Gemfibrozil 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

Gemfibrozil Tablets contain NLT 90.0% and NMT 110.0% of the labeled amount of gemfibrozil (C₁₅H₂₂O₃).

2 IDENTIFICATION

Change to read:

A.

Sample: Nominally (IRA 1-May-2021) 100 mg of gemfibrozil from a quantity of finely ground Tablets

Standard: 100 mg of USP Gemfibrozil RSA (IRA 1-May-2021)

Analysis: Shake the Sample with 10 mL of 0.1N sodium hydroxide. Filter the mixture into a 50-mL centrifuge tube, and acidify the filtrate with 3 N sulfuric acid to obtain a copious precipitate. Centrifuge, and discard the clear solution. Wash the precipitate with small portions of water, and allow it to air-dry. Prepare a potassium bromide dispersion of the precipitate and the Standard, each previously dried over silica gel for 4 h. (IRA 1-May-2021)

Acceptance criteria: The IR absorption spectrum of the Sample (IRA 1-May-2021) exhibits maxima only at the same wavelengths as the Standard. (IRA 1-May-2021)

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

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3.1 PROCEDURE

Mobile phase: Add 10 mL of acetic acid, glacial to 800 mL of methanol in a 1000-mL volumetric flask, and dilute with water to volume.

System suitability solution: 0.2 mg/mL of USP Gemfibrozil RS and 0.05 mg/mL of 2.5-dimethylphenol (IRA 1-May-2021) in Mobile phase

Standard stock solution: 1 mg/mL of USP Gemfibrozil RS in methanol

Standard solution: 0.2 mg/mL of USP Gemfibrozil RS from the Standard stock solution in Mobile phase

Sample stock solution: Nominally 1 mg/mL of gemfibrozil prepared as follows. Transfer the equivalent of 100 mg of gemfibrozil from NLT 20 finely powdered Tablets to a 100-mL volumetric flask. Add about 80 mL of methanol and shake to dissolve. Dilute with methanol to volume and pass through a suitable filter.

Sample solution: Nominally 0.2 mg/mL of gemfibrozil from the Sample stock solution in Mobile phase

3.2 Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 276 nm

Column: 3.9-mm x 30-cm; 10-µm (IRA 1-May-2021) packing L1

Flow rate: 0.8 mL/min

Injection volume: 10 µL

3.3 System suitability

Samples: System suitability solution and Standard solution

Suitability requirements

Resolution: NLT 8.0 between gemfibrozil and 2,5-dimethylphenol, (IRA 1-May-2021) System suitability solution

Relative standard deviation: NMT 2.0%, Standard solution

3.4 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gemfibrozil (C₁₅H₂₂O₃) in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of gemfibrozil (IRA 1-May-2021) from the Sample solution

r_S = peak response of gemfibrozil (IRA 1-May-2021) from the Standard solution

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

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

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

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4.1 DISSOLUTION (711)

Medium: 0.2 M phosphate buffer prepared as follows. Dissolve 545 g of potassium phosphate, monobasic in 5 L of water, add 131 g of sodium hydroxide, dilute with water to about 19.5 L, and mix well. Adjust with either 1 N phosphoric acid or 1 N sodium hydroxide to a pH of 7.5. Dilute with water to 20 L; 900 mL.

Apparatus 2: 50 rpm

Time: 30 min

Standard stock solution: 0.33 mg/mL of (IRA 1-May-2021) USP Gemfibrozil RS in Medium prepared as follows. Dissolve USP Gemfibrozil RS in an amount of methanol not to exceed 1% of the total volume of the Standard stock solution. Dilute with Medium to volume.

Standard solution: A known concentration of USP Gemfibrozil RS, similar to that of Sample solution, prepared by diluting the Standard stock solution with 1 N sodium hydroxide (IRA 1-May-2021)

Sample solution: Pass a portion of the solution under test through a suitable filter. Dilute with 1 N sodium hydroxide to a suitable nominal concentration of gemfibrozil. (IRA 1-May-2021)

Instrumental conditions

Mode: UV

Analytical wavelength: 276 nm

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of gemfibrozil (C₁₅H₂₂O₃) dissolved:

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

A_U = absorbance of the Sample solution

A_S = absorbance of the Standard solution

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

D = dilution factor of the Sample solution

V = volume of Medium, 900 mL

L = label claim (mg/Tablet) (IRA 1-May-2021)

Tolerances: NLT 80% (Q) of the labeled amount of gemfibrozil (C₁₅H₂₂O₃) is dissolved.

4.2 UNIFORMITY OF DOSAGE UNITS (905)

Meet the requirements

5 IMPURITIES

Change to read:

ORGANIC IMPURITIES

Mobile phase, System suitability solution, and Standard stock solution: Prepare as directed in the Assay.

Standard solution: 0.05 mg/mL of USP Gemfibrozil RS from the Standard stock solution in Mobile phase

Sensitivity solution: 0.005 mg/mL of USP Gemfibrozil RS from the Standard solution in Mobile phase

Sample solution: Nominally 10 mg/mL of gemfibrozil prepared as follows. Transfer 500 mg of gemfibrozil from NLT 20 finely powdered Tablets to a 50-mL volumetric flask, and add about 40 mL of Mobile phase. Sonicate and shake for 20 min. Dilute with Mobile phase to volume and pass through a suitable filter.

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 276 nm

Column: 4.6-mm × 15-cm; 5-µm packing L1

Flow rate: 1 mL/min

Injection volume: 10 µL

Run time: NLT 3 times the retention time of gemfibrozil

System suitability

Samples: System suitability solution and Sensitivity solution

Suitability requirements

Resolution: NLT 8.0 between gemfibrozil and 2,5-dimethylphenol, (IRA 1-May-2021) System suitability solution

Relative standard deviation: NMT 2.0% for the gemfibrozil peak, System suitability solution

Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of each impurity in the portion of Tablets taken:

Result = (r_U/r_S) x (C_S/C_U) x 100

r_U = peak response of each impurity from the Sample solution

r_S = peak response of gemfibrozil from the Standard solution

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

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

Acceptance criteria: The reporting threshold is 0.05% (IRA 1-May-2021)

Individual impurities: NMT 0.17%

Total impurities: NMT 1.0%

6 ADDITIONAL REQUIREMENTS

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6.1 PACKAGING AND STORAGE

Preserve in tight containers. Store at controlled roo I room temperature. Protect from light and humidity. (IRA 1-May-2021)

6.2 USP REFERENCE STANDARDS (11)

USP Gemfibrozil RS