IP 2010
DILOXANIDE FUROATE
In the chromatogram obtained with the test solution the peaks
following the solvent peak, in order of emergence, are due to
(a) 5-chloro-8-hydroxyquinoline, (b) 5,7-dichloro-8-hydroxyquinoline, (c) the internal standard, (d) 5-chloro-7-iodo-8hydroxyquinoline and (e) diiodohydroxyquinoline. In the
chromatogram obtained with reference solution (b) calculate
the content of 5-chloro-8-hydroxy-quinoline, 5,7-dichloro-8hydroxyquinoline and 5-chloro-7-iodo-8-hydroxyquinoline by
reference to the corresponding peaks in the chromatogram
obtained with the test solution. The total content of the named
impurities and any other impurities does not exceed 4.0 per
centw/w.
Sulphated ash (2.3.18). Not more than 0.1 percent.
Loss on drying (2.4.19). Not more than 0.5 per cent, determined
on 1.0 g by drying over phosphorus pentoxide at a pressure
not exceeding 0.7 kPa for 4 hours.
Assay. Weigh accurately about 0.3 g and dissolve in 50 rnl of
anhydrous pyridine. Titrate with 0.1 M tetrabutylammonium
hydroxide, determining the end-point potentiometrically
(2.4.25). Carry out a blank titration.
1 rnl of 0.1 M tetrabutylammonium hydroxide is equivalent to
0.03969 gofCgHsI2NO.
Storage. Store protected from light.
Tests
Soluble iodides. Digest a quantity of the powdered tablets
containing 0.1 g ofDiiodohydroxyquinoline with 5 rnl of water
for 10 minutes, cool and filter. To the filtrate add 1 rnl of 3 M
hydrochloric acid, 0.1 rnl of ferric chloride test solution and
2 rnl of chloroform, shake gently and allow to separate; any
violet colour in the chloroform is not more intense. than that in
a blank to which 1 rnl of a 0.02 per cent w/v solution of
potassium iodide has been added.
Disintego-ation (2.5.1).30 minutes.
Other tests. Comply with the tests stated under Tablets.
Assay. Weigh and powder 20 tablets. Weigh accurately a
quantity of the powder containing about 12 mg of
Diiodohydroxyquinoiine and determine by the oxygen-flask
method (2.3.34), using a mixture of 10 rnl of water and 2 rnlof
1 M sodium hydroxide as the absorbing liquid. When the
process is complete, add to the flask an excess (5 rnl to 10 rnl)
of acetic bromine solution and allow to stand for 2 minutes.
Remove the excess of bromine by the addition offormic acid
(about 0.5 rnl to 1 rnl). Rinse the sides of the flask with water
and sweep out any bromine vapour above the liquid with a
current of air. Add 1· g of potassium iodide and titrate with
0.02 M sodium thiosulphate using starch solution,· added
towards the end of the titra~ion, as the indicator.
1 ml of 0.02 M sodium thiosulphate is equivalent to
0.0006616 g ofCgHsI2NO.
Diiodohydroxyquinoline Tablets
Storage. Store protected from light.
Iodoquinol Tablets
Diiodohydroxyquinoline Tablets contain not less than
90.0 per cent and not more than 110.0 per cent of the stated
amount of diiodohydroxyquinoline, CgHsI2NO.
Diloxanide Furoate
Usual strengths. 300 mg; 600 mg.
Identification
A. Triturate a quantity of the powdered tablets containing
about 50 mg of Diiodohydroxyquinoline with 10 rnl of carbon
disulphide, filter and evaporate the solvent. The residue
complies with the following test.
Determine by infrared absorption spectrophotometry (2.4.6).
Compare the spectrum with that obtained with
diiodohydroxyquinoline RS or with the reference spectrum
of diiodohydroxyquinoline.
B. Shake a quantity of the powdered tablets containing about
10 mg ofDiiodohydroxyquinoline with 100 rnl of dioxan, filter
and dilute 5 rnl of the filtrate to 100 rnl with ethanol. When
examined in the range 230 nm to 360 nm (2.4.7), the resulting
solution shows an absorption maximum at about 258 nm;
absorbance at about 258 nm, about 0.53 (2.4.7).
C 1JfllChN04
Mol. Wt.328.2
Diloxanide Furoate is 4-(N-methyl-2,2-dichloroacetamido)
pheny12-furoate.
Diloxanide Furoate contains not less than 98.0 per cent and
not more than 102.0 per cent of CI4Hl1C12N04, calculated on
the dried basis.
Category. Antiamoebic.
Dose. 1.5 g daily, in divided doses:
1225
DILOXANIDE FUROATE
IP 2010
Description. A white or almost white, crystalline powder;
odourless or almost odourless
Diloxanide Tablets
Diloxanide Furoate Tablets
Identification
A. Determine by infrared absorption spectrophotometry (2.4.6).
Compare the spectrum with that obtained with diloxanide
furoate RS or with the reference spectrum of diloxanide furoate.
B. When examined in the range 230 nm to 360 nm (2.4.7), a
0.001 per cent w/v solution in ethanol (95 per cent) shows an
absorption maximum only at about 258 nm; absorbance at
about 258 nm, about 0.70.
C. On 20 mg determine by the oxygen-flask method (2.3.34),
using 10 ml of 1 M sodium hydroxide as the absorbing liquid.
When the process is complete, acidify the liquid with nitric
acid and add silver nitrate solution; a white precipitate is
produced.
Tests
Free acidity. Shake 3.0 g with SO ml of water, filter and wash
the residue with three quantities, each of 20 ml, of water. Titrate
the combined filtrate and washings with 0.1 M sodium
hydroxide using phenolphthalein solution as indicator; not
more than 1.3 ml is required.
..•••.........•......•...••.
Dilox.-anideTablets c6i:itai'rii:i6t less than 95.0 percellt and not
more than 105.0 per cent of the stated amount Of diloxanide
furoate, C14HIlC12N04'
Usual strength. 500 mg.
Identification
A. Extract a quantity of the powdered tablets containing 0.2 g
of Diloxanide Furoate with 20 ml of chlorofonn, fIlter and
evaporate the fIltrate to dryness. The residue complies with
the following test.
Determine by infrared absorption spectrophotometry (2.4.6).
Compare the spectrum with that obtained with diliJxanide
furoate RS or with the reference spectrum of diloxanide furoate.
B. On 20 mg of the residue obtained in test A determine by the
oxygen-flask method (2.3.34), using 10 ml of 1 M sodium
hydroxide as the absorbing liquid. When the process is
complete, acidify the liquid with nitric acid and add silver
nitrate solution; a white precipitate is produced.
C. The residue obtained in test A melts at 114° to 116° (2.4.21).
Related substances. Determine by thin-layer chromatography
(2.4.17), coating the.. plate with silica gel HE2i4. . .
Tests
Mobile phase. A mixture of 96 volumes of dichloromethane
and 4 volumes of methanol.
Related substances. Determine by thin-layer chromatography
(2.4.17), coating the plate with silica gel HF254,
Test solution. Dissolve 0.5 g of the substance under
examination in 5 ml of chloroform.
Mobile phase. A mixture of 96 volumes of dichloromethane
and 4 volumes of methanol.
Reference solution. Dilute 1 ml of the test solution to 100 ml
with chloroform and mix. Dilute 5 ml of the resulting solution
to 20 ml with chlorofonn.
Test solution. Shake a quantity of the powdered tablets
containing 0.5 g ofDiloxanide Furoate with 5 ml of chlorofonn,
centrifuge and use the supernatant liquid.
Apply to the plate 5 ~ of each solution. After development, Reference solution. Dilute 1 ml of the test solution to 100 ml
~._...•ULJ.y tbeplateinflirillJ9 ex.m:nine inllltrgt.YiQle!J!ght~t~~~Lnm,
with chlorofonn and mix. Dilute 5 ml of the resulting solution
...._..
Any secondary spot in the chromatogram obtained with the·-fO-20 mlwlihc1ilorojorm: ... _....
test solution is not more intense than the spot in the
chromatogram obtained with the reference solution.
Apply to the plate 5 ~ of each solution. After development,
dry the plate in air and examine in ultraviolet light at 254 nm.
Sulphated ash (2.3.18). Not more than 0.1 per cent.
Any secondary spot in the chromatogram obtained with the
test solution is not more intense than the spot in the
chromatogram obtained with the reference solution.
Loss on drying (2.3.19). Not more than 0.5 per cent, determined
on 1.0 g by drying in an oven at 105°.
Assay. Weigh accurately about 0.3 g and dissolve in 50mlof
Other tests. Comply with the tests stated under Tablets.
anhydrous pyridine. Titrate with 0.1 M tetrabutylammonium
hydroxide, determining the end-point potentiometrically
(2.4.25). Carry out a blank titration.
Assay. Weigh and powder 20 tablets. Weigh
a
quantity of the powder containing about 40 mg of Diloxanide
Furoate, shake with 150 ml of ethanol (95 per cent) for
1 ml of 0.1 M tetrabutylammonium hydroxide is equivalent to
0.03282 g of Cl~llChN0 .
4
30 minutes, add sufficient ethanol (95 per cent) to produce
200.0 ml, mix and fIlter. Dilute 10.0 ml ofthe fIltrate to 250.0 ml
with ethanol (95per cent) and measure the absorbance of
the resulting solution at the maximum at about 258 nm (2.4.7).
Storage. Store protected from light.
1226