title: Development and validation of a fast static headspace GC method for determination of residual solvents in permethrin.
abstract: A fast static headspace gas chromatography (HS-GC) method was developed to separate all residual solvents present in commercial active pharmaceutical ingredient (API) batches of permethrin. A total of six residual solvents namely 2-methylpentane, 3-methylpentane, methylcyclopentane, n-hexane, cyclohexane and toluene were found in typical commercial batches of permethrin; and three of them are not in the list of ICH solvents. All six residual solvents were baseline separated in five minutes by the new method presented in this paper. The method was successfully validated as per International Conference on Harmonisation (ICH) guidelines. Evaluation of this method was conducted to separate 26 commonly used solvents in the manufacturing of various APIs, key intermediates of APIs and pharmaceutical excipients. The results of the evaluation demonstrated that this method can also be used as a general method to determine residual solvents in various APIs, intermediates and excipients that are used in pharmaceutical products.
authors.affiliation: Merial Inc., Analytical R&D, 631 US Route 1 south, North Brunswick, NJ 08902, USA. Electronic address: Jingzhi.tian@merial.com.
authors.forename: Jingzhi
authors.initials: J
authors.lastname: Tian
authors.affiliation: Merial Inc., Analytical R&D, 631 US Route 1 south, North Brunswick, NJ 08902, USA.
authors.forename: Abu
authors.initials: A
authors.lastname: Rustum
mesh_terms: D002849:Chromatography, Gas / Q000379:methods*; D004340:Drug Contamination; D026023:Permethrin / Q000737:chemistry*; D012997:Solvents / Q000032:analysis*
chemical_list: D012997:Solvents; D026023:Permethrin
keywords: HS-GC method; Method development; Permethrin; Residual solvent; Validation