Selegiline Hydrochloride

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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» Selegiline Hydrochloride contains not less than 98.0 percent and not more than 101.0 percent of C₁₃H₁₇N · HCl, calculated on the dried basis.

Packaging and storage— Preserve in tight, light-resistant containers.

USP Reference standards 〈11〉—

USP Selegiline Hydrochloride RS

USP Methamphetamine Hydrochloride RS

1 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)

Solution: 0.5 mg per mL.

Medium: water.

C: The retention time of the major peak in the chromatogram of the Assay preparation corresponds to that of the Standard preparation obtained as directed in the Assay.

D: It responds to the tests for Chloride 〈191〉.

Melting range 〈741〉:

Not greater than 2°, within the limits of 141° and 145°.

Specific rotation 〈781S〉:

Between −10.0° and −12.0°.

Test solution: 100 mg per mL, in water.

Loss on drying 〈731〉—

Dry it in vacuum at 60° for 3 hours: it loses not more than 1.0% of its weight.

Residue on ignition 〈281〉:

Not more than 0.2%.

Chromatographic purity—

Buffer solution, Mobile phase, and System suitability solution— Proceed as directed in the Assay.

Standard solution—

Transfer 10.0 mL of the System suitability solution to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.

Transfer 10.0 mL of this solution to a 50-mL volumetric flask, dilute with Mobile phase to volume, and mix.

Test solution—

Transfer 50 mg of Selegiline Hydrochloride to a 50-mL volumetric flask, dissolve in and dilute with Mobile phase to volume, and mix.

Chromatographic system—

Proceed as directed in the Assay. Inject about 20 µL of the Standard solution, and record the peak responses as directed in the Procedure:

The resolution, R, between the methamphetamine and selegiline peaks is not less than 3, and the relative standard deviation for replicate injections is not more than 5.0%.

Procedure—

Separately inject equal volumes (about 20 µL) of the Standard solution and the Test solution into the chromatograph, and allow the Test solution to elute for not less than three times the retention time of selegiline.

Record the chromatograms, and measure the peak responses.

Calculate the percentage of each impurity in the portion of Selegiline Hydrochloride taken by the formula:

5000(C/W)(rᵢ/rₛ)

C = concentration (mg/mL) of USP Selegiline Hydrochloride RS in the Standard solution

W = weight (mg) of Selegiline Hydrochloride taken to prepare the Test solution

rᵢ = peak response for each impurity in the Test solution

rₛ = peak response for selegiline in the Standard solution

Acceptance criteria:

Not more than 0.2% of any individual impurity;

Sum of all impurities NMT 1.0%.

2 Assay—

Buffer solution—

Prepare a solution of 0.1 M monobasic ammonium phosphate, adjust with phosphoric acid to a pH of 3.1, and mix.

Mobile phase—

Filter and degas a mixture of Buffer solution and acetonitrile (80:20).

Make adjustments if necessary (see System Suitability under Chromatography 〈621〉).

Standard preparation—

Dissolve an accurately weighed quantity of USP Selegiline Hydrochloride RS, dilute quantitatively (stepwise if necessary) with Mobile phase to obtain a solution of about 0.1 mg/mL.

System suitability solution—

Dissolve accurately weighed USP Methamphetamine Hydrochloride RS and USP Selegiline Hydrochloride RS in Mobile phase to obtain 0.1 mg/mL of each.

Assay preparation—

Transfer an accurately weighed portion, about 50 mg of Selegiline Hydrochloride, to a 50-mL volumetric flask, dissolve in Mobile phase to volume, and mix.

Transfer 10.0 mL of this solution to a 100-mL volumetric flask, dilute with Mobile phase to volume, and mix.

Chromatographic system

(See Chromatography 〈621〉)

Detector: UV 205 nm

Column: 3.9-mm × 30-cm, packing L1

Flow rate: 1 mL/min

Chromatograph the System suitability solution and record peak responses:

Resolution between methamphetamine and selegiline ≥ 3

Relative standard deviation for replicate injections ≤ 2.0%

Procedure—

Inject equal volumes (about 20 µL) of the Standard preparation and the Assay preparation into the chromatograph.

Record the chromatograms, measure major peaks.

Calculate the amount, in mg, of C₁₃H₁₇N · HCl in the portion taken:

500C(rᵤ/rₛ)

C = concentration (mg/mL) of USP Selegiline Hydrochloride RS in the Standard preparation

rᵤ = selegiline peak response from the Assay preparation

rₛ = selegiline peak response from the Standard preparation