Accessed from 128.83.63.
20 by nEwp0rt1 on Mon Nov 21 23:18:20 EST 2011
USP 35
Benzoic Acid
.
C7H6O2 122.12
Benzoic acid.
Benzoic acid [65-85-0].
» Benzoic Acid contains not less than 99.5 per-
cent and not more than 100.5 per cent of
C7H6O2, calculated on the anhydrous basis.
Packaging and storage—Preserve in well-closed containers.
Identification—Prepare a saturated solution of Benzoic Acid in
water, and filter twice. T o one portion of the filtrate add ferric
chloride TS: a salmon-colored precipitate is formed. T o a sepa-
rate 10-mL portion of the filtrate add 1 mL of 7 N sulfuric acid
and cool the mixture: a white precipitate forms in about 10
minutes; this precipitate is soluble in ether.
Congealing range 〈651〉: between 121 ° and 123 °.
Water, Method I 〈921〉: not more than 0.7%, a 1 in 2 solu-
tion of methanol in pyridine being used as the solvent.
Readily carbonizable substances 〈271〉—Dissolve 500 mg in
5 mL of sulfuric acid: the solution has no more color than
Matching Fluid Q.
Residue on ignition 〈281〉: not more than 0.05%.
Heavy metals 〈231〉—Dissolve 2.0 g in 25 mL of acetone, and
add 2 mL of water. Add 1.2 mL of thioacetamide-glycerin base
TS and 2 mL of pH 3.5 Acetate Buffer, and allow to stand for 5
minutes: any color produced is not darker than that of a control
made with 25 mL of acetone, 2.0 mL of Standard Lead Solution,
and treated in the same manner. The limit is 10 µg per g.
Readily oxidizable substances—Add 1.5 mL of sulfuric acid
to 100 mL of water, heat to boiling, and add 0.1 N potassium
permanganate, dropwise, until the pink color persists for 30
seconds. Dissolve 1.00 g of Benzoic Acid in the hot solution,
and titrate with 0.1 N potassium permanganate VS to a pink
color that persists for 15 seconds: not more than 0.50 mL of
0.10 N potassium permanganate is consumed.
Assay—Dissolve about 500 mg of Benzoic Acid, accurately
weighed, in 25 mL of diluted alcohol that previously has been
neutralized with 0.1 N sodium hydroxide, add phenolphthalein
TS, and titrate with 0.1 N sodium hydroxide VS to a pink color.
Each mL of 0.1 N sodium hydroxide is equivalent to 12.21 mg
of C 7H6O2.
Benzoic and Salicylic Acids Ointment
.
» Benzoic and Salicylic Acids Ointment is Benzoic
Acid and Salicylic Acid, present in a ratio of
about 2 to 1, in a suitable ointment base. It con-
tains not less than 90.0 per cent and not more
than 110.0 per cent of the labeled amounts of
benzoic acid (C 7H6O2) and salicylic acid (C 7H6O3).
Packaging and storage—Preserve in well-closed containers,
and avoid exposure to temperatures exceeding 30 °.
Labeling—Label Ointment to indicate the concentrations of
Benzoic Acid and Salicylic Acid and to indicate whether the
ointment base is water-soluble or water-insoluble.
USP Reference standards 〈11〉—
USP Benzoic Acid RS
USP Salicylic Acid RS
Official from May 1, 2012
Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Benzoic 2325
Identification—Dissolve an amount of Ointment, equivalent
to about 60 mg of benzoic acid and 30 mg of salicylic acid, in
25 mL of a solvent consisting of equal volumes of chloroform
and methanol. Prepare separate Standard solutions in the same
solvent containing, respectively, 2.4 mg of USP Benzoic Acid RS
in each mL and 1.2 mg of USP Salicylic Acid RS in each mL.
Apply 5 µL of each solution at separate points 2.5 cm from the
bottom edge of a 20- × 20-cm thin-layer chromatographic plate
(see Chromatography 〈621〉) coated with a 0.25-mm layer of
chromatographic silica gel mixture, and allow the spots to dr y.
Develop the chromatogram in a solvent system consisting of a
mixture of chloroform, acetone, isopropyl alcohol, methanol,
and ammonium hydroxide (30:30:15:15:10) until the solvent
front has moved about three-fourths of the length of the plate.
Remove the plate from the chromatographic chamber, mark
the solvent front, and allow the solvent to evaporate. V iew the
chromatogram under short-wavelength (254 nm) UV radiation:
the two major fluorescent spots from the test solution corre-
spond in color and in RF value to those from the respective
Standard solutions.
Minimum fill 〈755〉: meets the requirements.
Assay—
Ferric chloride-urea reagent—On the day of use, dissolve,
without heating, 18 g of urea in a mixture of 2.5 mL of ferric
chloride solution (6 in 10) and 12.5 mL of 0.05 N hydrochloric
acid.
Column A—Insert a small pledget of glass wool above the
stem constriction of a 20- × 2.5-cm chromatographic tube. Mix
1 g of chromatographic siliceous earth with 0.5 mL of dilute
phosphoric acid (3 in 10) to form a uniform, fluffy mixture,
transfer to the chromatographic tube, and pack evenly over the
glass wool, exerting gentle pressure. Similarly, mix 4 g of chro-
matographic siliceous earth with 3 mL of Ferric chloride-urea rea-
gent, and pack uniformly over the first layer. Cover the column
with a pad of glass wool.
Column B—Insert a small pledget of glass wool above the
stem constriction of a second 20- × 2.5-cm chromatographic
tube. Mix 4 g of chromatographic siliceous earth with 2 mL of
sodium bicarbonate solution (1 in 12), prepared just prior to
use, to a uniform, fluffy mixture, and pack evenly over the glass
wool. Cover the column with a pad of glass wool.
Assay preparation—Transfer an accurately weighed amount of
Ointment, equivalent to about 100 mg of benzoic acid and 50
mg of salicylic acid, to a 250-mL volumetric flask, and dissolve
in about 150 mL of chloroform by warming on a steam bath.
Cool, dilute with chloroform to volume, and mix.
Procedure—Mount Column A directly over Column B, then pi-
pet 10 mL of Assay preparation onto Column A, and allow it to
pass into the column. W ash the columns with two 40-mL por-
tions of chloroform, allowing the first portion to recede to the
top of each column before adding the second portion. Discard
the eluates, and separate the columns.
Salicylic acid content—Elute Column A with 95 mL of a 3 in
100 solution of glacial acetic acid in chloroform, collecting the
eluate in a 100-mL volumetric flask. Dilute the contents of the
flask with the same solvent to volume, and mix. Dissolve an
accurately weighed quantity of USP Salicylic Acid RS in the
same solvent, and dilute quantitatively and stepwise with this
solvent to obtain a Standard solution having a known concen-
tration of about 20 µg per mL. Concomitantly determine the
absorbances of both solutions in 1-cm cells at the wavelength
of maximum absorbance at about 311 nm, with a suitable
spectrophotometer, using a 3 in 100 solution of glacial acetic
acid in chloroform as the blank. Calculate the quantity, in mg,
of salicylic acid (C 7H6O3) in the portion of Ointment taken by
the formula:
2.5C(AU / AS)
in which C is the concentration, in µg per mL, of USP Salicylic
Acid RS in the Standard solution; and AU and AS are the ab-
sorbances of the diluted eluate from Column A and the Stan-
dard solution, respectively.