Bromocriptine Mesylate 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

Bromocriptine Mesylate Tablets contain bromocriptine mesylate (C₃₂H₄₀BrN₅O₅ · CH₄SO₃) equivalent to NLT 90.0% and NMT 110.0% of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅).

2 IDENTIFICATION

A. The principal spot of the Sample solution corresponds, in R, value and color, to that of the Standard stock solution, as obtained in the test for Organic Impurities.

3 ASSAY

PROCEDURE

Buffer: 0.01 M ammonium carbonate in water

Mobile phase: Acetonitrile and Buffer (65:35)

Standard solution: 0.22 mg/mL of USP Bromocriptine Mesylate RS in methanol

Sample solution: Transfer a quantity of powdered Tablets (NLT 20), equivalent to 10 mg of bromocriptine, to an appropriate container. Add 40 mL of methanol, and stir for 20 min, protected from light. Quantitatively filter through a fine glass filtering funnel into a 50-ml volumetric flask. Rinse the filter with methanol, adding the rinsing to the filtrate, and dilute with methanol to volume.

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 300 nm

Column: 4-mm x 25-cm; packing L1

Flow rate: 2 mL/min

Injection volume: 50 µL

System suitability

Sample: Standard solution

Suitability requirements

Coefficient of variation: NMT 3.0% for 3 replicate injections

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) in the portion of Tablets taken:

Result = (r_u /r_s ) × (C_s /C_u ) × (M_r1 /M_r2 ) × 100

r_u = peak response from the Sample solution

r_s = peak response from the Standard solution

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

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

M_r1 = molecular weight of bromocriptine, 654.59

M_r2 = molecular weight of bromocriptine mesylate, 750.70

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

DISSOLUTION (711)

Test 1: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 1.

Medium: 0.1 N hydrochloric acid; 500 mL

Apparatus 1: 120 rpm

Time: 60 min

Standard solution: USP Bromocriptine Mesylate RS at a known concentration in Medium

[NOTE-A volume of alcohol not to exceed 5% of the total volume of the Standard solution may be used to dissolve the Standard before dilution with Medium.)

Sample solution: Sample per Dissolution (711), passed through a glass-fiber filter.

Blank: Medium

Instrumental conditions

(See Fluorescence Spectroscopy (853).)

Mode: Fluorometry

Excitation wavelength: 315 nm

Emission wavelength: 445 nm

Analysis

Samples: Standard solution, Sample solution, and Blank Calculate the percentage of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) dissolved.

Tolerances: NLT 80% (Q) of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) is dissolved.

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

Medium: 0.1 N hydrochloric acid; 500 mL

Apparatus 2: 50 rpm

Time: 30 min

Buffer: 0.01 M ammonium carbonate in water

Mobile phase: Acetonitrile and Buffer (65:35)

Standard solution: Dissolve USP Bromocriptine Mesylate RS in methanol, and quantitatively dilute with Medium to obtain a solution having

a known concentration similar to the expected concentration of the Sample solution.

Sample solution: Sample per Dissolution (711).

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 300 nm

Column: 3.9-mm x 30-cm; packing L1.

Flow rate: 1.5 mL/min

Injection volume: 100 µL

System suitability

Sample: Standard solution

Suitability requirements

Relative standard deviation: NMT 2.0%

Samples: Standard solution and Sample solution

Analysis

Calculate the percentage of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) dissolved.

Tolerances: NLT 80% (Q) of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) is dissolved.

Change to read:

UNIFORMITY OF DOSAGE UNITS (905): Meet the requirements _{(CN 1-Aug-2023)}

Procedure for content uniformity

Diluent: Dissolve 1.0 g of tartaric acid in 500 mL of water, add 500 mL of methanol, and mix.

[NOTE-Protect all solutions from light.]

Standard solution: 0.04 mg/mL of USP Bromocriptine Mesylate RS in Diluent

Sample solution: Transfer 1 Tablet into a 25-ml volumetric flask. Add 15 mL of Diluent, and shake by mechanical means for 30 min. Dilute with Diluent to volume, and mix. Filter, and dilute 10.0 mL of the clear filtrate with Diluent to 50.0 mL

Instrumental conditions

(See Ultraviolet-Visible Spectroscopy 〈857〉.)

Mode: UV

Analytical wavelength: 306 nm

Cell: 1 cm

Blank: Diluent

Analysis

Samples: Standard solution, Sample solution, and Blank

Calculate the percentage of the labeled amount of bromocriptine (C₃₂H₄₀BrN₅O₅) in the Tablet taken:

Result = (A_u /A_s ) × (C_s /C_u ) × (M_r1 /M_r2 ) × 100

A_u = absorbance of the Sample solution

A_s = absorbance of the Standard solution

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

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

M_r1 = molecular weight of bromocriptine, 654.59

M_r2 = molecular weight of bromocriptine mesylate, 750.70

5 IMPURITIES

ORGANIC IMPURITIES

[NOTE-Conduct this test without exposure to daylight and with minimum exposure to artificial light. Perform the test rapidly, preparing and spotting the Sample solution last.]

Standard stock solution: 1.2 mg/mL of USP Bromocriptine Mesylate RS in methanol, equivalent to 1 mg/mL of bromocriptine

Standard solution 1: 0.50 mg/mL (5%) of bromocriptine in methanol, from Standard stock solution

Standard solution 2: 0.30 mg/mL (3%) of bromocriptine in methanol, from Standard stock solution

Standard solution 3: 0.10 mg/mL (1%) of bromocriptine in methanol, from Standard stock solution

Sample solution: Transfer an equivalent to 20 mg of bromocriptine, from powdered Tablets, to a conical flask. Add 10 mL of methanol, and mix for 20 min. Centrifuge the suspension for 10 min at 4000 rpm. Use the clear supernatant.

Chromatographic system

(See Chromatography (621), Thin-Layer Chromatography.)

Mode: TLC

Adsorbent: 0.25-mm layer of chromatographic silica gel mixture

Application volumes

Standard solutions: 10-µL, as 1.5-cm bands

Sample solution: 50-µL, as 1.5-cm bands

Developing solvent system: Methylene chloride, dioxane, alcohol, and ammonium hydroxide (180:15:5:0.1)

Spray reagent: 0.2% o-phthalaldehyde in sulfuric acid

Analysis

Samples: Standard stock solution, Standard solutions, and Sample solution

Proceed as directed in Chromatography (621), Thin-Layer Chromatography. Dry the plate for 5 min in a current of cold air. Develop in a tank lined with filter paper, previously equilibrated for 20 min, using Developing solvent system until the solvent front has moved a distance of 10 cm on the plate. Dry the plate under vacuum at room temperature for 15 min. Spray evenly with the Spray reagent, and view the plate under long-wavelength UV light.

Acceptance criteria: Any spot, other than the principal spot, from the Sample solution is not greater in size and intensity than the spot from Standard solution 2 (3.0%). Any remaining spots are not greater in size and intensity than the spot obtained from Standard solution 3 (1.0%). The sum of the organic impurities is NMT 5.0%.

6 ADDITIONAL REQUIREMENTS

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

LABELING: The labeling indicates the Dissolution test with which the product complies.

USP REFERENCE STANDARDS (11)

USP Bromocriptine Mesylate RS