Printed on: Thu Feb 09 2023, 01:00:52 AM(EST) Status: Not Yet Official on 09-Feb-2023 DocId: GUID-C825B45A-6BC9-4745-9CA8-369E1AB1FC22_5_en-US
Printed by: Dang Van Vu Official Date: 01-Jun-2023 Document Type: USP & DS @2023 USPC
Do Not Distribute DOI Ref: 4dc26 DOI: https://doi.org/10.31003/USPNF_M1130_05_01
1
Fumaric acid standard solution: 0.05 mg/mL of USP
Alanine Fumaric Acid RS in water
Sample solution: 100 mg/mL of Alanine in water
Chromatographic system
(See Chromatography á621ñ, System Suitability.)
Mode: LC
Detector: UV 214 nm
Column: 7.8-mm × 30-cm; 9-µm packing L17
Column temperature: 30°
Flow rate: 0.6 mL/min
C3H7NO2 89.09 Injection volume: 10 µL
L-Alanine CAS RN®: 56-41-7; UNII: OF5P57N2ZX. System suitability
Sample: System suitability solution
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DEFINITION [NOTE—See Table 1 for the relative retention times.]
Alanine contains NLT 98.5% and NMT 101.5% of L-alanine Suitability requirements
(C3H7NO2), calculated on the dried basis. Resolution: NLT 1.5 between maleic acid and malic acid
Relative standard deviation: NMT 5.0% for each of
IDENTIFICATION fumaric acid, maleic acid, and malic acid
• A. SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared
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Analysis
Spectroscopy: 197K Samples: Standard solutions and Sample solution
ASSAY Calculate the percentage of each specified acid in the
• PROCEDURE portion of Alanine taken:
Sample: 80 mg of Alanine
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Titrimetric system Result = (r U/r S) × (C S/C U) × 100
(See Titrimetry á541ñ.)
Mode: Direct titration rU = peak response of maleic acid, malic acid, or
Titrant: 0.1 N perchloric acid VS fumaric acid from the Sample solution
Endpoint detection: Potentiometric rS = peak response of maleic acid, malic acid, or
Blank: 3 mL of formic acid in 50 mL of glacial acetic acid fumaric acid from the corresponding Standard
solution
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Analysis: Dissolve the Sample in a mixture of 3 mL of formic
acid and 50 mL of glacial acetic acid, and titrate with CS = concentration of USP Maleic Acid RS, USP Malic
Titrant. Acid RS, or USP Fumaric Acid RS in the
Calculate the percentage of L-alanine (C3H7NO2) in the corresponding Standard solution (mg/mL)
portion of Alanine taken: CU = concentration of Alanine in the Sample solution
(mg/mL)
Result = [(V S − V B) × N × F × 100]/W
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Calculate the percentage of any unspecified impurity in the
VS = Titrant volume consumed by the Sample (mL) portion of Alanine taken:
VB = Titrant volume consumed by the Blank (mL)
Result = (r U/r S) × (C S/C U) × 100
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N = actual normality of the Titrant (mEq/mL)
F = equivalency factor, 89.09 mg/mEq rU = peak response of any unspecified impurity from
W = Sample weight (mg) the Sample solution
rS = peak response of fumaric acid from the Fumaric
Acceptance criteria: 98.5%–101.5% on the dried basis acid standard solution
IMPURITIES CS = concentration of USP Fumaric Acid RS in the
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• RESIDUE ON IGNITION á281ñ: NMT 0.15% Fumaric acid standard solution (mg/mL)
• CHLORIDE AND SULFATE, Chloride á221ñ CU = concentration of Alanine in the Sample solution
Standard solution: 0.70 mL of 0.020 N hydrochloric acid (mg/mL)
Sample: 1.0 g of Alanine
Acceptance criteria: NMT 0.05% Acceptance criteria: See Table 1.
• CHLORIDE AND SULFATE, Sulfate á221ñ
Standard solution: 0.30 mL of 0.020 N sulfuric acid Table 1
Sample: 1.0 g of Alanine Relative Acceptance
Acceptance criteria: NMT 0.03% Retention Criteria,
Name Time NMT (%)
Change to read: Maleic acid 0.5 0.05
Malic acid 0.6 0.05
• ▲IRON á241ñ, Procedures, Procedure 1▲ (CN 1-Jun-2023): NMT
30 ppm Fumaric acid 1.0 0.05
• RELATED COMPOUNDS
Alanine Not observed —
Mobile phase: 0.008 N sulfuric acid solution
System suitability solution: A mixture of 0.05 mg/mL of Any unspecified
—
USP Fumaric Acid RS, 0.05 mg/mL of USP Maleic Acid RS, impurity 0.05
and 3 mg/mL of USP Malic Acid RS in water Total unspecified im-
Maleic acid standard solution: 0.05 mg/mL of USP Maleic —
purities 0.20
Acid RS in water
Malic acid standard solution: 3 mg/mL of USP Malic Acid
RS in water
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Printed on: Thu Feb 09 2023, 01:00:52 AM(EST) Status: Not Yet Official on 09-Feb-2023 DocId: GUID-C825B45A-6BC9-4745-9CA8-369E1AB1FC22_5_en-US
Printed by: Dang Van Vu Official Date: 01-Jun-2023 Document Type: USP & DS @2023 USPC
Do Not Distribute DOI Ref: 4dc26 DOI: https://doi.org/10.31003/USPNF_M1130_05_01
2
SPECIFIC TESTS ADDITIONAL REQUIREMENTS
• OPTICAL ROTATION, Specific Rotation á781Sñ • PACKAGING AND STORAGE: Preserve in tight containers, and
Sample solution: 100 mg/mL in 6 N hydrochloric acid store at controlled room temperature.
Acceptance criteria: +13.7° to +15.1° • USP REFERENCE STANDARDS á11ñ
• PH á791ñ: 5.5–7.0, in a solution (1 in 20) USP l-Alanine RS
• LOSS ON DRYING á731ñ USP Fumaric Acid RS
Analysis: Dry at 105° for 3 h. USP Maleic Acid RS
Acceptance criteria: NMT 0.2% USP Malic Acid RS
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