DICLOFENAC INJECTION
Heavy metals (2.3.13).1.0 g complies with the limit test for
heavy metals, Method B (10 ppm).
Loss on drying (2.4.19). Not more than 0.5 per cent, determined
.oliLOgbYdi}iiiigiiiarioveii afT05° fof 3 horns:
Assay. Weigh accurately about 0.2 g and dissolve in 50 rnl of
anhydrous glacial acetic acid. Titrate with 0.1 M perchloric
acid, deterrniriing the end-poiiit potentiometrically (2.4.25).
Carry out a blank titration.
1 rnl of 0.1 M perchloric acid is equivalent to 0.03181 g of
CI4HIOClzNNaOz.
Storage. Store protected from light.
Diclofenac Injection
Dic10fenac Sodium Injection
Diclofenac Injection is a sterile solution ofDiclofenac Sodium
iii Waterfor Injections. It may contairi Propylene Glycol, Benzyl
Alcohol and sufficient Sodium Hydroxide to adjust the pH of
the solution.
Diclofenac Injection contains not less than 95.0 per cent and
not more than 105.0 per cent of the stated amount ofdiclofenac
Usual strength. 25 mg per rnl.
Description. A clear, colollrless to yelloWish liquid.
Identification
Determine by thill-layer chromatography (2.4.17), coating the
plate with silica gel GF254.
Mobile phase. A mixture of 90 volumes of chloroform,
5 volumes of acetone and 5 volumes of fonnic acid in a
-saturatedcchamber; ..... --------- . -.-----------~------
Test solution. Dilute a suitable volume of the injection
containing 25 mg of Diclofenac Sodium to 10 rnl with
methanol.
Reference solution. A 0.25 per cent w/v solution of diclofenac
sodium RS in methanol.
j\ppl)' to the plate.2 III of each solution~ Aj'ter d~vel()pment,
cIiy the plate iii a cooent of Warnl aiiand exarnirie iii ultraviolet of hexane and 10 volumes of anhydrousfonnic acid.
light at 254 nm. Alternatively, spray with a 0.5 per cent w/v
solution of potassium dichromate iii sulphuric acid (20 per
cent). By both methods of visualisation, the priricipal spot in
the chromatogram obtained with the test solution corresponds
to that in the chromatogram obtained with the reference
solution.
1200
IP 2010
Tests
pH (2.4.24).8.1 to 9.0.
·Qtl1er:t~~ts,:G()lTIPlie~:\'Iith.the:tests:statedunderP-3!~l1te.r~··­
Preparations (Injections).
Assay. Determine by liquid chromatography (2.4.14).
Test solution. Dilute a suitable volume of the injection
containing 25 mg of Diclofenac Sodium to 10.0 rnl with the
mobile phase.
Reference solution. A 0.25 per cent w/v solution of diclofenac
sodium RS iii the mobile phase.
Chromatographic system
- a stainless steel column 12.5 cm x 4.6 mm, packed with
octylsilane bonded to porous silica (5 WU),
- mobile phase: a mixture of60volumes of methanol and
40 volumes of 0.1 M sodium acetate solution,
- flow rate. 1 rnl per minute,
- spectrophotometer set at 254 nm,
injection volume. 10 Ill.
Inject alternately the test solution and the reference solution
and record the chromatograms for 2.5 times the retention time
of the priricipal peak. If necessarY adjust the concentration of
methanol in the mobile phase to obtain the resolution of the
peak due to diclofenac sodium.
Calculate the content ofC l4H1oCIiNNaOziii the injection.
Diclofenac Tablets
Dic10fenac Sodium Tablets
Diclofenac Tablets contain not less than 90.0 per cent and not
more than 110.0 per cent of the stated amount of diclofenac
sodium, CI4HIOClzNNaOz. The tablets may be enteric-coated.
Usual strengths. 25 mg; 50 mg.
Identification
Determine by thin-layer chromatography (2.4.17), coating the
plate with silica gel 60 F254 or using a precoated silica gel
60 F254 plate.
Mobile phase. Amixture of 100 volumes of toluene, 10 volumes
Test solution. Shake a quantity of the powdered tablets
containing 50 mg ofDiclofenac Sodium with 5 rnl of methanol,
centrifuge and use the supernatant liquid.
Reference solution. A 1 per cent w/v solution of diclofenac
sodium RS iii methanol.
IP 2010
Apply separately to the plate 1 Iil of each solution. Mter
development, dry the plate in a current ofwarm air and examine
in ultraviolet light at 254 nm. Alternatively, spray the plate
with a 0.5 per cent w/v solution of potassium dichromate in
sulphuric acid (20 per cent). By both methods of
visualisation, the principal spot in the chromatogram obtained
with the test solution corresponds to that in the chromatogram
obtained with the reference solution.
Tests
Other tests. Comply with the tests stated under Tablets.
Assay. Weigh and powder 20 tablets. Weigh accurately a
quantity of the powder containing about 50 mg of Diclofenac
Sodium, shake with 60 rnl of methanol in a 200-rnl volumetric
flask and dilute to volume with methanol. Dilute 5.0 rnl of this
solution to 100.0 rnl with methanol and measure the absorbance
ofthe resulting solution at the maximum at about 285 nm (2.4.7).
Calculate the content of C14HlOChNNa02 from the absorbance
obtained by repeating the procedure using diclofenac sodium
RS in place of the substance under examination.
Storage. Store protected from light.
Dicloxacillin Sodium
Mol. Wt. 510.3
Dicloxacillin Sodium is sodium (6R)-6-[3-(2,6-
dichlorophenyl)-5-methylisoxazole-4-carboxamido]
penicillanate monohydrate.
Dicloxacillin Sodium contains not less than 95.0 per cent and
not more than 102.0 per cent of C19H16ChN3NaOsS, calculated
on the anhydrous basis.
Category. Antibact<erial.
Description. A white or almost white crystalline powder,
hygroscopic. .
Identification
Tests A and D may be omitted if tests B, C and D are carried
out. Tests B, C and D may be omitted if tests A and Dare
carried out.
1201
DICLOXACILLIN SODIUM
A. Determine by infrared absorption spectrophotometry (2.4.6).
Compare the spectrum with that obtained with dicloxacillin
sodium RS or with the reference spectrum of dicloxacillin
sodium.
B. Determine by thin layer chromatography (2.4.17), coating
the plate with silica gel H.
Mobile phase. A mixture of 30 volumes of acetone and
70 volumes of a 15.4 per cent w/v solution of ammonium
acetate, adjusted to pH 5.0 with glacial acetic acid.
Test solution. Dissolve 25 rng of the substance under
examination in 5 ml of water.
Reference solution (a). A 0.5 per cent w/v solution of
dicloxacillin sodium RS in water.
Reference solution (b). A solution containing 0.5 per cent
w/v each of cloxacillin sodium RS, dicloxacillin sodium RS
and flucloxacillin sodium RS in water.
Apply to the plate 1 Iil of each solution. Allow the mobile
phase to rise 15 cm. Dry the plate in air. Expose to iodine
vapour until the spots appear and examine in daylight, the
chromatogram obtained with reference s~lution (b) shows
three clearly separated spots. The principal spot in the
chromatogram obtained with the test solution corresponds to
that in the chromatogram obtained with reference solution (a).
C. Place about 2 mg in a test-tube about 150 rom long and
about 15 rom in diameter. Moisten with 0.05 rnl of water and
add 2 rnl of sulphuric acid10rmaldehyde reagent. Mix the
contents of the tube by swirling; the colour of the solution is
slightly greenish-yellow. Place the test-tube in a water-bath
for 1 minute; a yellow colour develops.
D. GivesreactionAofsodium (2.3.1).
Tests
Appearance ofsolution. A 10.0 per cent w/v solution in carbon
dioxide-free water (solution A) is clear (2.4.1) and its
absorbance at 430 nm (2.4.7) is not more than 0.04.
pH (2.4.24). 5.0to 7.0, determined in solution A.
Specific optical rotation (2.4.22). +128° to +143°, determined
in a 1 per cent w/v solution.
Related substances. Determine by liquid chromatography
(2.4.14).
Test solution (a). Dissolve 50 mg of the substance under
examination in 50.0 rnl of the mobile phase.
Test solution (b). Dilute 5.0 rnl of test solution (a) to 50.0 rnl
with the mobile phase.
Reference solution (a). A 0.01 per cent w/v solution of
dicloxacillin sodium RS in the mobile phase.