Pyridoxine Hydrochloride (pir'' i dox' een hye'' droe klor' ide). C8H11NO3·HCl205.64 3,4-Pyridinedimethanol, 5-hydroxy-6-methyl-, hydrochloride; Pyridoxol hydrochloride [58-56-0]. DEFINITION Pyridoxine Hydrochloride contains NLT 98.0% and NMT 102.0% of pyridoxine hydrochloride (C8H11NO3·HCl), calculated on the dried basis. IDENTIFICATION • B. Identification TestsGeneral, Chloride 191: Meets the requirements ASSAY • Procedure Mobile phase: Mix 10 mL of glacial acetic acid, 0.6 g of sodium 1-hexanesulfonate, and 700 mL of water in a 1000-mL volumetric flask. Adjust with glacial acetic acid or 1 N sodium hydroxide to a pH of 3.0. Add 235 mL of methanol, and dilute with water to volume. Internal standard solution: 5 mg/mL of p-hydroxybenzoic acid in Mobile phase Standard solution: Prepare a 0.5-mg/mL solution of USP Pyridoxine Hydrochloride RS in Mobile phase. Transfer 10.0 mL of this solution and 1.0 mL of Internal standard solution to a 100-mL volumetric flask, and dilute with Mobile phase to volume. Sample solution: Prepare a 0.5-mg/mL solution of Pyridoxine Hydrochloride in Mobile phase. Transfer 10.0 mL of this solution and 1.0 mL of Internal standard solution to a 100-mL volumetric flask, and dilute with Mobile phase to volume. Chromatographic system Mode: LC Detector: UV 280 nm Column: 4.6-mm × 25-cm; packing L1 Flow rate: 1.5 mL/min Injection size: 20 µL System suitability Sample: Standard solution [NoteThe relative retention times for pyridoxine and p-hydroxybenzoic acid are about 0.7 and 1.0, respectively. ] Suitability requirements Resolution: NLT 2.5 between pyridoxine and p-hydroxybenzoic acid Relative standard deviation: NMT 3.0% for the ratios of the pyridoxine peak area response to the internal standard peak area response Analysis Samples: Standard solution and Sample solution Calculate the percentage of pyridoxine hydrochloride (C8H11NO3·HCl) in the portion of Pyridoxine Hydrochloride taken: Result = (RU/RS) × (CS/CU) × 100
Acceptance criteria: 98.0%102.0% on the dried basis IMPURITIES • Residue on Ignition 281: NMT 0.1% • Heavy Metals, Method II 231: NMT 30 ppm SPECIFIC TESTS • Content of Chloride Sample: 500 mg of Pyridoxine Hydrochloride Blank: 50 mL of methanol Titrimetric system (See Titrimetry 541.) Mode: Direct titration Titrant: 0.1 N silver nitrate VS Endpoint detection: Visual Analysis: Dissolve the Sample in 50 mL of methanol. Add 5 mL of glacial acetic acid and 23 drops of eosin Y TS. Titrate with the Titrant. Perform a Blank determination. Calculate the percentage of chloride (Cl) in the Sample taken: Result = {[(VS VB) × N × F]/W} × 100
Acceptance criteria: 16.9%17.6% on the dried basis • Loss on Drying 731: Dry a sample in vacuum over silica gel for 4 h: it loses NMT 0.5% of its weight. 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 4491 Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |