Amiloxate

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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C₁₅ H₂₀O₃ 248.32

4-Methoxycinnamic acid, isoamyl ester;

3-Methylbutyl 3-(4-methoxyphenyl)-(E)-2-propenoate CAS RN®: 71617-10-2; UNII: 376KTP06K8.

1 DEFINITION

Amiloxate contains NLT 98.0% and NMT 102.0% of amiloxate (C₁₅ H₂₀O₃).

2 IDENTIFICATION

Change to read:

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

Change to read:

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

Sample solution: 5.0 μg/mL in alcohol

C. 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

Standard solution: 20 mg/mL of USP Amiloxate RS in tert-butyl methyl ether

Sample solution: 20 mg/mL of Amiloxate in tert-butyl methyl ether

3.2 Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: GC

Detector: Flame ionization

Column: 0.32-mm × 25-m; coated with a 0.1-μm film of phase G1

Temperatures

Injection port: 240°

Detector: 260°

Column: See Table 1.

Table 1

Carrier gas: Helium

Flow rate: 6 mL/min

Injection volume: 1 μL

3.3 System suitability

Sample: Standard solution

3.4 Suitability requirements

Relative standard deviation: NMT 0.73%

3.5 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of amiloxate (C₁₅ H₂₀O₃) in the portion of Amiloxate 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 Amiloxate RS in the Standard solution (mg/mL)

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

Acceptance criteria: 98.0%–102.0%

4 IMPURITIES

4.1 Organic Impurities

Standard solution, Sample solution, Chromatographic system, and System suitability: Proceed as directed in the Assay.

4.2 Analysis

Sample: Sample solution

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

Result = (r_u/r_T) × 100

r_u = peak response of each impurity from the Sample solution

r_T = sum of all the peak responses, excluding the solvent peak, from the Sample solution

4.3 Acceptance criteria

Individual impurities: NMT 0.5%

Total impurities: NMT 2.0%

5 SPECIFIC TESTS

Specific Gravity 〈841〉: 1.037–1.041

Refractive Index 〈831〉: 1.556–1.560 at 20°

Acidity

Sample solution: Transfer 50 mL of alcohol to a suitable container. Add 1 mL of phenolphthalein TS and suficient 0.1 N sodium hydroxide to obtain a persistent pink color. Transfer 50 mL of this solution to a suitable container, and add 5.0 mL of Amiloxate.

Analysis: Titrate with 0.1 N sodium hydroxide VS.

Acceptance criteria: NMT 0.2 mL of titrant per mL of Amiloxate is required for neutralization.

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers.

USP Reference Standards 〈11〉

USP Amiloxate RS