USP Aspartame

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Printed on: Mon May 08 2023, 10:21:17 PM(EST) Status: Currently Official on 09-May-2023 DocId: GUID-0B161E00-C2E8-4232-8E54-4E7AE6BF70C2_4_en-US

Printed by: Rahmawati Ekaputri Official Date: Official as of 01-May-2020 Document Type: NF @2023 USPC
Do Not Distribute DOI Ref: 3s5c9 DOI: https://doi.org/10.31003/USPNF_M6195_04_01
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CU = concentration of Aspartame in the Sample


Aspartame solution (mg/mL)

Acceptance criteria: 98.0%–102.0% on the dried basis


IMPURITIES
• RESIDUE ON IGNITION á281ñ: NMT 0.2%
• LIMIT OF 5-BENZYL-3,6-DIOXO-2-PIPERAZINEACETIC ACID
C14H18N2O5 294.30 Mobile phase, Diluent, System suitability solution, and
Chromatographic system: Proceed as directed in the
L-Phenylalanine,
N-L-α-aspartyl-, 1-methyl ester;
Assay.
3-Amino-N-(α-carboxyphenethyl)succinamic acid N-methyl
Standard solution: 75 µg/mL of USP Aspartame Related
ester CAS RN®: 22839-47-0.
Compound A RS in Diluent
DEFINITION Sample solution: 5 mg/mL of Aspartame in Diluent.
Aspartame contains NLT 98.0% and NMT 102.0% of [NOTE—Avoid heat and excessive holding times.]
aspartame (C14H18N2O5), calculated on the dried basis. System suitability
Samples: System suitability solution and Standard solution
IDENTIFICATION Suitability requirements
Change to read:
Resolution: NLT 8 between the L-phenylalanine and
aspartame related compound A peaks, System suitability
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared solution
Spectroscopy: 197M▲ (CN 1-May-2020) Tailing factor: NMT 2.0, Standard solution
[NOTE—Do not dry specimens.] Relative standard deviation: NMT 4.0%, Standard

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solution
ASSAY Analysis
• PROCEDURE Samples: Standard solution and Sample solution
Buffer: 0.05 M monobasic potassium phosphate, adjusted [NOTE—Continue the elution of the Sample solution for
with phosphoric acid to a pH of 4.3 ci 45 min.]
Mobile phase: Methanol and Buffer (18:82) Calculate the percentage of aspartame related compound A
Diluent: Methanol and water (1:9) in the portion of Aspartame taken:
System suitability solution: 0.1 mg/mL each of USP
Aspartame Related Compound A RS and USP Result = (r U/r S) × (C S/C U) × 100
l-Phenylalanine RS in Diluent
Standard solution: 0.5 mg/mL of USP Aspartame RS in rU = peak response of aspartame related compound A
ffi
Diluent from the Sample solution
Sample solution: 0.5 mg/mL of Aspartame in Diluent. rS = peak response of aspartame related compound A
[NOTE—Avoid heat and excessive holding times.] from the Standard solution
Chromatographic system CS = concentration of 5-benzyl-3,6-dioxo-
(See Chromatography á621ñ, System Suitability.) 2-piperazineacetic acid in the Standard solution
Mode: LC (mg/mL)
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Detector: UV 210 nm CU = concentration of Aspartame in the Sample


Column: 4.6-mm × 25-cm; 5-µm packing L1 solution (mg/mL)
Column temperature: 40°
Flow rate: 2 mL/min Acceptance criteria: NMT 1.5%
Injection volume: 20 µL • CHROMATOGRAPHIC PURITY
Run time: 30 min Mobile phase, Diluent, System suitability solution, and
System suitability Chromatographic system: Proceed as directed in the
Samples: System suitability solution and Standard solution Assay.
[NOTE—The relative retention times for the Sample stock solution: Proceed as directed in the Sample
L-phenylalanine and aspartame related compound A solution in the test for Limit of 5-Benzyl-3,6-dioxo-
peaks are 0.6 and 1.0, respectively.] 2-piperazineacetic Acid.
Suitability requirements Sample solution: 0.1 mg/mL of Aspartame from the Sample
Resolution: NLT 8 between the L-phenylalanine and stock solution in Diluent
aspartame related compound A peaks, System suitability System suitability
solution Sample: System suitability solution
Tailing factor: NMT 1.5, Standard solution Suitability requirements
Relative standard deviation: NMT 1.0%, Standard Resolution: NLT 8 between the L-phenylalanine and
solution aspartame related compound A peaks, System suitability
Analysis solution
Samples: Standard solution and Sample solution Analysis
Calculate the percentage of aspartame (C14H18N2O5) in the Samples: Sample stock solution and Sample solution
portion of Aspartame taken: [NOTE—Continue the elution of the Sample stock
solution for 45 min.]
Result = (r U/r S) × (C S/C U) × 100 Acceptance criteria: The sum of all of the peak responses of
the Sample stock solution, excluding the 5-benzyl-
rU = peak area of aspartame from the Sample solution 3,6-dioxo-2-piperazineacetic acid and aspartame peak
rS = peak area of aspartame from the Standard solution responses, is NMT the aspartame peak response of the
CS = concentration of USP Aspartame RS in the Sample solution, corresponding to NMT 2.0% of
Standard solution (mg/mL) chromatographic impurities.

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Printed on: Mon May 08 2023, 10:21:17 PM(EST) Status: Currently Official on 09-May-2023 DocId: GUID-0B161E00-C2E8-4232-8E54-4E7AE6BF70C2_4_en-US
Printed by: Rahmawati Ekaputri Official Date: Official as of 01-May-2020 Document Type: NF @2023 USPC
Do Not Distribute DOI Ref: 3s5c9 DOI: https://doi.org/10.31003/USPNF_M6195_04_01
2

SPECIFIC TESTS Acceptance criteria: NMT 4.5%


• TRANSMITTANCE
Sample solution: 10 mg/mL of Aspartame in 2 N ADDITIONAL REQUIREMENTS
hydrochloric acid, prepared by means of sonication • PACKAGING AND STORAGE: Preserve in well-closed
Analysis: Determine the transmittance in a 1-cm cell at containers.
430 nm with a suitable spectrophotometer. • USP REFERENCE STANDARDS á11ñ
Acceptance criteria: Transmittance of NLT 0.95, USP Aspartame RS
corresponding to an absorbance of NMT about 0.022 USP Aspartame Related Compound A RS
• OPTICAL ROTATION, Specific Rotation á781Sñ 5-Benzyl-3,6-dioxo-2-piperazineacetic acid.
Sample solution: 40 mg/mL in 15 N formic acid C13H14N2O4 262.27
Acceptance criteria: +14.5° to +16.5°, determined at 20° USP l-Phenylalanine RS
within 30 min after preparation of the Sample solution
• LOSS ON DRYING á731ñ
Analysis: Dry at 105° for 4 h.

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