Desloratadine Orally Disintegrating 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 Orally Disintegrating Tablets contain NLT 95.0% and NMT 105.0% of the labeled amount of desloratadine (C₁₉H₁₉ClN₂).

2 IDENTIFICATION

Change to read:

A. Spectroscopic Identification Tests 〈197〉, Ultraviolet-Visible Spectroscopy: 197U

Standard solution and Sample solution: Proceed as directed in the Assay.

Instrumental conditions

• Mode: UV
• Wavelength range: 230–330 nm
• [Note-Alternatively, a diode array detector may be used in the Assay to obtain the spectra.]

Acceptance criteria: The UV spectrum of the Sample solution corresponds to that of the Standard solution.

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

Buffer: 6.8 g/L of monobasic potassium phosphate. Adjust with phosphoric acid to a pH of 3.0.

Mobile phase: Acetonitrile, methanol, and Buffer (28:7:65)

Diluent: Methanol and 0.1 N hydrochloric acid (40:60)

Standard solution: 0.05 mg/mL of USP Desloratadine RS in Diluent. Sonication may be used to aid dissolution.

Sample stock solution: Nominally 0.25 mg/mL of desloratadine, prepared as follows. Transfer 10 Tablets to a suitable volumetric flask, add water to 15% of the flask volume, and shake until the Tablets disintegrate completely. Add 75% of the flask volume of Diluent and sonicate for 30 min with intermittent shaking, and dilute with Diluent to volume. Centrifuge a portion of this solution. Use the supernatant.

Sample solution: Nominally 0.05 mg/mL of desloratadine from the Sample stock solution in Diluent; centrifugate.

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detector: UV 258 nm
• Column: 4.6-mm × 25-cm; 5-µm packing L1
• Flow rate: 1 mL/min
• Injection volume: 20 µL

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: 95.0%–105.0%

4 PERFORMANCE TESTS

4.1 Disintegration 〈701〉: NMT 30 s

4.2 Dissolution 〈711〉

Medium: 0.1 N hydrochloric acid (degassed); 900 mL

Apparatus 2: 50 rpm

Time: 10 min

Buffer: 6.8 g/L of monobasic potassium phosphate

Solution A: Acetonitrile and methanol (80:20)

Mobile phase: Solution A and Buffer (40:60)

Standard stock solution: 0.28 mg/mL of USP Desloratadine RS in methanol. Sonication may be used to aid dissolution.

Standard solution: (L/900) mg/mL of USP Desloratadine RS from the Standard stock solution in Medium, where L is the label claim (mg/Tablet)

Sample solution: Pass a portion of the solution under test through a suitable filter.

Chromatographic system

• (See Chromatography 〈621〉, System Suitability.)
• Mode: LC
• Detector: UV 258 nm
• Column: 4.6-mm × 25-cm; 5-µm packing L1
• Flow rate: 1 mL/min
• Injection volume: 40 µL

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) dissolved:

Result = (r_u/r_s) × C_s × V × (1/L) × 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)

V = volume of Medium, 900 mL

L = label claim (mg/Tablet)

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

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

5 IMPURITIES

Change to read:

5.1 Organic Impurities

Buffer: Add 10 mL/L of triethylamine to a 1.36 g/L solution of monobasic potassium phosphate. Adjust with phosphoric acid to a pH of 2.5.

Solution A: Methanol, acetonitrile, and Buffer (15:5:80)

Solution B: Acetonitrile, tetrahydrofuran, and Buffer (70:5:30)

Solution C: Dilute 8.5 mL of hydrochloric acid with methanol to 1 L.

Mobile phase: See Table 1.

Diluent: Solution C and Buffer (30:70)

System suitability stock solution: 0.05 mg/mL each of USP Desloratadine Related Compound A RS and USP Desloratadine Related Compound F RS in methanol.

System suitability solution: 0.5 mg/mL of USP Desloratadine RS, 1.0 µg/mL each of USP Desloratadine Related Compound A RS and USP Desloratadine Related Compound FRS, prepared as follows. Transfer 50 mg of USP Desloratadine RS into a 100-mL volumetric flask, add 70 mL of Diluent, and sonicate to dissolve. Add 2 mL of the System suitability stock solution and dilute with Diluent to volume.

Standard solution: 0.0025 mg/mL of USP Desloratadine RS and 0.001 mg/ml. of USP Desloratadine Related Compound F RS in Diluent

Sample solution: Nominally 0.5 mg/mL of desloratadine from NLT 40 Tablets, prepared as follows. Transfer an amount of powder to a suitable volumetric flask to obtain the nominal concentration of desloratadine. Add 70% of the flask volume of Diluent and sonicate for 20 min with intermittent shaking. Dilute with Diluent to volume. Centrifuge a portion of the solution and use the supernatant.

Chromatographic system

• (See Chromatography (621), System Suitability.)
• Mode: LC
• Detector: UV 280 nm
• Column: 4.6-mm x 25-cm; 5-µm packing LZ
• Column temperature: 30*
• Flow rate: 1 mL/min
• Injection volume: 40 µL

System suitability

• Samples: System suitability solution and Standard solution
• [NOTE-Relative retention times are given in Table 2.
• Suitability requirements
• Resolution: NLT 2.0 between desloratadine and desloratadine related compound A, System suitability solution
• Tailing factor: NMT 2.0 for desloratadine and desloratadine related compound F, Standard solution
• Relative standard deviation: NMT 10.0% desloratadine related compound F, Standard solution
• Signal-to-noise ratio: NLT 10 for desloratadine peak, Standard solution

Analysis

Samples: Standard solution and Sample solution

Identify the impurities using the relative retention times given in Table 2.

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 the Sample solution

r_s = peak response of desloratadine related compound F from the Standard solution

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

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

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

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak response of any unspecified degradation product 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 (µg/mL)

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

Acceptance criteria: See Table 2.

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

b This is a process impurity… (controlled in drug substance, not reported for drug product).

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.

6 ADDITIONAL REQUIREMENTS

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

USP Reference Standards 〈11〉

USP Desloratadine RS

USP Desloratadine Related Compound A RS

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

C₁₉H₁₉BrN₂   355.27

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