Menadione

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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1 DEFINITION

Menadione contains NLT 98.5% and NMT 101.0% of menadione (C₁₁H₈O₂), calculated on the dried basis.

[Caution—Menadione powder is irritating to the respiratory tract and to the skin, and a solution of it in alcohol is a vesicant.]

2 IDENTIFICATION

Change to read:

A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197K (CN 1-May-2020)

Change to read:

B. Spectroscopic Identification Tests 〈197〉, Ultraviolet-Visible Spectroscopy: 197U (CN 1-May-2020)

Standard solution: 5 μg/mL of USP Menadione RS in alcohol

Sample solution: 5 μg/mL in alcohol

Analytical wavelength: 250 nm

Acceptance criteria: Absorptivities, calculated on the dried basis, do not differ by more than 3.0%.

3 ASSAY

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Procedure

Sample solution: Transfer about 150 mg of Menadione into a 150-mL volumetric flask. Add 15 mL each of glacial acetic acid and 3 N hydrochloric acid, and rotate the flask until Menadione is dissolved. Add about 3 g of zinc dust, and close the flask with a stopper bearing a Bunsen valve. Shake, and allow to stand in the dark for 1 h, with frequent shaking. Rapidly decant the solution through a pledget of cotton into another flask, immediately wash the reduction flask with three 10-mL portions of freshly boiled and cooled water, and add 0.1 mL of orthophenanthroline TS.

Titrimetric system

Mode: Direct titration

Titrant: 0.1 N ceric sulfate VS

Endpoint detection: Visual (ERR 1-May-2020)

Analysis: Immediately titrate the combined filtrate and washings with Titrant. Perform a blank determination, and make any necessary correction. Each mL of 0.1 N ceric sulfate is equivalent to 8.609 mg of menadione (C₁₁H₈O₂).

Acceptance criteria: 98.5%–101.0% on the dried basis

4 IMPURITIES

Residue on Ignition 〈281〉: NMT 0.1%

Ordinary Impurities 〈466〉

Standard solution and Sample solution: Methanol

Eluant: Chloroform

Visualization: 1

Acceptance criteria: Meets the requirements

5 SPECIFIC TESTS

Melting Range or Temperature, Class I 〈741〉: 105°–107°

Loss on Drying 〈731〉

Analysis: Dry over silica gel for 4 h.

Acceptance criteria: NMT 0.3%

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in well-closed, light-resistant containers. Store at 25°, excursions permitted between 15° and 30°.

USP Reference Standards 〈11〉

USP Menadione RS