Bromocriptine Mesylate Capsules

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

DOWNLOAD PDF HERE

1 DEFINITION

Bromocriptine Mesylate Capsules 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 solution, as obtained in the test for Organic Impurities.

3 ASSAY

PROCEDURE

Conduct this procedure without exposure to daylight and with minimum exposure to artificial light.

Buffer: 0.125 g/L of ammonium carbonate in water

Mobile phase: Acetonitrile and Buffer (3:2)

Standard solution: 1.0 mg/mL of bromocriptine from USP Bromocriptine Mesylate RS in dehydrated alcohol. Sonicate as needed.

Sample solution: 1.0 mg/mL of bromocriptine in methanol, prepared as follows. Remove, as completely as possible, the contents of NLT 10 Capsules. Weigh and determine the average weight per Capsule. Mix the combined contents, and transfer a weighed quantity of the powder, nominally equivalent to 50 mg of bromocriptine, to a 50-mL volumetric flask. Add 30 mL of dehydrated alcohol, and shake for 15 min. Dilute with dehydrated alcohol to volume, mix, and filter. Use this solution without

Chromatographic system

(See Chromatography (621), System Suitability.)

Mode: LC

Detector: UV 300 nm

Column: 4-mm x 25-cm; packing L7

Flow rate: 2 mL/min

Injection volume: 20 µL

System suitability

Sample: Standard solution

Suitability requirements

Column efficiency: NLT 1000 theoretical plates

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

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

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

r_u = peak response from the Sample solution

r_s = peak response from the Standard solution

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

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

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

Dissolution 〈711〉

Medium: 0.1 N hydrochloric acid; 500 mL

Apparatus 2: 50 rpm

Time: 60 min

Standard solution: USP Bromocriptine Mesylate RS in Medium, at a concentration similar to the Sample solution. [Note—A volume of alcohol not to exceed 5% of the total volume of the Standard solution may be used to bring the Standard into solution before dilution with Medium.]

Sample solution: Sample per Dissolution 〈711〉, passed through a glass-ber lter.

Instrumental conditions

(See Fluorescence Spectroscopy 〈853〉.)

Mode: Fluorometry

Excitation wavelength: 315 nm

Emission wavelength: 445 nm

Blank: Medium

Analysis

Samples: Standard solution and Sample solution

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

Tolerances: NLT 75% (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

Protect all solutions from light.

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

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

Sample solution: Transfer the contents of 1 Capsule into a 25-mL volumetric ask. Add 15 mL of Diluent, and shake by mechanical means

for 20 min. Dilute with Diluent to volume, and mix. Filter, and dilute 10.0 mL of the clear ltrate with Diluent to 50.0 mL.

Instrumental conditions

(See Ultraviolet-Visible Spectroscopy 〈857〉.)

Mode: UV

Analytical wavelength: Maximum absorbance (about 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 Capsule 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

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: 2.3 mg/mL of USP Bromocriptine Mesylate RS in methanol, equivalent to 2 mg/mL of bromocriptine

Standard solution 1: 0.06 mg/mL (3.0%) of bromocriptine in methanol, from Standard stock solution

Standard solution 2: 0.04 mg/mL (2.0%) of bromocriptine in methanol, from Standard stock solution

Standard solution 3: 0.02 mg/mL (1.0%) of bromocriptine in methanol, from Standard stock solution

Standard solution 4: 0.01 mg/mL (0.50%) of bromocriptine in methanol, from Standard stock solution

Sample solution: 2.0 mg/mL, of bromocriptine in methanol, prepared as follows. Transfer a quantity of the Capsule contents, equivalent to 20 mg of bromocriptine, to a conical flask. Add 10 mL of methanol, and stir by mechanical means for 20 min. Centrifuge the suspension for 10 min at about 3500 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 volume: 50 µL as 1.5-cm bands

Developing solvent: Methylene chloride, dioxane, alcohol, and ammonium hydroxide (180:15:5:1)

Spray reagent: 0.2% 0-phthalaldehyde in sulfuric acid.

Analysis

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

Develop under the exclusion of light in a tank lined with filter paper, previously equilibrated for 30 min, using Developing solvent until the solvent front has moved a distance of 15 cm on the plate. Dry the plate briefly in a current of cold air. Spray evenly with the Spray reagent, and view the plate under long-wavelength UV light.

Acceptance criteria: Any major secondary spot, other than the principal spot, obtained from the Sample solution is not greater in size and intensity than the spot obtained from Standard solution 1 (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.

USP REFERENCE STANDARDS (11)

USP Bromocriptine Mesylate RS