Accessed from 10.6.1.

1 by longwingnet on Tue Feb 28 15:31:24 EST 2017

USP 39 Official Monographs / Benzoyl 2723

Standard solution: Dissolve a quantity of Hydrous Ben-
zoyl Peroxide, previously subjected to the Assay, in ace-
tonitrile to obtain a solution containing 0.32 mg/mL.
Sample solution: 0.32 mg/mL of benzoyl peroxide in
acetonitrile
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 235 nm
Column: 4.6-mm 25-cm; packing L1
Flow rate: 1.2 mL/min
Injection size: 10 L
System suitability
Sample: System suitability solution
Suitability requirements
Resolution: NLT 2.0 between benzoic acid and
methylparaben
Tailing factors: NMT 2.0 for the benzoic acid and
methylparaben peaks
Analysis
Samples: Standard solution and Sample solution
Calculate the area, as a percentage, of each peak in
the chromatogram of the Sample solution:
Result = (rU/rT) 100
rU = peak response for any individual peak other
than the principal peak in the Sample
solution
rT = sum of the peak responses of all the
individual peaks including the principal peak
in the Sample solution
Acceptance criteria: The area of any individual peak
other than the principal peak is NMT 1.5% of the total
area. The sum of the areas of all peaks other than the
principal peak is NMT 2.0% of the total area.
ADDITIONAL REQUIREMENTS
tion and 5 mL of Internal standard solution, and dilute
with acetonitrile to 25 mL.
Sample stock solution: Transfer an equivalent to 40 mg
of benzoyl peroxide from Gel into a 50-mL volumetric
flask, add 40 mL of acetonitrile, and shake until the ma-
terial is thoroughly dispersed. Sonicate the mixture for
5 min, dilute with acetonitrile to volume, mix, and
filter.
Sample solution: 10 mL of Sample stock solution and
5 mL of Internal standard solution; dilute with acetoni-
trile to 25 mL.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 254 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 1 mL/min
Injection volume: 10 L
System suitability
Sample: Standard solution (three replicate injections)
[NOTEThe retention times for ethyl benzoate and ben-
zoyl peroxide are 7 and 14 min, respectively.]
Suitability requirements
Resolution: NLT 2.0 between ethyl benzoate and
benzoyl peroxide
Tailing factors: NMT 2.0 for the ethyl benzoate and
benzoyl peroxide peaks
Peak response ratios: The lowest and highest peak
response ratios (RS) agree within 2.0%.
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of ben-
zoyl peroxide (C14H10O4) in the portion of Gel taken:
Result = (RU/RS) (CS/CU) 100
RU = peak response ratio of benzoyl peroxide to
ethyl benzoate from the Sample solution

USP Monographs
PACKAGING AND STORAGE: Store in the original container, RS = peak response ratio of benzoyl peroxide to
at room temperature. [NOTEDo not transfer Hydrous ethyl benzoate from the Standard solution
Benzoyl Peroxide to metal or glass containers fitted with CS = concentration of benzoyl peroxide in the
friction tops. Do not return unused material to its original Standard solution (mg/mL)
container, but destroy it by treatment with sodium hy- CU = nominal concentration of benzoyl peroxide in
droxide solution (1 in 10) until addition of a crystal of the Sample solution (mg/mL)
potassium iodide results in no release of free iodine.] Acceptance criteria: 90.0%125.0%
IMPURITIES

Change to read:
.

Benzoyl Peroxide Gel

ORGANIC IMPURITIES
DEFINITION Solution A: Acetonitrile and glacial acetic acid (1000:1)
Benzoyl Peroxide Gel is benzoyl peroxide in a suitable gel Solution B: Water and glacial acetic acid (1000:1)
base. It contains NLT 90.0% and NMT 125.0% of the Mobile phase: See Table 1.
labeled amount of benzoyl peroxide (C14H10O4).
IDENTIFICATION Table 1
A. The retention time of the major peak for benzoyl perox- Time Solution A Solution B
ide of the Sample solution corresponds to that of the Stan- (min) (%) (%)
dard solution, as obtained in the Assay.
0 18 82
ASSAY 20 60 40
PROCEDURE 30 60 40
Mobile phase: Acetonitrile in water (5 in 10)
Internal standard solution: 3.6 mg/mL of ethyl benzo- System suitability solution: 100 g/mL of benzoic acid
ate in acetonitrile and 60 g/mL of methylparaben in acetonitrile
Standard stock solution: 0.8 mg/mL of benzoyl perox- Standard solution A: 500 g/mL of benzoic acid in
ide prepared as follows. Transfer a suitable quantity of acetonitrile
benzoyl peroxide, recently subjected to the Assay in Hy- Standard solution B: 20 g/mL of ethyl benzoate in
drous Benzoyl Peroxide, into a weighed conical flask fit- acetonitrile
ted with a glass stopper. Weigh again to obtain the Standard solution C: 20 g/mL of benzaldehyde in
weight of the specimen, and quantitatively dissolve in acetonitrile
acetonitrile. Standard solution D: Equivalent to 40 g/mL of anhy-
Standard solution: 0.32 mg/mL of benzoyl peroxide drous benzoyl peroxide in acetonitrile, prepared from
prepared as follows. Mix 10 mL of Standard stock solu- hydrous benzoyl peroxide, which has been analyzed as

Official from December 1, 2016

Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
 Accessed from 10.6.1.1 by longwingnet on Tue Feb 28 15:31:24 EST 2017
2724 Benzoyl / Official Monographs
follows. Place 300 mg of previously mixed hydrous ben- ASSAY
zoyl peroxide in a conical flask fitted with a ground- PROCEDURE
glass stopper. Weigh again to obtain the weight of the
sample. Add 30 mL of glacial acetic acid, previously
sparged with carbon dioxide for NLT 2 min just before
use, and swirl the flask gently to dissolve. Add 5 mL of
potassium iodide solution (1 in 2), and mix. Allow the
solution to stand for 1 min. Titrate the liberated iodine
with 0.1 N sodium thiosulfate VS. As the endpoint is
approached, add 1 drop of starch iodide paste TS, or
equivalent, and continue the titration to the discharge
of the blue color. Perform a blank determination, and
make any necessary correction (see Titrimetry 541).
Each mL of 0.1 N sodium thiosulfate is equivalent to
12.11 mg of anhydrous benzoyl peroxide (C14H10O4).
. 0.32 mg/mL of benzoyl peroxide.
(ERR 1-Jun-2015)
Sample solution: Transfer an amount of Gel equivalent
to 100 mg of benzoyl peroxide to a 50-mL volumetric
flask, and add 25 mL of acetonitrile. Shake vigorously to
disperse the specimen, sonicate for 5 min, dilute with
acetonitrile to volume, and filter.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 235 nm
Column: 4.6-mm 25-cm; packing L1
Flow rate: 1.2 mL/min
Injection volume: 10 L
System suitability
Sample: System suitability solution
Suitability requirements
Resolution: NLT 2.0 between benzoic acid and
methylparaben
Tailing factor: NMT 2.0 for the benzoic acid and
methylparaben peaks
Analysis
Samples: Standard solution and Sample solution
Acceptance criteria: The responses of any peaks from
USP Monographs
the Sample solution corresponding to benzoic acid, ethyl
benzoate, and benzaldehyde are NMT those of the
main peaks from Standard solution A (25%), Standard
solution B (1%), and Standard solution C (1%), respec-
tively. The response of any other impurity peak from
the Sample solutionother than the main benzoyl per-
oxide peak, any benzoic acid, ethyl benzoate, benzalde-
hyde, methylparaben, or propylparaben peak, and any
solvent peakis NMT that from Standard solution D
(2%); and the sum of the responses of all the impurity
peaksother than those of benzoic acid, ethyl benzo-
ate, and benzaldehydeis NMT that from Standard so-
lution D (2%).
SPECIFIC TESTS
PH 791: 2.86.6
ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in tight containers.
.
IMPURITIES
Benzoyl Peroxide Lotion ORGANIC IMPURITIES
DEFINITION
Benzoyl Peroxide Lotion is benzoyl peroxide in a suitable
lotion base. It contains NLT 90.0% and NMT 110.0% of
the labeled amount of benzoyl peroxide (C14H10O4).
IDENTIFICATION
A. The retention time of the major peak of the Sample
solution corresponds to that of the Standard solution, as
obtained in the Assay.
Official from December 1, 2016
Copyright (c) 2017 The United States Pharmacopeial Convention. All rights reserved.
USP 39
Mobile phase: Acetonitrile in water (5 in 10)
Internal standard solution: 3.6 mg/mL of ethyl benzo-
ate in acetonitrile
Standard stock solution: Transfer a suitable quantity of
benzoyl peroxide, recently subjected to the Assay under
Hydrous Benzoyl Peroxide, in a weighed conical flask fit-
ted with a glass stopper. Weigh again to obtain the
weight of the specimen, and quantitatively dissolve in
acetonitrile to obtain a solution containing 0.8 mg/mL.
Standard solution: 10 mL of Standard stock solution
and 5 mL of Internal standard solution. Dilute with ace-
tonitrile to 25 mL. This Standard solution contains
Sample stock solution: Transfer the equivalent to
40 mg of benzoyl peroxide from Lotion in a 50-mL vol-
umetric flask, and add 40 mL of acetonitrile. Shake vig-
orously until the material is thoroughly dispersed. Soni-
cate the mixture for 5 min, dilute with acetonitrile to
volume, mix, and filter.
Sample solution: 10 mL of Sample stock solution and
5 mL of Internal standard solution. Dilute with acetoni-
trile to 25 mL.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 254 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 1 mL/min
Injection volume: 10 L
System suitability
Sample: Standard solution (three replicate injections)
[NOTEThe retention times for ethyl benzoate and ben-
zoyl peroxide are 7 and 14 min, respectively.]
Suitability requirements
Resolution: NLT 2.0 between ethyl benzoate and
benzoyl peroxide
Tailing factor: NMT 2.0 for the ethyl benzoate and
benzoyl peroxide peaks
Peak response ratios: The lowest and highest peak
response ratios (RS) agree within 2.0%.
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of ben-
zoyl peroxide (C14H10O4) in the portion of Lotion
taken:
Result = (RU/RS) (CS/CU) 100
RU = peak response ratio of benzoyl peroxide to
ethyl benzoate from the Sample solution
RS = peak response ratio of benzoyl peroxide to
ethyl benzoate from the Standard solution
CS = concentration of benzoyl peroxide in the
Standard solution (mg/mL)
CU = nominal concentration of benzoyl peroxide in
the Sample solution (mg/mL)
Acceptance criteria: 90.0%110.0%
Solution A: Acetonitrile and glacial acetic acid (1000:1)
Solution B: Glacial acetic acid and water (1:1000)
Mobile phase: See Table 1.
Table 1
Time Solution A Solution B
(min) (%) (%)
0 18 82
20 60 40
30 60 40