title: Measurement of residual solvents in a drug substance by a purge-and-trap method.
abstract: The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.
authors.affiliation: Department of Inorganic and Analytical Chemistry, Budapest University of Technology and Economics, Szent Gellért tér 4, H-1111 Budapest, Hungary. lakatos@mail.bme.hu
authors.forename: Miklós
authors.initials: M
authors.lastname: Lakatos
mesh_terms: D001554:Benzene / Q000737:chemistry; D002251:Carbon Tetrachloride / Q000737:chemistry; D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods* / Q000592:standards; D004126:Dimethylformamide; D004340:Drug Contamination; D005018:Ethyl Chloride / Q000031:analogs & derivatives / Q000737:chemistry; D005410:Flame Ionization / Q000295:instrumentation / Q000379:methods* / Q000592:standards; D005559:Formamides / Q000737:chemistry; D008752:Methylene Chloride / Q000737:chemistry; D009584:Nitrogen / Q000737:chemistry; D004364:Pharmaceutical Preparations / Q000032:analysis* / Q000737:chemistry; D012015:Reference Standards; D015203:Reproducibility of Results; D012107:Research Design; D012680:Sensitivity and Specificity; D012984:Software; D012997:Solvents / Q000032:analysis* / Q000737:chemistry / Q000145:classification; D013696:Temperature; D014867:Water / Q000737:chemistry
chemical_list: D005559:Formamides; D004364:Pharmaceutical Preparations; D012997:Solvents; D014867:Water; C501196:1,1-dichloroethane; D005018:Ethyl Chloride; D008752:Methylene Chloride; D004126:Dimethylformamide; D002251:Carbon Tetrachloride; D001554:Benzene; D009584:Nitrogen