Cholecalciferol Tablets

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

DOWNLOAD PDF HERE

1 DEFINITION

Cholecalciferol Tablets contain NLT 90.0% and NMT 115.0% of the labeled amount of cholecalciferol (C₂₇H₄₄O).

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 spectrum 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

[NOTE—Use amber, low-actinic glassware.]

Diluent: Water, dimethylformamide, and isopropyl alcohol (5:10:35, v/v) Mobile phase: Acetonitrile and water (70:30)

Standard stock solution: 0.5 mg/mL of USP Cholecalciferol RS in isopropyl alcohol

Ergocalciferol stock solution: 0.5 mg/mL of USP Ergocalciferol RS in isopropyl alcohol

System suitability solution: Combine equal volumes of Standard stock solution and Ergocalciferol stock solution and dilute with Diluent to obtain a concentration of about 1 µg/mL each of cholecalciferol and ergocalciferol.

Standard solution: 1 µg/mL of USP Cholecalciferol RS in Diluent from the Standard stock solution, prepared accurately

Sample solution: Finely powder NLT 20 Tablets. Transfer a portion of the powder, nominally equivalent to 50 µg of cholecalciferol, into a 50- mL volumetric flask, add 5 mL of water and sonicate for 10 min with intermittent shaking. Add 10 mL of dimethylformamide, sonicate for 15 min with intermittent shaking, cool to room temperature, and dilute with isopropyl alcohol to volume. Mix well and pass through a 0.45- µm nylon filter.

3.1.1 Chromatographic system

(See Chromatography 〈621〉, System Suitability.) Mode: LC

Detector: UV 265 nm

Column: 4.6-mm × 15-cm; 2.7-µm packing L96 Column temperature: 40°

Flow rate: 1 mL/min Injection volume: 20 µL

3.1.2 System suitability

Samples: System suitability solution and Standard solution

[NOTE—The relative retention times for cholecalciferol and ergocalciferol are 1.0 and 1.1, respectively.]

Suitability requirements

Resolution: NLT 1.5 between the cholecalciferol and ergocalciferol peaks, System suitability solution Relative standard deviation: NMT 2.0%, Standard solution

3.1.3 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of cholecalciferol (C₂₇H₄₄O) in the portion of Tablets taken:

Result = (r_u/r_s) × (C_s/C_u) × 100

r_u = peak area of cholecalciferol from the Sample solution

r_s = peak area of cholecalciferol from the Standard solution

C_s = concentration of cholecalciferol in the Standard solution (µg/mL)

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

Acceptance criteria: 90.0%–115.0%

4 PERFORMANCE TESTS

4.1 DISSOLUTION 〈711〉

[NOTE—Perform this test under light conditions that minimize photodegradation.] Medium: 0.1% (w/v) octoxynol-9 in water; 500 mL

Apparatus 2: 75 rpm

Time: 30 min

Mobile phase: Acetonitrile and water (70:30)

Standard stock solution: 0.5 mg/mL of USP Cholecalciferol RS in isopropyl alcohol

Standard solution: Dilute Standard stock solution with Medium to obtain the concentration equivalent to that expected in the Sample solution.

Sample solution: Withdraw a portion of the solution under test, pass through a 0.45-µm PVDF filter, and use the pooled sample as the test specimen.

4.1.1 Chromatographic system

(See Chromatography 〈621〉, System Suitability.) Mode: LC

Detector: UV 265 nm

Column: 4.6-mm × 15-cm; 2.7-µm packing L96 Column temperature: 40°

Flow rate: 1 mL/min Injection volume: 100 µL

4.1.2 System suitability

Sample: Standard solution

Suitability requirements

Relative standard deviation: NMT 2.0% Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of cholecalciferol dissolved:

Result = (r_u/r_s) × (C_s × V/L) × 100

r_u = peak area of cholecalciferol from the Sample solution

r_s = peak area of cholecalciferol from the Standard solution

C_s = concentration of cholecalciferol in the Standard solution (µg/mL)

V = volume of Medium, 500 mL

L = label claim of cholecalciferol (µg/Tablet)

Tolerances: NLT 75% (Q ) of the labeled amount of cholecalciferol is dissolved.

4.2 UNIFORMITY OF DOSAGE UNITS 〈905〉

Meet the requirements

5 ADDITIONAL REQUIREMENTS

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

LABELING: Label the Tablets to indicate the content of cholecalciferol in µg.

USP REFERENCE STANDARDS 〈11〉

USP Cholecalciferol RS USP Ergocalciferol RS