Clopidogrel 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

Clopidogrel Compounded Oral Suspension contains NLT 90.0% and NMT 110.0% of the labeled amount of clopidogrel (C₁₆H₁₆CINO₂S).

Prepare Clopidogrel Compounded Oral Suspension 5 mg/mL as follows (see Pharmaceutical Compounding-Nonsterile Preparations (795)).

^a Clopidogrel 75-mg tablets, Dr. Reddy's Laboratory Limited, Bridgewater, NJ.

^b Perrigo Pharmaceuticals, Allegan, MI.

Crush the Clopidogrel tablet(s) to a fine powder using a mortar and pestle or by other mechanical means. Wet the powder with a small amount of Vehicle, and triturate to make a smooth paste. Add the Vehicle to make the contents pourable. Transfer the contents stepwise and quantitatively to a calibrated container using the remainder of the Vehicle. Add sufficient Vehicle to bring to final volume. Shake to mix well.

2 ASSAY

2.1 PROCEDURE

Solution A: 10 mM sodium phosphate adjusted with phosphoric acid to a pH of 3.0. Pass through a nylon filter of 0.45-µm pore size, and degas.

Mobile phase: Acetonitrile and Solution A (65:35)

Diluent: Water adjusted with phosphoric acid to a pH of 3.0

Standard stock solution: 5 mg/mL of clopidogrel prepared from USP Clopidogrel Bisulfate RS and Diluent. Mix well, and sonicate for 3 min.

Store at 2°-8°

Standard solution: Transfer 2.0 mL of the Standard stock solution to a 1-L volumetric flask, and dilute with Diluent to volume. Mix well, centrifuge a portion of the solution for 5 min at 14,000 rpm, and use the supernatant. Protect from light, and store at 2"-8".

Sample solution: Shake each bottle of Oral Suspension thoroughly. Transfer 2.0 mL of the Oral Suspension to a 1-L volumetric flask, and dilute with Diluent to volume. Mix well, centrifuge a portion of the solution for 5 min at 14,000 rpm, and use the supernatant. Protect from light, and store at 2°-8°.

2.1.1 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 235 nm

Column: 2.1-mm x 25-cm; 5-µm packing L7

2.1.2 Temperatures

Column: 35°

Autosampler: 5"

Flow rate: 0.3 mL/min

Injection volume: 20 µL

2.1.3 System suitability

Sample: Standard solution

[NOTE-The retention time for clopidogrel is about 7.4 min.]

2.1.4 Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0% for replicate injections

2.1.5 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of clopidogrel (C₁₆H₁₆CINO₂S) in the portion of Oral Suspension taken:

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

r_U = peak response of clopidogrel from the Sample solution

r_S = peak response of clopidogrel from the Standard solution

C_S = concentration of clopidogrel in the Standard solution (mg/mL)

C_U = nominal concentration of clopidogrel in the Sample solution (mg/mL)

Acceptance criteria: 90.0%-110.0%

3 SPECIFIC TESTS

PH(791): 2.1-3.1

4 ADDITIONAL REQUIREMENTS

PACKAGING AND STORAGE: Package in tight, light-resistant containers. Store at 2°-8° or at controlled room temperature.

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

BEYOND-USE DATE: NMT 90 days after the date on which it was compounded, when stored at 2°-8° or at controlled room temperature

USP REFERENCE STANDARDS (11)

USP Clopidogrel Bisulfate RS