppm Pb) R.
TESTS
ASSAY Appearance of solution The solution is clear (2.2.1) and not
To 8.60 g add a solution of 10 g of sodium chloride R in more intensely coloured than reference solution BY5 (2.2.2,
30 mL of water R. Titrate with 1 M sodium hydroxide, using Method II).
phenolphthalein solution R as indicator. Dissolve 1.0 g in 1 M sodium hydroxide and dilute to 20 mL
1 mL of 1 M sodium hydroxide is equivalent to 49.00 mg with the same solvent.
of H3PO4. Acidity. To 2.0 g add 20 mL of water R, shake continuously
for 30 min and filter. To 10 mL of the filtrate add 0.1 mL of
phenolphthalein solution R. Not more than 0.2 mL of 0.1 M
sodium hydroxide is required to change the colour of the
indicator.
01/2008:0352 Sulfathiazole and other primary aromatic amines :
corrected 6.0 maximum 2.0 per cent.
Dissolve 5 mg in a mixture of 3.5 mL of water R, 6 mL of
PHTHALYLSULFATHIAZOLE dilute hydrochloric acid R and 25 mL of ethanol (96 per
cent) R, previously cooled to 15 °C. Place immediately in iced
water and add 1 mL of a 2.5 g/L solution of sodium nitrite R.
Phthalylsulfathiazolum Allow to stand for 3 min, add 2.5 mL of a 40 g/L solution of
sulfamic acid R and allow to stand for 5 min. Add 1 mL of a
4 g/L solution of naphthylethylenediamine dihydrochloride R
and dilute to 50 mL with water R. Measured at 550 nm, the
absorbance (2.2.25) is not greater than that of a standard
prepared at the same time and in the same manner using a
mixture of 1 mL of a 100 mL aqueous solution containing
10 mg of sulfathiazole R and 0.5 mL of hydrochloric acid R ;
2.5 mL of water R ; 6 mL of dilute hydrochloric acid R ; and
C17H13N3O5S2 Mr 403.4 25 mL of ethanol (96 per cent) R.
[85-73-4]
Heavy metals (2.4.8) : maximum 20 ppm.
DEFINITION 1.0 g complies with test C. Prepare the reference solution using
2 mL of lead standard solution (10 ppm Pb) R.
2-[[4-(Thiazol-2-ylsulfamoyl)phenyl]carbamoyl]benzoic acid.
Loss on drying (2.2.32) : maximum 2 per cent, determined on
Content : 98.5 per cent to 101.5 per cent (dried substance). 1.00 g by drying in an oven at 105 °C.
CHARACTERS Sulfated ash (2.4.14) : maximum 0.1 per cent, determined on
1.0 g.
Appearance : white or yellowish-white, crystalline powder.
Solubility : practically insoluble in water, freely soluble in ASSAY
dimethylformamide, slightly soluble in acetone and in ethanol Dissolve 0.300 g in 40 mL of dimethylformamide R. Titrate
(96 per cent). with 0.1 M sodium hydroxide until the colour becomes blue.
using 0.2 mL of thymolphthalein solution R as indicator. Carry
IDENTIFICATION out a blank titration.
First identification : A, B, E. 1 mL of 0.1 M sodium hydroxide is equivalent to 20.17 mg
of C17H13N3O5S2.
Second identification : B, C, D, E.
A. Infrared absorption spectrophotometry (2.2.24). STORAGE
Comparison : phthalylsulfathiazole CRS. Protected from light.

3026 See the information section on general monographs (cover pages)