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Ergotaman-3¢,6¢,18-trione, 2-bromo-12¢-hydroxy-2¢-(1-methylethyl)-5¢-(2-methylpropyl)-, monomethanesulfonate (salt), (5¢)-;
2-Bromoergocryptine monomethanesulfonate (salt) [22260-51-1].
Bromocriptine Mesylate contains NLT 98.0% and NMT 102.0% of C32H40BrN5O5·CH4SO3, calculated on the dried basis.
• A. Infrared Absorption 197M: Undried
• B. Ultraviolet Absorption 197U
Sample solution: 50 µg/mL in 0.1 M methanolic methanesulfonic acid
Acceptance criteria: Meets the requirements
Sample solution: 600 mg of Bromocriptine Mesylate
Analysis: Dissolve with 80 mL of a mixture of acetic anhydride and glacial acetic acid (7:1). Titrate with 0.1 N perchloric acid VS. Perform a blank determination, and make any necessary correction (see Titrimetry 541). Each mL of 0.1 N perchloric acid is equivalent to 75.07 mg of C32H40BrN5O5·CH4SO3.
Acceptance criteria: 98.0%102.0% on the dried basis
• Procedure 1: Limit of Methanesulfonic Acid Content
Sample solution: 400 mg of Bromocriptine Mesylate
Analysis: Dissolve with 70 mL of methanol. Titrate under nitrogen with 0.1 N methanolic potassium hydroxide VS. Perform a blank determination, and make any necessary correction (see Titrimetry 541). Each mL of 0.1 N methanolic potassium hydroxide is equivalent to 9.61 mg of CH3SO3H.
Acceptance criteria: NLT 12.5% and NMT 13.4% of CH3SO3H on the dried basis
• Procedure 2
Solution A: 0.1 N citric acid solution. Adjust with hydrochloric acid to a pH of 2.0.
Diluent: Methanol and Solution A (1:1)
Solution B: Acetonitrile and 0.01 M phosphate buffer, pH 7.0 (2:3)
Solution C: Acetonitrile and 0.01 M phosphate buffer, pH 7.0 (3:2)
Mobile phase: See the gradient table below.
System suitability solution: 2.0 mg/mL each of -ergocryptine and Bromocriptine Mesylate in Diluent
Standard stock solution: 46 µg/mL of USP Bromocriptine Mesylate RS in methanol and Solution A (1:1). [NoteDissolve in 50% of the flask volume of methanol and dilute with Solution A to volume. ]
Standard solution: 4.6 µg/mL of USP Bromocriptine Mesylate RS in Diluent from the Standard stock solution
Sample solution: 4.6 mg/mL of Bromocriptine Mesylate in methanol and Solution A (1:1). [NoteDissolve in 50% of the flask volume of methanol and dilute with Solution A to volume. ]
Detector: UV 300 nm
Column: 4.6-mm × 15-cm; 3-µm packing L1
Flow rate: 2 mL/min
Injection size: 20 µL
Samples: System suitability solution and Standard solution
[NoteThe relative retention times for -ergocryptine and bromocriptine mesylate are 0.46 and 1.0, respectively. ]
Resolution: NLT 15 between -ergocryptine and bromocriptine mesylate, System suitability solution
Tailing factor: NMT 1.5, System suitability solution
Relative standard deviation: NMT 10.0%, Standard solution
Samples: Standard solution and Sample solution
[NoteThe relative retention times for bromocriptine and bromocriptinine are 1.0 and 1.7, respectively. ]
Calculate the percentage of each impurity in the portion of Bromocriptine Mesylate taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
Individual impurities: NMT 0.4% of bromocriptinine is found; NMT 0.1% of any individual impurity is found.
Total impurities: NMT 1.0%
• Color of Solution 631
Matching solutions: Prepare three solutions, A, B, and C, containing, respectively, the following parts of cobaltous chloride CS, ferric chloride CS, cupric sulfate CS, and dilute hydrochloric acid (1 in 40).
A: 3.0: 3.0: 2.4: 31.6
B: 1.0: 2.4: 0.4: 36.2
C: 0.6: 2.4: 0: 37.0
Sample solution: 10 mg/mL of Bromocriptine Mesylate in methanol
Analysis: Compare the Sample solution with 10-mL portions of the Matching solutions in suitable matched tubes.
Acceptance criteria: The solution is clear and not darker in color than Matching solutions A, B, and C.
• Optical Rotation, Specific Rotation 781S
Sample solution: 10 mg/mL, in a mixture of methylene chloride and methanol (1:1)
Acceptance criteria: +95 to +105
• Loss on Drying
(See Thermal Analysis 891.)
Analysis: Determine the percentage of volatile substances by thermogravimetric analysis using 10 mg of Bromocriptine Mesylate. Heat the specimen under test at the rate of 10/min in an atmosphere of nitrogen at a flow rate of 45 mL/min. Record the thermogram from ambient temperature to 160.
Acceptance criteria: It loses NMT 4.0% of its weight.
• Packaging and Storage: Preserve in tight, light-resistant containers, in a cold place.
• USP Reference Standards 11
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USP35NF30 Page 2387Pharmacopeial Forum: Volume No. 36(5) Page 1173