Entacapone 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

Entacapone Tablets contain an amount of entacapone equivalent to NLT 90.0% and NMT 110.0% of the labeled amount of entacapone (C₁₄H₁₅N₃O₅).

2 IDENTIFICATION

Change to read:

A. SPECTROSCOPIC IDENTIFICATION TESTS (197), Infrared Spectroscopy: 197K (CN) 1-MAY-2020): The sample shows a medium band at about 2216 crm and strong bands at about 1628, 1604, 1544, 1512, 1440, 1376, 1348, 1296, 1280, and 1208 cm similar to the reference preparation.

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

PROCEDURE

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Buffer: 2.1 g/L of monobasic sodium phosphate. Adjust with phosphoric acid to a pH of 2.1.

Diluent: Methanol and tetrahydrofuran (70:30)

Mobile phase: Methanol, tetrahydrofuran, and Buffer (44:2:54)

Standard solution: 0.5 mg/ml. of USP Entacapone RS in Diluent

30% of the final flask volume of methanol, and shake for 5 min. Dilute with methanol to volume. Centrifuge a portion of this solution, and use the supernatant.

Chromatographic system

(See Chromatography (621) System Suitability)

Mode: LC

Detector: UV 300 nm

Column: 4.6-mm x 25-cm, 5-μm packing L11

Flow rate: 1 mL/min

Injection volume: 10 μm

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 1.5%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of entacapone (C₁₄H₁₅N₃O₅) in the portion of Tablets taken:

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

r_U = peak response from the Sample solution

r_S = peak response from the Standard solution

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

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

Acceptance criteria: 90.0%-110.0%

4 PERFORMANCE TESTS

DISSOLUTION (711)

Test 1

Medium: pH 5.5 phosphate buffer (6.8 g/L of monobasic potassium phosphate in water adjusted with 1 Maodium hydroxide to a pit of 3.5) 900 mL

Apparatus 2: 50 rpm

Times: 30 min

Standard stock solution: 0.22 mg/ml of UP Entacapone RS, prepared as follows. Transfer a suitable quantity of USP Ertacacone RS to an appropriate volumetric flank, and dische in 2% of the flask volume of retrahydrofuran. Dilute with Medium to volume. Protect this

solution from light

Standard colution: 0.022 mg/m, of fiP Entacaeone RS from the Standard stock solution in Medium, Protect this solution from light

Sample solution: Pass a portion of the solution through a suitable filter of 20 µm pore size. Dilate with Medium, if necessary Protect this solution from light

Instrumental conditions

(See Ulzopletable Spectroscopy (857).)

Moder UV

Analytical wavelength: 313 m

Path length: 1 cm

Blank: Tetrahydrofuran and Medium (0.1:99.8)

Analysis

Samples: Standard solution and Sample solution

Carculate the percentage of the labeled amount of entacapone (C₁₄H₁₅N₃O₅) dissolved:

Result = (A_u/A_s) x (C_s/L) x V x 100

A_u = absorbance of the Sample solution

A_s = absorbance of the Standard solution

C_s = concentration of the Standard solution (mg/m)

L =  label claim (mg/Tablet)

V = volume of Ahdium, 900 ml.

Tolerances: NLT 80% (Q) of the labeled amount of entacapone (C₁₄H₁₅N₃O₅) is dissolved.

Test 2: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.

Medium: pi 55 phosphate buffer (6.8 g/L of monobasic potassium phosphate in water, adjusted with 5 M sodium hydroxide to a pH of 5.5); 900 mL

Apparatus 2:50 rpm

Time: 45 min

Standard stack solution: 45 mg/ml, of Face RS prepared as follows. Transfer a mustalrie santity of Entacapore RS to an appropriate volumetric flask, and dissolve in Sts of the flask volume of methanol Deute with Medium to volume. Use this solution within 6.5h.

Standard solution: 0.018 mg/m of UP Ensacocone is from the Standard stock solution in Medium. Use this solution within 6.5h.

Sample solution: Pass a portion of the solution under test through a suitable filter. Transfer 2 mL of the fiftrate to a 25-ml volumetric flask, and dilute with Medium to solume Pass the resulting solution through a suitable filter of 0.45 um pore size. Use this solution within 6.5 h

Instrumental conditions

(See Ultraviolet-Visible Spectroscopy (857).)

Mode: UV

Analytical wavelength: 313 nm

Path length: 1 cm

Blank: Medium

Analysis

Samples: Standurnd colution and Sample solution

Calinulate the percentage of the labelind amount of entacapone (C₁₄H₁₅N₃O₅) dissolved:

Result = (A_u/A_s) x (C_s/L) x V x 100

A_u = absorbance of the Sample solution

A_s = absorbance of the Standard solution

C_s = concentration of the Standard solution (mg/m)

L =  label claim (mg/Tablet)

V = volume of Ahdium, 900 ml.

Tolerances: NLT 80% (2) of the labelest amount of entasapine (CH, NO) is dissved.

Test 3: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 8.

Medium: pH 15 phosphate buffer (6.8 g/L of monobasic potassium phosphate and 0.05 g/L of sodium hydrocide in water, atjusted with

M sodium hydroxide to a pH of 5.5): 900 ml

Apperstus 2:50 rpm

Time: 30 min

Standard stock solution: 0.45 mg/mt, of LISP Entacanne prepared as follows. Transfer a suitable quantity of USP Entacasone to an appropriate volumetric flask, and dissolve in 30% of the flask volume of methanol. Sonicate to dissolve, and allow the solution to cool to room temperature Dilute with methanol to volume Law the solution within th

Standard solution: 0.009 mg/ml, of USE Entagesans, BS from the Standard stock solution in Medium. Use this solution within 6h

Sample stock solutions Pass a portion of the solution through a suitable filter of 0.45-um pore size. Use this solution within 6

Sample solution: Transfer 2.0 m of the Sample stock solution to a 50 ml volumetric flask, and dilute with Medium to volume Use this

solution within 6h.

Instrumental conditions

(See Ultraviolet-Visible Spectroscopy (85).)

Mode: UV

Analytical wavelength: 578 mm

Blank: Medium

Analysis

Samples: Standard solbion and Sample solution

Calculate the percentage of the labeled amount of entacapone (C₁₄H₁₅N₃O₅​​​​​​​) dissolved:

Result = (A_u/A_s) x (C_s/L) x V x D x 100

A_u = absorbance of the Sample solution

A_s = absorbance of the Standard solution

C_s = concentration of the Standard solution (mg/m)

L =  label claim (mg/Tablet)

V = volume of Ahdium, 900 ml.

D = diution factor for the Sample solutions

Tolerances: NLT 70% (Q) of the labeled amount of entacapone (C₁₄H₁₅N₃O₅​​​​​​​) is dissolved.

Uniformity of Dosage Units (905): Meet the requirements

5 IMPURITIES

OKE UPURITIES

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Buffer, Diluent, Mobile phase, and Chromatographic system: Procced as directed in the Assay.

System sultability solution: 0.03 mg/ml each of Entacatione RS and US Entacanne Related Compound A RS in Diluent

Standard solution: 0003 mgres, of USP Entacanone RS in Diluent

Sample solution: Nominally 3 mgimt, of entacapone prepared as follows. Frely powder NLT 20 Tallets, and transfer a suitable portion of the powder to an appropriate volumetric flask Add NLT 30% if the fesal fask volume of tetrahydrofuran, and sanicate for 3 min. Add NLT 30% of the final flask volume of methanol, and shake for 5 min. Dilute with methanol to volume. Centrifuge a portion of this solution, and use the supermatant within 7h

System suitability

Samples: System stability solution and Standard solution

Suitability requirements

Resolution: NLT 2.0 between entacapone related compound A and entacapone, System suttability solution

Relative standard deviation: NMT 10.0%, Standard solution

Analysis

Samples: Standan solution and Sample solution

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

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

r_U = peak response of each impurity from the Sample solution

r_S = peak response of entacapone from the Standard solution

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

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

Acceptance criteria: See Table 1.

^a Do not include unitacapone related compound A In the calculation of total ampurities

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in light-resistant containers. Store at controlled room temperature.

Labeling: When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used.