(vek'' ue roe' nee um broe' mide; vek' ure oh'' nee um broe' mide).
Piperidinium, 1-[(2,3,5,16,17)-3,17-bis(acetyloxy)-2-(1-piperidinyl) androstan-16-yl]-1-methyl-, bromide;
1-(3,17-Dihydroxy-2-piperidino-5-androstan-16,5-yl)-1-methylpiperidinium bromide, diacetate [50700-72-6].
Vecuronium Bromide contains NLT 98.0% and NMT 102.0% of C34H57BrN2O4, calculated on the dried basis.
• A. Infrared Absorption 197K: Meets the requirements
• B. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
Diluent: Pipet 1.0 mL of 1 N hydrochloric acid into a 1000-mL volumetric flask, and dilute with acetonitrile to volume.
Solution A: Dissolve 8.0 g of sodium perchlorate in 6.0 mL of water, and dilute with acetonitrile to 1 L.
Solution B: Dissolve 1.6 g of ammonium chloride in 8 mL of ammonium hydroxide, and dilute with methanol to 1 L.[NoteAvoid excessive degassing to prevent the loss of ammonium hydroxide. ]
Mobile phase: Solution A and Solution B (60:40)
Standard solution: 0.5 mg/mL of USP Vecuronium Bromide RS in Diluent
Sample solution: 0.5 mg/mL of Vecuronium Bromide in Diluent
Detector: UV 215 nm
Column: 4.6-mm × 25-cm; 5-µm packing L3
Column temperature: 40
Flow rate: 0.5 mL/min
Injection size: 20 µL
Sample: Standard solution
Column efficiency: NLT 5000 theoretical plates
Relative standard deviation: NMT 2.0%
Samples: Standard solution and Sample solution
Calculate the percentage of vecuronium bromide (C34H57BrN2O4) in the portion of Vecuronium Bromide taken:
Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria: 98.0%102.0% on the dried basis
• Organic Impurities
Cation suppressor regeneration solution: 0.02 M tetrabutylammonium hydroxide
[NoteFilter components before combining. Avoid evaporation of tetrahydrofuran during degassing. ]
Combine methanol, water, and hydrochloric acid (250:1500:1). Leave at room temperature for a few min. Add 45 mL of tetrahydrofuran, and then dilute with water to 2 L.
[NoteThis applies to all of the solution preparations. The addition, with sonication, of a small amount of acetonitrile (NMT 0.5 mL per 25 mg) to the weighed quantity of the samples may be used to aid in dissolution. Shaking and sonication may also be used after the addition of the required amount of 2.5 mM hydrochloric acid. ]
System suitability solution: 5 µg/mL each of USP Vecuronium Bromide RS, USP Pancuronium Bromide RS, USP Vecuronium Bromide Related Compound A RS, USP Vecuronium Bromide Related Compound B RS, USP Vecuronium Bromide Related Compound C RS, and USP Vecuronium Bromide Related Compound F RS in 2.5 mM hydrochloric acid
Standard solution: 0.005 mg/mL of USP Vecuronium Bromide RS in 2.5 mM hydrochloric acid
Sample solution: 1 mg/mL of Vecuronium Bromide prepared as follows. To 25 mg of Vecuronium Bromide in a 25-mL volumetric flask add 0.5 mL of acetonitrile, sonicate, and rapidly dilute with 2.5 mM hydrochloric acid.
Detector: Conductivity with 4-mm cation suppressor
Column: 4.6-mm × 25-cm; 5-µm packing L1
Flow rate: 1.5 mL/min
Flow rate (for cation suppressor): 2 mL/min
Injection size: 25 µL
Samples: System suitability solution and Standard solution
[NoteThe system may need equilibration for 4 h. Rinse and store the column in acetonitrile and water (1:1). ]
Peak-to-valley ratio: NLT 2.0 between the vecuronium bromide related compound F peak and the height of the trough between the vecuronium bromide related compound F and pancuronium peaks, System suitability solution
Relative standard deviation: NMT 10.0% for three replicate injections, Standard solution
Samples: Standard solution and Sample solution
Calculate the percentage of each impurity in the portion of Vecuronium Bromide taken:
Result = (rU/rS) × (CS/CU) × (1/F) × 100
Acceptance criteria: See Table 1.
• Optical Rotation, Specific Rotation 781S
Sample solution: 10 mg/mL, in dehydrated alcohol
Acceptance criteria: 16 to 20 at 20
• Bacterial Endotoxins Test 85: NMT 10 USP Endotoxin Units/mg of vecuronium bromide
• Loss on Drying 731: Dry a sample at 105 for 2 h: it loses NMT 2.5% of its weight.
• Packaging and Storage: Preserve in tight containers, and store at room temperature.
• USP Reference Standards 11
USP Endotoxin RS
USP Pancuronium Bromide RS
3,17-dihydroxy-2,16-dipiperidinyl-5-androstane, 3,17-diacetate, dimethobromide.
USP Vecuronium Bromide Related Compound A RS
USP Vecuronium Bromide Related Compound B RS
Piperidinium, 1-[(2,3,5,16,17)-3-acetyloxy-17-hydroxy-2-(1-piperidinyl) androstan-16-yl]-1-methyl bromide.
USP Vecuronium Bromide Related Compound C RS
Piperidinium, 1-[(2,3,5,16,17)-3,17-dihydroxy-2-(1-piperidinyl) androstan-16-yl]-1-methyl bromide.
USP Vecuronium Bromide Related Compound F RS
Piperidinium, 1-[(2,3,5,16,17)-17-acetyloxy-3-hydroxy-2-(1-piperidinyl) androstan-16-yl]-1-methyl bromide.
Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 5007Pharmacopeial Forum: Volume No. 33(4) Page 682