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Printed by: USP NF Official Date: Official as of 01-May-2020 Document Type: NF @2024 USPC
Do Not Distribute DOI Ref: xnp2n DOI: https://doi.org/10.31003/USPNF_M52650_02_01
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Standard solution C: Dilute 1.0 mL of the Sample solution

Methylparaben with Mobile phase to 20.0 mL. Dilute 1.0 mL of this solution
with Mobile phase to 10.0 mL.
Chromatographic system
(See Chromatography á621ñ, System Suitability.)
Mode: LC
Detector: UV 272 nm
C8H8O3 152.15 Column: 4.6-mm × 15-cm; 5-µm packing L1
Benzoic acid, 4-hydroxy-, methyl ester; Flow rate: 1.3 mL/min
Methyl p-hydroxybenzoate CAS RN®: 99-76-3. Injection size: 10 µL
Run time: About 5 times the retention time of
DEFINITION methylparaben
Methylparaben contains NLT 98.0% and NMT 102.0% System suitability
of C8H8O3. Sample: Standard solution A
IDENTIFICATION [NOTE—The retention time of methylparaben is about
2.3 min; the relative retention time for p-hydroxy
Change to read: benzoic acid is about 0.6.]
Suitability requirements
• A. ▲SPECTROSCOPIC IDENTIFICATION TESTS á197ñ, Infrared Resolution: NLT 2.0 between the p-hydroxybenzoic acid
Spectroscopy: 197M▲ (CN 1-May-2020) and methylparaben peaks
• B. MELTING RANGE OR TEMPERATURE á741ñ: 125°–128° Analysis
ASSAY Samples: Sample solution and Standard solution C

al
• PROCEDURE [NOTE—Disregard any limit that is 0.2 times the area of the
Mobile phase, Sample solution, Standard solution B, and principal peak in the chromatogram obtained with
Chromatographic system: Proceed as described in the Standard solution C (0.1%).]
procedure for Related Substances. Acceptance criteria
System suitability p-Hydroxybenzoic acid: The peak area in the Sample
solution, multiplied by 1.4 to correct for the calculation of
Sample: Standard solution B
Suitability requirements
Relative standard deviation: NMT 0.85% for 6
injections
ci content, is NMT the area of the principal peak in Standard
solution C (0.5%).
Unspecified impurities: The peak area of each impurity in
Analysis the Sample solution is NMT the area of the principal peak in
Samples: Sample solution and Standard solution B Standard solution C (0.5%).
ffi
Calculate the percentage of Methylparaben in the Sample Total impurities: The total peak area for all impurities in the
solution: Sample solution is NMT twice the area of the principal peak
in Standard solution C (1.0%).
Result = P × (rU × CS)/(rS × CU) SPECIFIC TESTS
• COLOR OF SOLUTION
P = labeled purity of USP Methylparaben RS
O

Sample solution: 100 mg/mL in alcohol

expressed as a percentage Comparison solution: Mix 2.4 mL of ferric chloride CS,
rU = peak area of methylparaben from the Sample 1.0 mL of cobaltous chloride CS, and 0.4 mL of cupric
solution sulfate CS with 0.3 N hydrochloric acid to make 10 mL.
CS = concentration of methylparaben in Standard Dilute 5 mL of this solution with 0.3 N hydrochloric acid to
solution B make 100 mL. [NOTE—Prepare and use this solution
rS = peak area of methylparaben from Standard immediately.]
solution B Analysis
CU = concentration of Methylparaben in the Sample Samples: Alcohol, Sample solution, and Comparison
solution solution
Make the comparison by viewing the solutions downward in
Acceptance criteria: 98.0%–102.0% matched color-comparison tubes against a white surface
IMPURITIES (see Color and Achromicity á631ñ).
INORGANIC IMPURITIES Acceptance criteria: The Sample solution is clear and not
• Residue on Ignition á281ñ: NMT 0.1%, determined on more intensely colored than alcohol or the Comparison
1.0 g solution.
ORGANIC IMPURITIES • ACIDITY
• Procedure: Related Substances Sample solution: To 2 mL of the Sample solution prepared
Mobile phase: Methanol and a 6.8 g/L solution of potassium in the test for Color of Solution, add 3 mL of alcohol, 5 mL
dihydrogen phosphate (65:35 v/v) of carbon dioxide-free water, and 0.1 mL of bromocresol
Sample solution: Dissolve 50.0 mg of Methylparaben in green TS.
2.5 mL of methanol, and dilute with Mobile phase to 50.0 mL. Analysis: Titrate with 0.10 N sodium hydroxide.
Dilute 10.0 mL of this solution with Mobile phase to Acceptance criteria: NMT 0.1 mL is required to produce a
100.0 mL. blue color.
Standard solution A: 5.0 µg/mL each of p-hydroxy benzoic ADDITIONAL REQUIREMENTS
acid and USP Methylparaben RS in Mobile phase • PACKAGING AND STORAGE: Preserve in well-closed
Standard solution B: Dissolve 50.0 mg of USP containers.
Methylparaben RS in 2.5 mL of methanol, and dilute with • USP REFERENCE STANDARDS á11ñ
Mobile phase to 50.0 mL. Dilute 10.0 mL of this solution with USP Methylparaben RS
Mobile phase to 100.0 mL.

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