Printed on: Wed Feb 08 2023, 11:46:47 PM(EST) Status: Currently Official on 09-Feb-2023 DocId: GUID-99D8A3EC-D6A0-4C60-A4A4-BCF7390AA587_4_en-US

Printed by: Dang Van Vu Official Date: Official as of 01-May-2020 Document Type: NF @2023 USPC
Do Not Distribute DOI Ref: ch0h7 DOI: https://doi.org/10.31003/USPNF_M145_04_01
1

dilute with water to volume. Each mL of this solution

Acesulfame Potassium contains 10 µg of fluoride ion.
Standard solution A: Mix 0.5 mL of Standard stock solution
and 15.0 mL of Buffer solution, and dilute with water to
50 mL.
Standard solution B: Mix 1.0 mL of Standard stock solution
and 15.0 mL of Buffer solution, and dilute with water to
C4H4NO4SK 201.24 50 mL.
6-Methyl-1,2,3-oxathiazine-4(3H)-one-2,2-dioxide potassium Standard solution C: Mix 1.5 mL of Standard stock solution
salt; and 15.0 mL of Buffer solution, and dilute with water to
3,4-Dihydro-6-methyl-1,2,3-oxathiazine-4-one-2,2-dioxide 50 mL.
potassium salt CAS RN®: 55589-62-3. Standard solution D: Mix 3.0 mL of Standard stock solution
and 15.0 mL of Buffer solution, and dilute with water to
DEFINITION 50 mL.
Acesulfame Potassium contains NLT 99.0% and NMT 101.0% Sample solution: To a 50-mL volumetric flask add 3 g of
of C4H4NO4SK, calculated on the dried basis. Acesulfame Potassium. Dissolve in water, add 15.0 mL of
IDENTIFICATION Buffer solution, and dilute with water to volume.
Analysis
Change to read: Samples: Standard solution A, Standard solution B, Standard
solution C, Standard solution D, and Sample solution
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared Concomitantly measure the potential (see Titrimetry
Spectroscopy: 197K▲ (CN 1-May-2020) á541ñ), in mV, of the Standard solutions and the Sample
• B. IDENTIFICATION TESTS—GENERAL, Potassium á191ñ

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solution, with a suitable pH meter equipped with a
Sample solution: 100 mg/mL fluoride-specific ion electrode and a silver–silver chloride
Acceptance criteria: Meets the requirements reference electrode. When taking the measurements,
ASSAY transfer the solution to a 25-mL beaker, and immerse the
• PROCEDURE electrodes. Insert a polytef-coated stirring bar into the
beaker, place the beaker on a magnetic stirrer having an
Sample: 150 mg
Titrimetric system
(See Titrimetry á541ñ.)
Mode: Direct titration
ci insulated top, and allow to stir until equilibrium is
attained (1–2 min). Rinse, and dry the electrodes
between measurements, taking care not to scratch the
Titrant: 0.1 N perchloric acid VS crystal in the fluoride-specific ion electrode. Measure the
Blank: 50 mL of glacial acetic acid potential of each Standard solution, and plot the fluoride
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Endpoint detection: Potentiometric concentration, in µg/mL, versus the potential, in mV, on
Analysis: Dissolve the Sample in 50 mL of glacial acetic acid. semilogarithmic paper. Measure the potential of the
Titrate with 0.1 N perchloric acid VS. Perform a blank Sample solution, and determine the fluoride
determination. concentration from the standard curve, in µg/mL.
Calculate the percentage of acesulfame potassium Calculate the content, in ppm, of fluoride in the portion of
(C4H4NO4SK) in the Sample: Acesulfame Potassium taken:
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Result = (V × C/W)
Result = [(V − B) × N × F × 100]/W
V = volume of the Sample solution (mL)
V = titrant volume consumed by the Sample (mL)
C = concentration of fluoride in the Sample solution,
B = titrant volume consumed by the Blank (mL)
from the standard curve (µg/mL)
N = titrant actual normality (mEq/mL)
W = weight of Acesulfame Potassium taken to
F = equivalency factor, 201.2 mg/mEq
prepare the Sample solution (g)
W = weight of Sample (mg)
Acceptance criteria: NMT 3 ppm
Acceptance criteria: 99.0%–101.0% on the dried basis
• CHROMATOGRAPHIC PURITY
IMPURITIES Solution A: 3.3 mg/mL of tetrabutylammonium hydrogen
• LIMIT OF FLUORIDE sulfate
[NOTE—Use plasticware throughout this test.] Mobile phase: Acetonitrile and Solution A (2:3)
Solution A: Dissolve 210 g of citric acid monohydrate in System suitability solution: 2 µg/mL each of USP
400 mL of water. Adjust with concentrated ammonia to a Acesulfame Potassium RS and ethylparaben
pH of 7.0, and dilute with water to 1000 mL. Standard solution: 0.2 µg/mL of USP Acesulfame
Solution B: 132 mg/mL of dibasic ammonium phosphate Potassium RS
Solution C: To a suspension of 292 g of edetic acid in Sample solution: 10 mg/mL
500 mL of water, add 200 mL of ammonium hydroxide, Chromatographic system
adjust with ammonium hydroxide to a pH between 6 and (See Chromatography á621ñ, System Suitability.)
7, and dilute with water to make 1000 mL. Mode: LC
Buffer solution: Mix equal volumes of Solution A, Detector: UV 227 nm
Solution B, and Solution C, and adjust with ammonium Column: 4.6-mm × 25-cm; 5-µm packing L1
hydroxide to a pH of 7.5. Flow rate: 1 mL/min
Standard stock solution: Weigh 0.442 g of sodium fluoride, Injection size: 20 µL
previously dried at 300° for 12 h, into a 1-L volumetric flask, System suitability
and dilute with water to volume. Store the solution in a Sample: System suitability solution
closed plastic container. Immediately before use, pipet Suitability requirements
5 mL of this solution into a 100-mL volumetric flask, and Resolution: NLT 2 between acesulfame potassium and
ethylparaben

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Printed on: Wed Feb 08 2023, 11:46:47 PM(EST) Status: Currently Official on 09-Feb-2023 DocId: GUID-99D8A3EC-D6A0-4C60-A4A4-BCF7390AA587_4_en-US
Printed by: Dang Van Vu Official Date: Official as of 01-May-2020 Document Type: NF @2023 USPC
Do Not Distribute DOI Ref: ch0h7 DOI: https://doi.org/10.31003/USPNF_M145_04_01
2

Analysis produce a blue color. If the solution is blue, titrate with

Samples: Standard solution and Sample solution 0.01 N hydrochloride acid to produce a yellow color.
Record the chromatograms for a run time NLT 3 times the Acceptance criteria: NMT 0.2 mL of 0.01 N sodium
retention time of the acesulfame potassium peak, and hydroxide or NMT 0.2 mL of 0.01 N hydrochloric acid is
measure the area responses of the peaks. required.
Acceptance criteria: The response of any peak at a retention • LOSS ON DRYING á731ñ: Dry a sample at 105° for 3 h: it loses
time other than that of acesulfame potassium from the NMT 1.0% of its weight.
Sample solution does not exceed the response of the
acesulfame potassium peak from the Standard solution ADDITIONAL REQUIREMENTS
(0.002%). • PACKAGING AND STORAGE: Preserve in a well-closed
container, and protect from light. Store at room
SPECIFIC TESTS temperature.
• ACIDITY OR ALKALINITY • USP REFERENCE STANDARDS á11ñ
Sample solution: 4.0 g in 20 mL of carbon dioxide-free USP Acesulfame Potassium RS
water
Analysis: Add 0.1 mL of bromothymol blue TS. If the
solution is yellow, titrate with 0.01 N sodium hydroxide to

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