质量标准求助？USP38 Iohexol Injection DEFINITION Iohexol Injection is a sterile solution of Iohexol in Water for Injection. It contains NLT 95.0% and NMT 105.0% of the labeled amount of iohexol (C19H26I3N3O9) as organically bound iodine. It may contain small amounts of suitable buffers and Edetate Calcium Disodium as a stabilizer. Iohexol Injection intended for intravascular or intrathecal use contains no antimicrobial agents. IDENTIFICATION • A. The retention times of the major peaks of the Sample solution correspond to those of the System suitability solution, as obtained in the test for Organic Impurities. ASSAY • Procedure Sample: A volume of Injection equivalent to 300 mg of iodine Analysis: Transfer the Sample to a glass-stoppered, 250-mL conical flask. Add 25 mL of 1.25 N sodium hydroxide and 500 mg of powdered zinc, connect the flask to a reflux condenser, and reflux the solution for 1 h. Cool the flask to room temperature, rinse the condenser with 20 mL of water, disconnect the flask from the condenser, and filter the mixture. Rinse the flask and the filter thoroughly with small portions of water, adding the rinsings to the filtrate. Add 5 mL of glacial acetic acid, and titrate with 0.1 N silver nitrate VS. Each mL of 0.1 N silver nitrate is equivalent to 27.37 mg of C19H26I3N3O9. Acceptance criteria: 95.0%–105.0% IMPURITIES • Organic Impurities Solution A: Acetonitrile Solution B: Water Mobile phase: The percentage of Solution A increases from 1% to 13% at a rate of 0.2%/min. System suitability solution: 1.5 mg/mL, 0.0075 mg/mL, and 0.0069 mg/mL each of USP Iohexol RS, USP Iohexol Related Compound A RS, and USP Iohexol Related Compound C RS in water Sample solution: 1.5 mg/mL of Iohexol Chromatographic system (See Chromatography 621, System Suitability.) Mode: LC Detector: UV 254 nm Column: 4.6-mm × 25-cm stainless steel column; packing L1 Flow rate: 1.0 mL/min Injection volume: 10 µL System suitability Sample: System suitability solution Suitability requirements Resolution: NLT 20.0 between iohexol related compound A and iohexol related compound C Analysis Sample: Sample solution Excluding peaks with retention times between 0.84 (relative to the endo-isomer of iohexol, which is the first main peak) and 1.0, calculate the percentage of O-alkylated compounds and any other individual impurity peak, in the portion of Iohexol taken: Result = (rU/rT) × 100 rU = = peak response of each impurity rT = = sum of all the peak responses Acceptance criteria Individual impurity: NMT 0.6% of O-alkylated compounds; NMT 0.1% of any other individual impurity Total impurities: NMT 0.3%, excluding O-alkylated compounds SPECIFIC TESTS • Bacterial Endotoxins Test 85: NMT 0.2 USP Endotoxin Unit per 50 mg of iodine • pH 791: 6.8–7.7 • Particulate Matter in Injections 788: The Injection labeled for intrathecal use meets the requirements for small-volume injections. • Free Iodide: Transfer 5.0 mL of Injection to a suitable container, add 20 mL of water, and titrate with 0.001 N silver nitrate VS using a silver electrode in combination with an appropriate reference electrode. Each mL of 0.001 N silver nitrate is equivalent to 0.1269 mg of iodine. Acceptance criteria: NMT 0.02%, based on the content of iohexol • Injections 1: Meets the requirements ADDITIONAL REQUIREMENTS • Packaging and Storage: Preserve Injection intended for intravascular or intrathecal use in single-dose or multiple-dose plastic or Type I glass containers. Store at controlled room temperature, protected from light. Do not freeze. • Labeling: Label containers of Injection to direct the user to discard any unused portion. The labeling states also that it is not to be used if it is discolored or contains a precipitate. Label it also to state its routes of administration. When the specific dose strength is not intended for intrathecal use, label it to indicate “serious injury can occur if given by intrathecal route”. • USP Reference Standards 11 USP Endotoxin RS USP Iohexol RS USP Iohexol Related Compound A RS 5-(Acetylamino)-N,N¢-bis(2,3-dihydroxypropyl)-2,4,6-triiodo-1,3-benzenedicarboxamide. USP Iohexol Related Compound C RS N,N¢-Bis(2,3-dihydroxypropyl)-5-nitro-1,3-benzenedicarboxamide.查看更多
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