Ursodiol Compounded Oral Suspension

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

Ursodiol Compounded Oral Suspension contains NLT 90.0% and NMT 110.0% of the labeled amount of ursodiol (C₂₄H₄₀O₄)

Prepare Ursodiol Compounded Oral Suspension 50 mg/mL in Ora-Sweet SF and Ora-Plus _{(USP 1-Dec-2021)} as follows (see Pharmaceutical Compounding-Nonsterile Preparations (795)).

^a Urso 250-mg tablets, Axcan Pharma U.S. Inc., Birmingham, AL.

^b Paddock Laboratories, Minneapolis, MN.

Calculate the required quantity of each ingredient for the total amount to be prepared. Place the required number of Ursodiol tablets in a suitable mortar, and comminute to a fine powder. Add the Vehicle in small portions, and triturate to make a smooth paste. Add increasing volumes of the Vehicle to make a ursodiol liquid that is pourable. Transfer the contents of the mortar, stepwise and quantitatively, to a calibrated bottle. Add enough of the Vehicle to bring to final volume, and mix well.

Prepare Ursodiol Compounded Oral Suspension 50 mg/mL in Suspendit as follows (see Pharmaceutical Compounding-Nonsterile Preparations (795)).

^a PCCA, Houston, TX.

Place the Ursodiol powder, Acesulfame potassium, and Steviol glycosides 95% in a suitable container and triturate to a ne powder. Add a small amount of SuspendIt and mix well to form a smooth paste. Add a sucient amount of SuspendIt to make a liquid that is pourable. Transfer contents stepwise and quantitatively to a calibrated container using the remainder of the SuspendIt. Add a sucient amount of SuspendIt to bring to nal volume, and mix well.

Prepare Ursodiol Compounded Oral Suspension 100 mg/mL in SuspendIt as follows (see Pharmaceutical Compounding—Nonsterile Preparations 〈795〉).

^a PCCA, Houston, TX.

Place the Ursodiol powder, Acesulfame potassium, and Steviol glycosides 95% in a suitable container and triturate to a ne powder. Add a small amount of SuspendIt and mix well to form a smooth paste. Add a sucient amount of SuspendIt to make a liquid that is pourable. Transfer contents stepwise and quantitatively to a calibrated container using the remainder of the SuspendIt. Add a sucient amount of SuspendIt to bring to nal volume, and mix well. _{(USP 1-Dec-2021)}

2 ASSAY

Change to read:

Procedure 1: Oral Suspension in Ora-Sweet SF and Ora-Plus _{(USP 1-Dec-2021)}

Mobile phase: Methanol and 0.01 M dihydrogen potassium phosphate buffer (75:25). Adjust with dilute phosphoric acid to a pH of 5.25. Filter and degas.

Standard solution: 1.25 mg/mL of USP Ursodiol RS in methanol

Sample solution: Shake thoroughly by hand each bottle of Oral Suspension. Prepare 1.25 mg/mL of ursodiol from Oral Suspension and methanol, and centrifuge.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 201 nm

Column: 4.6-mm × 25-cm; 5-µm packing L1

Column temperature: 40°

Flow rate: 1.2 mL/min

Injection volume: 15 µL

System suitability

Sample: Standard solution

[Note—The retention time for ursodiol is about 7 min.]

Suitability requirements

Relative standard deviation: NMT 2.0% for replicate injections

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of ursodiol (C₂₄H₄₀O₄) in the portion of Oral Suspension 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 Ursodiol RS in the Standard solution (mg/mL)

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

Acceptance criteria: 90.0%–110.0%

Add the following:

PROCEDURE 2: ORAL SUSPENSION IN SUSPENDIT

Mobile phase: Methanol and 1 mg/mL of acetic acid (58:42)

Standard stock solution: 10 mg/mL of USP Ursodiol RS in methanol

Standard solution: Transfer 1 mL of the Standard stock solution into a 10-ml volumetric flask, and dilute with Mobile phase to volume to

create a 1-mg/mL solution of ursodiol.

Sample solution: Prepare the appropriate solution as follows.

For 50 mg/mL: Shake the bottle of Oral Suspension thoroughly. Transfer 0.1 mL of Oral Suspension into a 5-ml volumetric flask, dissolve with 1 mL of methanol, dilute with Mobile phase to volume, and mix well. Transfer into HPLC vials, taking care not to transfer any globular-gelled Suspendit.

For 100 mg/mL: Shake the bottle of Oral Suspension thoroughly. Transfer 0.1 mL of Oral Suspension into a 10-mL volumetric flask, dissolve with 1 mL of methanol, dilute with Mobile phase to volume, and mix well. Transfer into HPLC vials, taking care not to transfer any globular- gelled SuspendIt.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: Refractive index

Column: 2.1-mm × 10-cm; 5-µm packing L1

Flow rate: 0.8 mL/min

Injection volume: 30 µL

System suitability

Sample: Standard solution

[Note—The retention time for ursodiol is about 6.1 min.]

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0% for replicate injections

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of ursodiol (C₂₄H₄₀O₄) in the portion of Oral Suspension taken:

Result = (r_u /r_s ) × (C_s /C_u ) × 100

r_u = peak response of ursodiol from the Sample solution

r_s = peak response of ursodiol from the Standard solution

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

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

Acceptance criteria: 90.0%–110.0% _{(USP 1-Dec-2021)}

3 SPECIFIC TESTS

Change to read:

PH (791)

Oral Suspension in Ora-Sweet SF and Ora-Plus: 4.0-5.0

Oral Suspension in Suspendit: 4.5-5.5 _{(USP 1-Dec-2021)}

4 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Package in tight, light-resistant containers. Store in a refrigerator or at controlled room temperature.

Change to read:

BEYOND-USE DATE

Oral Suspension in Ora-Sweet SF and Ora-Plus: NMT 90 days after the date on which it was compounded when stored at controlled room temperature or in a refrigerator

Oral Suspension in Suspendit: NMT 90 days after the date on which it was compounded when stored in a refrigerator or at controlled room temperature _{(USP 1-Dec-2021)}

LABELING: Label it to indicate that it is to be well shaken before use and to state the Beyond-Use Date.

USP REFERENCE STANDARDS (11)

USP Ursodiol RS