Desloratadine Tablets

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

Desloratadine Tablets contain NLT 93.0% and NMT 105.0% of the labeled amount of desloratadine (C₁₉H₁₉ClN₂).

2 IDENTIFICATION

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

B. The UV absorption spectra of the desloratadine peak of the Sample solution exhibit maxima and minima at the same wavelengths as those of the corresponding peak of the Standard solution, as obtained in the Assay.

3 ASSAY

3.1 Procedure

Use amber, low-actinic glassware.

Buffer: Dissolve 4.35 g of dibasic potassium phosphate in 1 L of water. Adjust with phosphoric acid to a pH of 3.0.

Mobile phase: Methanol and Buffer (20:80)

Diluent: Methanol and water (90:10)

Standard solution: 0.02 mg/mL of USP Desloratadine RS in Diluent

Sample stock solution: Nominally 0.2 mg/mL of desloratadine, prepared as follows. Transfer NLT 20 Tablets into a suitable volumetric flask, add water to fill 10% of the flask volume, and allow the Tablets to disperse. Add methanol, about 50% of the flask volume, and stir for NLT 60 min. Allow the solution to cool to room temperature and dilute with methanol to volume. Centrifuge a portion of this solution and use the supernatant.

Sample solution: Nominally 0.02 mg/mL of desloratadine in Diluent, from Sample stock solution

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detectors
• • Assay: UV 241 nm
• • Identification B: Diode array; UV 230–400 nm
• Column: 4.6-mm × 15-cm; 5-µm packing L10
• Column temperature: 30°
• Flow rate: 1 mL/min
• Injection volume: 20 µL
• Run time: NLT 4.2 times the retention time of desloratadine

System suitability

• Sample: Standard solution
• Suitability requirements
• Tailing factor: NMT 2.0
• Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of desloratadine (C₁₉H₁₉ClN₂) in the portion of Tablets 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 Desloratadine RS in the Standard solution (mg/mL)

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

Acceptance criteria: 93.0%–105.0%

4 PERFORMANCE TESTS

4.1 Dissolution 〈711〉

Medium: 0.1 N hydrochloric acid; 500 mL

Apparatus 2: 50 rpm

Time: 45 min

Standard solution: 0.01 mg/mL of USP Desloratadine RS in Medium

Sample solution: Pass a portion of the solution under test through a suitable filter of 0.45-µm pore size. Discard the first 5 mL of the filtrate.

Instrumental conditions

• Mode: UV
• Analytical wavelength: 282 nm
• Cell: 1.0 cm

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of desloratadine (C₁₉H₁₉ClN₂) dissolved:

Result = (A_U/A_S) × C_S × V × (1/L) × 100

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

V = volume of Medium, 500 mL

L = label claim (mg/Tablet)

Tolerances: NLT 80% (Q) of the labeled amount of desloratadine (C₁₉H₁₉ClN₂) is dissolved.

4.2 Uniformity of Dosage Units 〈905〉: Meet the requirements

5 IMPURITIES

Change to read:

5.1 Organic Impurities

Protect all solutions containing desloratadine from light.

Solution A: Dissolve 4.35 g of dibasic potassium phosphate in 1 L of water. Adjust with phosphoric acid to a pH of 3.2.

Solution B: Acetonitrile

Solution C: Methanol

Mobile phase: See Table 1.

Diluent: Methanol and water (90:10)

Standard solution: 0.002 mg/mL each of USP Desloratadine RS and USP Desloratadine Related Compound F RS in Diluent

Sensitivity solution: 0.1 µg/mL of USP Desloratadine RS in Diluent

Sample solution: Nominally 0.2 mg/mL of desloratadine, prepared as follows. Transfer NLT 20 Tablets into a suitable volumetric flask, add 10% of the flask volume of water, and allow the Tablets to disperse. Add methanol, about 50% of the flask volume, and stir for at least 60 min. Allow the solution to cool to room temperature, and dilute with methanol to volume. Centrifuge a portion and use the supernatant.

Chromatographic system

• (See Chromatography (621), System Suitability.)
• Mode: LC
• Mode: LC
• Detector: UV 241 nm
• Column: 4.6-mm × 15-cm; 3-µm packing L7
• Column temperature: 35°
• Flow rate: 1 mL/min
• Injection volume: 20 µL

System suitability

• Samples: Standard solution and Sensitivity solution
• Suitability requirements
• Column efficiency: NLT 1500 theoretical plates for desloratadine, Standard solution
• Relative standard deviation: NMT 5.0% for desloratadine, Standard solution
• Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Standard solution, Sensitivity solution, and Sample solution

Calculate the percentage of desloratadine related compound F in the portion of Tablets taken:

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak response of desloratadine related compound F from Sample solution

r_s = peak response from Standard solution

C_s = concentration of USP Desloratadine Related Compound F RS in Standard solution (mg/mL)

C_u = nominal concentration of desloratadine in Sample solution (mg/mL)

Calculate the percentage of any unspecifed degradation product in the portion of Tablets taken:

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak response of each unspecified impurity from the Sample solution

r_s = peak response of desloratadine from the Standard solution

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

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

Acceptance criteria: See Table 2. Disregard peaks less than 0.05%.

a 6,11-Dihydro-11-(piperidin-4-ylidene)-5H-benzo[5,6]cyclohepta[1,2-b]pyridine.

b Process impurity controlled in the drug substance monograph. Provided for information only; the content is not calculated and not

reported.

c 8-Chloro-11-(piperidin-4-ylidene)benzo[5,6]cyclohepta[1,2-b]pyridine.

d 8-Chloro-6,11-dihydro-11-(1-ethoxycarbonylpiperidin-4-ylidene)-5H-benzo[5,6]cyclohepta[1,2-b]pyridine (Loratadine).

6 ADDITIONAL REQUIREMENTS

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

USP Reference Standards 〈11〉

USP Desloratadine RS

USP Desloratadine Related Compound F RS

8-Chloro-6,11-dihydro-11-(N-formyl-4-piperidinylidene)-5H-benzo[5,6]cyclohepta[1,2-b]pyridine.

C₂₀H₁₉ClN₂O 338.83