Thiamine Hydrochloride
(thye' a min hye'' droe klor' ide).
C12H17ClN4OS·HCl 337.27 Thiazolium, 3-[(4-amino-2-methyl-5-pyrimidinyl)methyl]-5-(2-hydroxyethyl)-4-methyl-, chloride, monohydrochloride; Thiamine monohydrochloride [67-03-8]. DEFINITION
Thiamine Hydrochloride contains NLT 98.0% and NMT 102.0% of thiamine hydrochloride (C12H17ClN4OS·HCl), calculated on the anhydrous basis.
IDENTIFICATION
• A. Infrared Absorption 197K
Analysis:
Dry specimens at 105 for 2 h.
Acceptance criteria:
Meets the requirements
• B. Identification TestsGeneral, Chloride 191:
A 20-mg/mL solution meets the requirements.
ASSAY
• Procedure
Solution A:
0.005 M sodium 1-octanesulfonate in dilute glacial acetic acid (1 in 100)
Solution B:
Methanol and acetonitrile (3:2)
Mobile phase:
Solution B and Solution A (40:60)
Internal standard solution:
2% (v/v) of methylbenzoate in methanol
Standard solution:
Prepare a 1-mg/mL solution of USP Thiamine Hydrochloride RS in Mobile phase. Transfer 20.0 mL of this solution and 5.0 mL of Internal standard solution to a 50-mL volumetric flask, and dilute with Mobile phase to volume. The Standard solution contains 400 µg/mL of thiamine hydrochloride.
Sample solution:
Prepare a 2-mg/mL of Thiamine Hydrochloride in Mobile phase. Transfer 10.0 mL of this solution and 5.0 mL of Internal standard solution to a 50-mL volumetric flask, and dilute with Mobile phase to volume.
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
4-mm × 30-cm; packing L1
Flow rate:
1 mL/min
[NoteThe flow rate may be adjusted as needed to obtain a retention time of about 12 min for thiamine hydrochloride. ]
Injection size:
10 µL
System suitability
Sample:
Standard solution
Suitability requirements
Resolution:
NLT 4.0 between the thiamine and methylbenzoate peaks
Tailing factor:
NMT 2.0 for the thiamine peak
Column efficiency:
NLT 1500 theoretical plates for the thiamine peak
Relative standard deviation:
NMT 2.0% for the ratios of thiamine peak areas to the internal standard peak area
Analysis
Samples:
Standard solution and Sample solution
Calculate the percentage of thiamine hydrochloride (C12H17ClN4OS·HCl) in the portion of Thiamine Hydrochloride taken:
Result = (RU/RS) × (CS/CU) × 100
Acceptance criteria:
98.0%102.0% on the anhydrous basis
IMPURITIES
• Residue on Ignition 281:
NMT 0.2%
• Limit of Nitrate
Sample solution:
20 mg/mL of Thiamine Hydrochloride
Analysis:
To 2 mL of the Sample solution add 2 mL of sulfuric acid. Cool, and superimpose 2 mL of ferrous sulfate TS.
Acceptance criteria:
No brown ring is produced at the junction of the two layers.
• Related Compounds
Solution A, Solution B, and Mobile phase:
Proceed as directed in the Assay.
Sample solution:
1.0 mg/mL of Thiamine Hydrochloride in Mobile phase
Chromatographic system
Mode:
LC
Detector:
UV 254 nm
Column:
4.0-mm × 15-cm; packing L1
Flow rate:
0.75 mL/min
Injection size:
10 µL
Analysis
Sample:
Sample solution
Allow the Sample solution to elute for NLT three times the retention time of the main peak.
Calculate the percentage of total secondary peaks in the portion of Thiamine Hydrochloride taken:
Result = (rU/rT) × 100
Acceptance criteria:
NMT 1.0%
SPECIFIC TESTS
• Water Determination, Method I 921:
NMT 5.0%
• Absorbance of Solution
Sample solution:
100 mg/mL in water. Filter through a fine-porosity, sintered-glass funnel.
Blank:
Water
Instrumental conditions
Mode:
UV-Vis
Analytical wavelength:
400 nm
Cell:
1 cm
Analysis
Samples:
Sample solution and Blank
Determine the absorbance of the Sample solution against that of the Blank.
Acceptance criteria:
NMT 0.025
ADDITIONAL REQUIREMENTS
• Packaging and Storage:
Preserve in tight, light-resistant containers.
Auxiliary Information
Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 4835
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