D-(+)-Glucosamine Hydrochloride CAS 66-84-2 Assay 98.0%~102.0% Factory

Glucosamine Hydrochloride
C6H13NO5·HCl 215.63
d-Glucose, 2-amino-2-deoxy-, hydrochloride;
2-Amino-2-deoxy--d-glucopyranose hydrochloride [66-84-2].
DEFINITION
Glucosamine Hydrochloride contains NLT 98.0% and NMT 102.0% of glucosamine hydrochloride (C6H13NO5·HCl), calculated on the dried basis.
IDENTIFICATION
• A. Infrared Absorption <197K>
• B. Identification Tests-General, Chloride <191>: Meets the requirements
• C. The retention time of the glucosamine peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.
ASSAY
• Procedure
Buffer: In a 1-L volumetric flask, dissolve 3.5 g of dibasic potassium phosphate in water. Add 0.25 mL of ammonium hydroxide, dilute with water to volume, and mix. Adjust with phosphoric acid to a pH of 7.5.
Mobile phase: Acetonitrile and Buffer (75:25)
Diluent: Acetonitrile and water (50:50)
Standard solution: 3.8 mg/mL of USP Glucosamine Hydrochloride RS in Diluent
Sample solution: 3.8 mg/mL of Glucosamine Hydrochloride in Diluent. [Note-Shake by mechanical means to aid dissolution.]
Chromatographic system
(See Chromatography <621>, System Suitability.)
Mode: LC
Detector: UV 195 nm
Column: 4.6-mm × 15-cm; 5-µm packing L8
Column temperature: 35
Flow rate: 1.5 mL/min
Injection size: 10 µL
System suitability
Sample: Standard solution
[Note-The peak for the glucosamine moiety elutes at about 10 min. The chromatogram shows a large additional peak near the void volume, due to the chloride ion. ]
Suitability requirements
Tailing factor: NMT 2.0 for the glucosamine peak
Efficiency: NLT 1500 theoretical plates
Relative standard deviation: NMT 2.0%
Analysis
Samples: Standard solution and Sample solution
Calculate the percentage of glucosamine hydrochloride (C6H13NO5·HCl) in the portion of Glucosamine Hydrochloride taken:
Result = (rU/rS) × (CS/CU) × 100
rU = peak response from the Sample solution
rS = peak response from the Standard solution
CS = concentration of USP Glucosamine Hydrochloride RS in the Standard solution (mg/mL)
CU = concentration of Glucosamine Hydrochloride in the Sample solution (mg/mL)
Acceptance criteria: 98.0%-102.0% on the dried basis
IMPURITIES
• Residue on Ignition <281>: NMT 0.1%
• Chloride and Sulfate, Sulfate 221: A 0.10-g portion shows no more sulfate than corresponds to 0.25 mL of 0.020 N sulfuric acid (NMT 0.24%).
• Arsenic, Method II <211>: NMT 3 ppm
• Heavy Metals, Method II <231>: NMT 10 ppm
SPECIFIC TESTS
• Optical Rotation, Specific Rotation <781S>: +70.0 to +73.0
Sample solution: 25 mg/mL. Measure the specific rotation 3 h after preparation.
• pH <791>
Sample solution: 20 mg/mL
Acceptance criteria: 3.0-5.0
• Loss on Drying <731>: Dry a sample at 105 for 2 h: it loses NMT 1.0% of its weight.
ADDITIONAL REQUIREMENTS
• Packaging and Storage: Preserve in tight, light-resistant containers.
• USP Reference Standards <11>
USP Glucosamine Hydrochloride RS