Ubidecarenone C59H90O4863.37 2,5-Cyclohexadiene-1,4-dione, 2-[(2E,6E,10E,14E,18E,22E,26E,30E,34E)-3,7,11,15,19,23,27,31,35,39-decamethyl-2,6,10,14,18,22,26,30,34,38-tetracontadecaenyl]-5,6-dimethoxy-3-methyl; 2-[(all-E)-3,7,11,15,19,23,27,31,35,39-Decamethyl-2,6,10,14,18,22,26,30,34,38-tetracontadecaenyl)-5,6-dimethoxy-3-methyl-p-benzoquinone [303-98-0]. DEFINITION Ubidecarenone (Coenzyme Q10) contains NLT 98.0% and NMT 101.0% of ubidecarenone (C59H90O4), calculated on the anhydrous basis. IDENTIFICATION • B. Analysis: Dissolve 50 mg of Ubidecarenone in 1 mL of ethyl ether, and add 10 mL of dehydrated alcohol. To 2 mL of this solution add 3 mL of dehydrated alcohol and 2 mL of dimethyl malonate. Add 1 mL of potassium hydroxide solution (1 in 5) dropwise. Acceptance criteria: A blue color appears. ASSAY • Procedure Mobile phase: Methanol and dehydrated alcohol (65:35) System suitability solution: 0.5 mg/mL each of USP Ubidecarenone RS and USP Ubidecarenone Related Compound A RS in dehydrated alcohol. Heat at 50 for 2 min, if necessary, for complete dissolution. Standard solution: 1.0 mg/mL of USP Ubidecarenone RS in dehydrated alcohol. Heat at 50 for 2 min, if necessary, for complete dissolution. Sample solution: 1.0 mg/mL of Ubidecarenone in dehydrated alcohol. Heat at 50 for 2 min, if necessary, for complete dissolution. Chromatographic system Mode: LC Detector: UV 275 nm Column: 4.6-mm × 15-cm; packing L1 Column temperature: 35 Flow rate: Adjust to obtain a retention time of about 11 min for ubidecarenone. Injection size: 5 µL System suitability Sample: System suitability solution [NoteThe relative retention times for ubidecarenone related compound A and ubidecarenone are about 0.75 and 1.0, respectively. ] Suitability requirements Resolution: NLT 4 between ubidecarenone related compound A and ubidecarenone Relative standard deviation: NMT 0.8% for ubidecarenone Analysis Samples: Standard solution and Sample solution Calculate the percentage of ubidecarenone (C59H90O4) in the portion of Ubidecarenone taken: Result = (rU/rS) × (CS/CU) × 100
Acceptance criteria: 98.0%101.0% on the anhydrous basis IMPURITIES • Residue on Ignition 281: NMT 0.1% • Heavy Metals, Method II 231: NMT 20 ppm • Chromatographic Purity Procedure 1: Coenzymes Q7,Q8, Q9, Q11, and Related Impurities Mobile phase, System suitability solution, Sample solution, Chromatographic system, and System suitability: Proceed as directed in the Assay. Analysis Sample: Sample solution Calculate the percentage of impurities in the portion of Ubidecarenone taken: Result = (rT1/rT2) × 100
Acceptance criteria: NMT 1.0% Procedure 2: Ubidecarenone (2Z)-Isomer and Related Impurities Mobile phase: n-Hexane and ethyl acetate (97:3) System suitability solution: 1 mg/mL of USP Ubidecarenone for System Suitability RS in n-hexane Sample solution: 1 mg/mL of Ubidecarenone in n-hexane Chromatographic system Mode: LC Detector: UV 275 nm Column: 4.6-mm × 25-cm; packing L3 Flow rate: 2 mL/min Injection size: 20 µL System suitability Sample: System suitability solution [NoteThe relative retention times for ubidecarenone (2Z)-isomer and ubidecarenone are about 0.85 and 1.0, respectively. ] Suitability requirements Resolution: NLT 1.5 between the ubidecarenone (2Z)-isomer and ubidecarenone Analysis Sample: Sample solution Calculate the percentage of impurities in the portion of Ubidecarenone taken: Result = (rT1/rT2) × 100
Acceptance criteria: NMT 1.0% Total impurities: NMT 1.5%, obtained from Chromatographic Purity Procedures 1 and 2 SPECIFIC TESTS • Water Determination, Method I 921: NMT 0.2% ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve in well-closed, light-resistant containers. • USP Reference Standards 11 USP Ubidecarenone for System Suitability RS Auxiliary Information Please check for your question in the FAQs before contacting USP.
USP35NF30 Page 1460 Pharmacopeial Forum: Volume No. 31(1) Page 86Chromatographic Column Chromatographic columns text is not derived from, and not part of, USP 35 or NF 30. |