Altretamine

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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C₉H₁₈N₆   210.28

1,3,5-Triazine-2,4,6-triamine, N,N,N′,N′,N′′,N′′-hexamethyl-;

Hexamethylmelamine CAS RN®: 645-05-6.

1 DEFINITION

Altretamine contains NLT 98.0% and NMT 102.0% of altretamine (C₉H₁₈N₆), calculated on the anhydrous basis.

2 IDENTIFICATION

Change to read:

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

B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

3.1 Procedure

Solution A: 1.7 g/L of dibasic potassium phosphate in water. Adjust with phosphoric acid to a pH of 7.0 ± 0.1.

Solution B: Acetonitrile

Mobile phase: See Table 1.

Table 1

Standard stock solution: 1.0 mg/mL of USP Altretamine RS prepared as follows. Dissolve a suitable amount of USP Altretamine RS in about 40% of the flask volume of acetonitrile. Sonicate as needed to dissolve. Add water almost to volume and allow the solution to reach room temperature. Dilute with water to volume and mix.

Standard solution: 0.1 mg/mL of USP Altretamine RS in water from Standard stock solution

Sample stock solution: 1.0 mg/mL of Altretamine prepared as follows. Dissolve a suitable amount of Altretamine in about 40% of the flask volume of acetonitrile. Sonicate as needed to dissolve. Add water almost to volume and allow the solution to reach room temperature.

Dilute with water to volume and mix.

Sample solution: 0.1 mg/mL of Altretamine in water from Sample stock solution

3.2 Chromatographic system

Mode: LC

Detector: UV 242 nm

Column: 4.6-mm × 25-cm; 5-μm packing L96

Flow rate: 1.5 mL/min

Injection volume: 20 μL. [Note - An in-line filter may be needed to reduce system pressure.]

3.3 System suitability

Sample: Standard solution

3.4 Suitability requirements

Tailing factor: NMT 1.5

Relative standard deviation: NMT 2.0%

3.5 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of altretamine (C₉H₁₈N₆) in the portion of Altretamine taken:

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak response from the Sample solution

r_s = peak response from the Standard solution

C_s = concentration of USP Altretamine RS in the Standard solution (mg/mL)

C_u = concentration of Altretamine in the Sample solution (mg/mL)

Acceptance criteria: 98.0%-102.0% on the anhydrous basis

4 IMPURITIES

Residue on Ignition 〈281〉: NMT 0.1%

Organic Impurities

Solution A, Solution B, Mobile phase, Standard solution, and Sample solution: Prepare as directed in the Assay.

Sensitivity solution: 0.06 μg/mL of USP Altretamine RS in water from Standard solution

Chromatographic system

Mode: LC

Detector: UV 215 and 242 nm (see Table 2)

Column: 4.6-mm × 25-cm; 5-μm packing L96

Flow rate: 1.5 mL/min

Injection volume: 20 μL

System suitability

Samples: Standard solution and Sensitivity solution

Suitability requirements

Tailing factor: NMT 1.5, Standard solution

Relative standard deviation: NMT 2.0%, Standard solution

Signal-to-noise ratio: NLT 10 for the altretamine peak, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of each impurity in the portion of Altretamine taken:

Result = (r_u/r_s) × (C_s/C_u) × (1/F) × 100

r_u = peak response of each impurity from the Sample solution

r_s = peak response of altretamine from the Standard solution

C_s = concentration of USP Altretamine RS in the Standard solution (mg/mL)

C_u = concentration of Altretamine in the Sample solution (mg/mL)

F = relative response factor (see Table 2)

Acceptance criteria: See Table 2. The reporting threshold is NMT 0.06%.

Table 2

^a 6-(Dimethylamino)-1,3,5-triazine-2,4[1H,3H]-dione.

^b 4-Chloro-6-(dimethylamino)-1,3,5-triazine-2[1H]-one.

^c 4,6-Bis(dimethylamino)-1,3,5-triazine-2[1H]-one.

^d 4,6-Dichloro-N,N-dimethyl-1,3,5-triazine-2-amine.

^e 6-Chloro-,N²,N²,N⁴,N^{4 -} tetramethyl-1,3,5-triazine-2,4-diamine.

^f Use the detector consistent with respective impurity.

5 SPECIFIC TESTS

Water Determination 〈921〉, Method I: NMT 1%

Tests for Specified Microorganisms 〈62〉: The total aerobic microbial count is NMT 103 cfu/g. The total combined molds and yeasts count is NMT 102cfu/g.

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers, and store at controlled room temperature.

USP Reference Standards 〈11〉

USP Altretamine RS