title: Sensitive quantitation of residual phenylhydrazine in antipyrine by LC-ICP-MS with iodo derivatization.
abstract: Phenylhydrazine is a genotoxic impurity commonly used as a raw material in active pharmaceutical ingredients. In this study, a novel method, using inductively coupled plasma-mass spectrometry combined with two-dimensional liquid chromatography (LC-ICP-MS), was employed for the quantitation of residual phenylhydrazine in antipyrine. The compound 2,3,5-triiodobenzoyl chloride, which contains three iodine atoms, was investigated as a derivatization reagent. The DL 0.06 ppm was obtained, and the method was applied to the quantitation of residual phenylhydrazine in antipyrine. No residual phenylhydrazine was detected in five lots of antipyrine obtained from the commercial source.
authors.affiliation: Analytical Research Laboratories, CMC Division, Mitsubishi Tanabe Pharma Corp.
authors.forename: Koki
authors.initials: K
authors.lastname: Harigaya
authors.forename: Hiroyuki
authors.initials: H
authors.lastname: Yamada
authors.forename: Shingo
authors.initials: S
authors.lastname: Horimoto
authors.forename: Hiroyuki
authors.initials: H
authors.lastname: Nishi
authors.forename: Jun
authors.initials: J
authors.lastname: Haginaka
mesh_terms: D000983:Antipyrine / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D057230:Limit of Detection; D013058:Mass Spectrometry / Q000379:methods*; D010659:Phenylhydrazines / Q000032:analysis*
chemical_list: D010659:Phenylhydrazines; C030299:phenylhydrazine; D000983:Antipyrine