Accessed from 10.6.1.

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7102 Acetaminophen / Official Monographs

Second Supplement to USP 37NF 32

C. THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST

201
Sample solution: Triturate 0.4 g of the powder with
25 mL of methanol, and filter.
Chromatographic system
Developing solvent system: Methylene chloride and
methanol (4:1)
Acceptance criteria: Meets the requirements

USP REFERENCE STANDARDS 11

USP Acetaminophen RS

ASSAY
PROCEDURE
Mobile phase: Methanol and water (1:3)
Standard solution: 0.01 mg/mL of USP Acetaminophen
RS in Mobile phase
Sample stock solution: Dissolve 10 g of Acetaminophen for Effervescent Oral Solution in 200 mL of water
in a 1000-mL volumetric flask, using gentle heat if necessary, until effervescence subsides, and then dilute
with water to volume.
Sample solution: Nominally 0.16 mg/mL of acetaminophen in Mobile phase from the Sample stock solution.
Pass a portion of this solution through a filter of 0.5-m
or finer pore size, discarding the first 10 mL of the
filtrate.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 243 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 1.5 mL/min
Injection volume: 10 L
System suitability
Sample: Standard solution
Suitability requirements
Column efficiency: NLT 1000 theoretical plates
Tailing factor: NMT 2.0
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the quantity, in g, of acetaminophen
(C8H9NO2) in 100 g of Acetaminophen for Effervescent
Oral Solution taken:

DEFINITION
Acetaminophen Oral Suspension is a suspension of Acetaminophen in a suitable aqueous vehicle. It contains NLT
90.0% and NMT 110.0% of the labeled amount of acetaminophen (C8H9NO2).

Result = (rU/rS) (CS/CU) (1/F1) L F2

rU
rS
CS

= peak response from the Sample solution

= peak response from the Standard solution
= concentration of USP Acetaminophen RS in
the Standard solution (mg/mL)
CU
= nominal concentration of acetaminophen in
the Sample solution (mg/mL)
F1
= conversion factor, 1000 mg/g
L
= label claim (mg/unit)
F2
= conversion factor, 100, based on the label
claim of g of acetaminophen per 100 g of
sample
Acceptance criteria: 5.636.88 g
PERFORMANCE TESTS
MINIMUM FILL 755: Meets the requirements for solids
packaged in multiple-unit containers
UNIFORMITY OF DOSAGE UNITS 905: Meets the requirements for solids packaged in single-unit containers
IMPURITIES
Add the following:

4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG

PRODUCTS 227: Meets the requirements2S (USP37)

ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in air-tight containers,
and store at controlled room temperature.

Acetaminophen Oral Suspension

IDENTIFICATION
A. INFRARED ABSORPTION 197K
Sample: Transfer a volume of Oral Suspension, equivalent to 240 mg of acetaminophen, to a separator. Add
50 mL of ethyl acetate, and shake. Filter the ethyl acetate extract through a funnel containing glass wool and
10 g of anhydrous sodium sulfate. Collect the filtrate in
a beaker, and evaporate on a steam bath to dryness.
Dry the residue under vacuum over silica gel.
Acceptance criteria: The crystals so obtained meet the
requirements.
ASSAY
PROCEDURE
Mobile phase: Methanol and water (1:3)
Standard solution: 0.01 mg/mL of USP Acetaminophen
RS in Mobile phase
Sample stock solution: Nominally 0.5 mg/mL of acetaminophen prepared as follows. Transfer 100 mg of
acetaminophen from a volume of Oral Suspension, previously well shaken, to a 200-mL volumetric flask. Add
100 mL of Mobile phase, and shake by mechanical
means for 10 min. Dilute with Mobile phase to volume.
Sample solution: Nominally 0.01 mg/mL of acetaminophen from the Sample stock solution in Mobile phase.
Pass a portion of this solution through a filter of 0.5-m
pore size or finer, discarding the first 10 mL of the filtrate. Use the clear filtrate.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 243 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 1.5 mL/min
Injection volume: 10 L
System suitability
Sample: Standard solution
Suitability requirements
Column efficiency: NLT 1000 theoretical plates
Tailing factor: NMT 2.0
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of acetaminophen (C8H9NO2) in the portion of Oral Suspension taken:
Result = (rU/rS) (CS/CU) 100
rU
rS
CS

= peak response from the Sample solution

= peak response from the Standard solution
= concentration of USP Acetaminophen RS in
the Standard solution (mg/mL)
CU
= nominal concentration of acetaminophen in
the Sample solution (mg/mL)
Acceptance criteria: 90.0%110.0%
PERFORMANCE TESTS
UNIFORMITY OF DOSAGE UNITS 905: Meets the requirements for oral suspensions packaged in single-unit
containers

Official from December 1, 2014

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.

Accessed from 10.6.1.1 by kalbefarma on Mon Mar 02 00:34:22 EST 2015

Second Supplement to USP 37NF 32

DELIVERABLE VOLUME 698: Meets the requirements for
oral suspensions packaged in multiple-unit containers
IMPURITIES
Delete the following:

LIMIT OF 4-AMINOPHENOL
Solvent A: Methanol, formic acid, and water (75:2:425)
Mobile phase: 0.01 M sodium butanesulfonate in Solvent A
Standard solution: 24 g/mL of USP 4-Aminophenol
RS in Mobile phase
Sample solution: Equivalent to 4.8 mg/mL of acetaminophen from Oral Suspension in Mobile phase
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 272 nm
Column: 4.6-mm 20-cm; 10-m packing L1
Flow rate: 2.0 mL/min
Injection volume: 20 L
Analysis
Samples: Standard solution and Sample solution
Acceptance criteria: The peak area for 4-aminophenol
from the Sample solution is not greater than the corresponding peak area from the Standard solution.2S (USP37)

Add the following:

4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG

PRODUCTS 227: Meets the requirements2S (USP37)

SPECIFIC TESTS
PH 791: 4.06.9
ADDITIONAL REQUIREMENTS
PACKAGING AND STORAGE: Preserve in tight containers,
and store at controlled room temperature.
USP REFERENCE STANDARDS 11
USP Acetaminophen RS
USP 4-Aminophenol RS

Acetaminophen Tablets
DEFINITION
Acetaminophen Tablets contain NLT 90.0% and NMT
110.0% of the labeled amount of acetaminophen
(C8H9NO2).
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.
B. THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST
201
Sample solution: Nominally 1 mg/mL of acetaminophen prepared as follows. Triturate 50 mg of acetaminophen from powdered Tablets in 50 mL of methanol,
and filter. Use the clear filtrate.
Chromatographic system
Developing solvent system: Methylene chloride and
methanol (4:1)
Acceptance criteria: Meet the requirements
ASSAY
PROCEDURE
Mobile phase: Methanol and water (1:3)
Standard solution: 0.01 mg/mL of USP Acetaminophen
RS in Mobile phase

Official Monographs / Acetaminophen 7103

Sample stock solution: Nominally 0.5 mg/mL of acetaminophen prepared as follows. Weigh, and finely powder NLT 20 Tablets. Transfer 100 mg of acetaminophen
from a portion of powdered Tablets to a 200-mL volumetric flask, add 100 mL of Mobile phase, shake by mechanical means for 10 min, sonicate for 5 min, and
dilute with Mobile phase to volume.
Sample solution: Nominally 0.01 mg/mL of acetaminophen in Mobile phase from the Sample stock solution.
Pass a portion of this solution through a filter of 0.5-m
or finer pore size, discarding the first 10 mL of the filtrate. Use the clear filtrate.
Chromatographic system
(See Chromatography 621, System Suitability.)
Mode: LC
Detector: UV 243 nm
Column: 3.9-mm 30-cm; packing L1
Flow rate: 1.5 mL/min
Injection volume: 10 L
System suitability
Sample: Standard solution
Suitability requirements
Column efficiency: NLT 1000 theoretical plates
Tailing factor: NMT 2
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of acetaminophen (C8H9NO2) in the portion of Tablets taken:
Result = (rU/rS) (CS/CU) 100
rU
rS
CS

= peak response from the Sample solution

= peak response from the Standard solution
= concentration of USP Acetaminophen RS in
the Standard solution (mg/mL)
CU
= nominal concentration of acetaminophen in
the Sample solution (mg/mL)
Acceptance criteria: 90.0%110.0%
PERFORMANCE TESTS
DISSOLUTION 711
Medium: pH 5.8 phosphate buffer (see Reagents, Indicators, and SolutionsBuffer Solutions); 900 mL
Apparatus 2: 50 rpm
Time: 30 min
Standard solution: A known concentration of USP
Acetaminophen RS in Medium
Sample solution: A filtered portion of the solution
under test, suitability diluted with Medium to obtain a
concentration similar to that of the Standard solution
Instrumental conditions
Mode: UV
Analytical wavelength: Maximum absorbance at
about 243 nm
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of the labeled amount of acetaminophen (C8H9NO2) dissolved.
Tolerances: NLT 80% (Q) of the labeled amount of
acetaminophen (C8H9NO2) is dissolved.
For Tablets labeled as chewable
Medium: pH 5.8 phosphate buffer (see Reagents, Indicators, and SolutionsBuffer Solutions); 900 mL
Apparatus 2: 75 rpm
Time: 45 min
Standard solution, Sample solution, Instrumental
conditions, and Analysis: Proceed as directed above.
Tolerances: NLT 75% (Q) of the labeled amount of
acetaminophen (C8H9NO2) is dissolved.
UNIFORMITY OF DOSAGE UNITS 905: Meet the
requirements

Official from December 1, 2014

Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.