Ibuprofen JP XV

744 Ibuprofen / O‹cial Monographs JP XV

and water (2:2:1), and titrate <2.50> with 0.1 mol W

L sodium gel with ‰uorescent indicator for thin-layer chromatography.
hydroxide VS (indicator: 2 drops of phenolphthalein TS). Develop the plate with a mixture of hexane, ethyl acetate and
Perform a blank determination, and make any necessary cor- acetic acid (100) (15:5:1) to a distance of about 10 cm, and
rection. air-dry the plate. Examine the plate under ultraviolet light
(main wavelength: 254 nm): the spots other than the principal
Amount (z) of carboxybenzoyl group (C8H5O3)
spot from the sample solution are not more intense than the
＝｛(0.01×149.1×V)/W｝－｛(2×149.1×P)/166.1｝
spot from the standard solution.
P: amount (z) of phthalic acid obtained in the Purity (3)
Loss on drying <2.41> Not more than 0.5z (1 g, in vacuum
V: amount (mL) of 0.1 mol WL sodium hydroxide VS con-
at a pressure not exceeding 0.67 kPa, phosphorus (V) oxide, 4
sumed
hours).
W: amount (g) of the sample, calculated on the anhydrous
basis Residue on ignition <2.44> Not more than 0.1z (1 g).
Containers and storage Containers—Tight containers. Assay Weigh accurately about 0.5 g of Ibuprofen, previ-
ously dried, dissolve in 50 mL of ethanol (95), and titrate
<2.50> with 0.1 mol WL sodium hydroxide VS (indicator: 3
Ibuprofen drops of phenolphthalein TS). Perform a blank determina-
tion, and make any necessary correction.
イブプロフェン
L sodium hydroxide VS
Each mL of 0.1 mol W
＝ 20.63 mg of C13H18O2
Containers and storage Containers—Well-closed contain-
ers.
C13H18O2: 206.28
(2RS )-2-[4-(2-Methylpropyl)phenyl]propanoic acid Ichthammol
[15687-27-1 ]
イクタモール
Ibuprofen, when dried, contains not less than 98.5z
of C13H18O2.
Ichthammol, calculated on the dried basis, contains
Description Ibuprofen occurs as a white crystalline powder. not less than 2.5z of ammonia (NH3: 17.030), not
It is freely soluble in ethanol (95) and in acetone, and prac- more than 8.0z of ammonium sulfate [(NH4)2SO4:
tically insoluble in water. 132.14], and not less than 10.0z of total sulfur (as S:
It dissolves in dilute sodium hydroxide TS. 32.07).
Identiˆcation (1) Determine the absorption spectrum of a Description Ichthammol is a red-brown to blackish brown,
solution of Ibuprofen in dilute sodium hydroxide TS (3 in viscous fluid. It has a characteristic odor.
20,000) as directed under Ultraviolet-visible Spectrophoto- It is miscible with water, and is partially soluble in ethanol
metry <2.24>, and compare the spectrum with the Reference (95) and in diethyl ether.
Spectrum: both spectra exhibit similar intensities of absorp-
Identification (1) To 4 mL of a solution of Ichthammol (3
tion at the same wavelengths.
in 10) add 8 mL of hydrochloric acid: a yellow-brown to
(2) Determine the infrared absorption spectrum of
blackish brown, oily or resinous mass is produced. Cool the
Ibuprofen, previously dried, as directed in the potassium
mass with ice to solidify, and discard the water layer. Wash
bromide disk method under Infrared Spectrophotometry
the residue with diethyl ether: a part of the mass dissolves but
<2.25>, and compare the spectrum with the Reference Spec-
it does not dissolve completely even when it is washed until
trum: both spectra exhibit similar intensities of absorption at
almost no color develops in the washing. Perform the follow-
the same wave numbers.
ing tests with this residue.
Melting point <2.60> 75 – 779C (i) To 0.1 g of the residue add 1 mL of a mixture of
diethyl ether and ethanol (95) (1:1): it dissolves.
Purity (1) Heavy metals <1.07>—Proceed with 3.0 g of
(ii) To 0.1 g of the residue add 2 mL of water: it dis-
Ibuprofen according to Method 2, and perform the test. Pre-
solves. To 1 mL of this solution add 0.4 mL of hydrochloric
pare the control solution with 3.0 mL of Standard Lead Solu-
acid: a yellow-brown to blackish brown oily or resinous sub-
tion (not more than 10 ppm).
stance is produced.
(2) Arsenic <1.11>—Prepare the test solution with 1.0 g
(iii) To 1 mL of the solution obtained in (ii) add 0.3 g of
of Ibuprofen according to Method 3, and perform the test
sodium chloride: a yellow-brown or blackish brown oily or
(not more than 2 ppm).
resinous substance is produced.
(3) Related substances—Dissolve 0.50 g of Ibuprofen in
(2) Boil 2 mL of a solution of Ichthammol (1 in 10) with 2
exactly 5 mL of acetone , and use this solution as the sample
mL of sodium hydroxide TS: the gas evolved changes
solution. Pipet 1 mL of the sample solution, add acetone to
moistened red litmus paper to blue.
make exactly 100 mL, and use this solution as the standard
solution. Perform the test with these solutions as directed Loss on drying <2.41> Not more than 50z (0.5 g, 1059
C, 6
under Thin-layer Chromatography <2.03>. Spot 5 mL each of hours).
the sample solution and standard solution on a plate of silica
Residue on ignition <2.44> Not more than 0.5z (1 g).

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744 Ibuprofen / O‹cial Monographs JP XV

and water (2:2:1), and titrate <2.50> with 0.1 mol W

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