Accessed from 10.6.1.
1 by merck1 on Mon May 11 20:43:30 EDT 2015
2008 Acetaminophen / Official Monographs
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 µL
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:
Result = (rU/rS) × (CS/CU) × (1/F1) × L × F2
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = 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: 5.63–6.88 g
PERFORMANCE TESTS
• MINIMUM FILL 〈755〉: Meets the requirements for solids
packaged in multiple-unit containers
• UNIFORMITY OF DOSAGE UNITS 〈905〉: Meets the require-
USP Monographs
ments for solids packaged in single-unit containers
IMPURITIES
• 4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG
PRODUCTS 〈227〉: Meets the requirements
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in air-tight containers,
and store at controlled room temperature.
• USP REFERENCE STANDARDS 〈11〉
USP Acetaminophen RS
.
Acetaminophen Suppositories
DEFINITION
Acetaminophen Suppositories contain NLT 90.0% and NMT
110.0% of the labeled amount of acetaminophen
(C8H9NO2).
IDENTIFICATION
• A. The retention time of the chromatogram of the Sam-
ple solution corresponds to that of the Standard solution,
as obtained in the Assay.
• B. THIN-LAYER CHROMATOGRAPHIC IDENTIFICATION TEST
〈201〉
Sample solution: Transfer a portion of Suppositories,
equivalent to 20 mg of acetaminophen, to a beaker.
Add 20 mL of methanol, and heat on a steam bath un-
til melted. Remove the beaker from the steam bath,
allow to cool with occasional stirring, and filter.
Chromatographic system
Developing solvent system: Methylene chloride and
methanol (4:1)
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
USP 38
Acceptance criteria: The clear filtrate meets the
requirements.
ASSAY
Change to read:
• PROCEDURE
Mobile phase: Methanol and water (1:3)
Standard solution: 0.01 mg/mL of USP Acetaminophen
RS in Mobile phase
Sample stock solution: Tare a small dish and a glass
rod, place NLT 5 Suppositories in the dish, heat gently
on a steam bath until melted, stir, cool while stirring,
and weigh. Transfer a weighed portion of the mass,
equivalent to 100 mg of acetaminophen, to a separator,
•add 30 mL of solvent hexane,• (ERR 1-Jun-2014) and dis-
.
solve. Add 30 mL of water, shake gently, and allow the
phases to separate. If an emulsion forms, allow suffi-
cient time for it to separate. Transfer the aqueous layer
to a 200-mL volumetric flask, •wash the solvent hex-
.
ane• (ERR 1-Jun-2014) in the separator with three 30-mL por-
tions of water, adding the washings to the volumetric
flask, and dilute with Mobile phase to volume.
Sample solution: Transfer 5.0 mL of the Sample stock
solution to a 250-mL volumetric flask, and dilute with
Mobile phase to volume. Pass a portion of this solution
through a filter of 0.5-µm 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 µL
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 each Suppository taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = 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%
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers,
and store at controlled room temperature or in a cool
place.
• USP REFERENCE STANDARDS 〈11〉
USP Acetaminophen RS
.
Acetaminophen Oral Suspension
DEFINITION
Acetaminophen Oral Suspension is a suspension of Acet-
aminophen in a suitable aqueous vehicle. It contains NLT
90.0% and NMT 110.0% of the labeled amount of acet-
aminophen (C8H9NO2).
Accessed from 10.6.1.1 by merck1 on Mon May 11 20:43:30 EDT 2015
USP 38
IDENTIFICATION
• A. INFRARED ABSORPTION 〈197K〉
Sample: Transfer a volume of Oral Suspension, equiva-
lent to 240 mg of acetaminophen, to a separator. Add
50 mL of ethyl acetate, and shake. Filter the ethyl ace-
tate 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 acet-
aminophen prepared as follows. Transfer 100 mg of
acetaminophen from a volume of Oral Suspension, pre-
viously 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 acetamino-
phen from the Sample stock solution in Mobile phase.
Pass a portion of this solution through a filter of 0.5-µm
pore size or finer, discarding the first 10 mL of the fil-
trate. 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 µL
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 acet-
aminophen (C8H9NO2) in the portion of Oral Suspen-
sion taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = 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 require-
ments for oral suspensions packaged in single-unit
containers
• DELIVERABLE VOLUME 〈698〉: Meets the requirements for
oral suspensions packaged in multiple-unit containers
IMPURITIES
• 4-AMINOPHENOL IN ACETAMINOPHEN-CONTAINING DRUG
PRODUCTS 〈227〉: Meets the requirements
SPECIFIC TESTS
• PH 〈791〉: 4.0–6.9
ADDITIONAL REQUIREMENTS
• PACKAGING AND STORAGE: Preserve in tight containers,
and store at controlled room temperature.
Official from May 1, 2015
Copyright (c) 2015 The United States Pharmacopeial Convention. All rights reserved.
Official Monographs / Acetaminophen 2009
• 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 acetamino-
phen prepared as follows. Triturate 50 mg of acetamin-
ophen 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
Sample stock solution: Nominally 0.5 mg/mL of acet-
aminophen prepared as follows. Weigh, and finely pow-
der NLT 20 Tablets. Transfer 100 mg of acetaminophen
from a portion of powdered Tablets to a 200-mL volu-
USP Monographs
metric flask, add 100 mL of Mobile phase, shake by me-
chanical means for 10 min, sonicate for 5 min, and
dilute with Mobile phase to volume.
Sample solution: Nominally 0.01 mg/mL of acetamino-
phen in Mobile phase from the Sample stock solution.
Pass a portion of this solution through a filter of 0.5-µm
or finer pore size, discarding the first 10 mL of the fil-
trate. 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 µL
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 acet-
aminophen (C8H9NO2) in the portion of Tablets taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution