Triprolidine 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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C₁₉H₂₂N₂ · HCI · H₂O            332.87

C₁₀H₁₅NO· HCI               314.86

Pyridine, 2-[1-(4-methylphenyl)-3-(1-pyrrolidinyl)-1-propenyl]-, monohydrochloride, monohydrate, (E)-;

(E)-2-[3-(1-Pyrrolidinyl)-1-p-tolylpropenyl]pyridine monohydrochloride monohydrate   CAS RN^®: 6138-79-0; UNII: YAN7R5L890.

Anhydrous CAS RN^®:: 550-70-9; UNII: NG7A104R3J.

1 DEFINITION

Triprolidine Hydrochloride contains NLT 98.0% and NMT 102.0% of triprolidine hydrochloride (C₁₀H₁₅NO· HCI), calculated on the anhydrous basis.

2 IDENTIFICATION

Change to read:

A. ^▲Spectroscopic Identification Tests (197), Infrared Spectroscopy: 197K_{▲(CN 1-May-2020)}

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

C. IDENTIFICATION TESTS GENERAL, Chloride (191)

3 ASSAY

PROCEDURE

Mobile phase: Acetonitrile, formic acid, and water (200:1:800) prepared as follows. Mix 200 mL of acetonitrile with 800 mL of water, add 1 mL of formic acid, and sonicate.

Diluent: Acetonitrile and water (20:80)

System suitability solution: 0.01 mg/ml. each of USP Triprolidine Hydrochloride RS and USP Triprolidine Hydrochloride Z-Isomer RS in Diluent

Standard solution: 0.1 mg/mL of USP Triprolidine Hydrochloride RS in Diluent prepared as follows. Transfer a suitable amount of USP Triprolidine Hydrochloride RS to a suitable volumetric flask and dissolve, by sonication, in about 60% of the flask volume of Diluent. Dilute with Diluent to volume.

Sample solution: 0.1 mg/mL of Triprolidine Hydrochloride in Diluent prepared as follows. Transfer a suitable amount of Triprolidine Hydrochloride to a suitable volumetric flask and dissolve, by sonication, in about 60% of the flask volume of Diluent. Dilute with Diluent to volume.

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 254 nm

Column: 4.6-mm x 25.0-cm; 5-µm packing L1

Column temperature: 45°

Flow rate: 1 mL/min

Injection volume: 20 μL

Run time: 20 min

System suitability

Samples: System suitability solution and Standard solution

[NOTE-See Table 1 for the relative retention times.]

Suitability requirements

Resolution: NLT 5.0 between triprolidine hydrochloride and triprolidine hydrochloride Z-isomer, Systern suitability solution

Tailing factor: NMT 2.0, Standard solution

Relative standard deviation: NMT 1.0%, Standard solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of triprolidine hydrochloride (C₁₀H₁₅NO· HCI) in the portion of Triprolidine Hydrochloride 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 s

C_S = concentration of USP Triprolidine Hydrochloride RS in the Standard solution (mg/mL)

C_U = concentration of Triprolidine Hydrochloride in the Sample solution (mg/mL)

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

4 IMPURITIES

4.1 RESIDUE ON IGNITION (281)

NMT 0.1%

4.2 ORGANIC IMPURITIES

Mobile phase, Diluent, and Chromatographic system: Proceed as directed in the Assay.

Standard solution: 10 µg/mL each of USP Triprolidine Hydrochloride RS and USP Triprolidine Hydrochloride Z-Isomer RS in Diluent

Sample solution: 0.5 mg/mL of Triprolidine Hydrochloride in Diluent prepared as follows. Transfer a suitable amount of Triprolidine Hydrochloride to a suitable volumetric flask and dissolve, by sonication, in about 60% of the flask volume of Diluent. Dilute with Diluent to volume.

System suitability

Sample: Standard solution

[NOTE-See Table 1 for the relative retention times.]

Suitability requirements

Resolution: NLT 5.0 between triprolidine hydrochloride and triprolidine hydrochloride Z-isomer

Relative standard deviation: NMT 1.8% for each peak

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of triprolidine hydrochloride Z-isomer in the portion of Triprolidine Hydrochloride taken:

                         Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak response of triprolidine hydrochloride Z-isomer from the Sample solution

r_S = peak response of triprolidine hydrochloride Z-isomer from the Standard solution

C_S = concentration of USP Triprolidine Hydrochloride Z-Isomer RS in the Standard solution (mg/mL)

C_U = concentration of Triprolidine Hydrochloride in the Sample solution (mg/mL)

Calculate the percentage of any individual unspecified impurity in the portion of Triprolidine Hydrochloride taken:

                         Result = (r_U/r_S) × (C_S/C_U) × 100

r_U = peak response of any unspecified impurity from the Sample solution 

r_S = peak response of triprolidine hydrochloride from the Standard solution

C_S = concentration of USP Triprolidine Hydrochloride RS in the Standard solution (mg/mL)

C_U = concentration of Triprolidine Hydrochloride in the Sample solution (mg/mL) 

Acceptance criteria: See Table 1.

Table 1

5 SPECIFIC TESTS

WATER DETERMINATION, Method / (921); 4.0%-6.0%

6 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Preserve in tight, light-resistant containers.

USP REFERENCE STANDARDS (11)

USP Triprolidine Hydrochloride RS

USP Triprolidine Hydrochloride Z-Isomer RS

(Z)-2-[3-(1-Pyrrolidinyl)-1-p-tolylpropenyl]pyridine monohydrochloride.

C₁₉H₂₂N₂ · HCI                314.85