title: LC/MS/MS method for the determination of trace amounts of cefmetazole and cefpodoxime proxetil contaminants in pharmaceutical manufacturing environments.
abstract: In this study, a selective and sensitive LC/MS/MS method for the determination of trace amounts of cefmetazole (CMZ) and cefpodoxime proxetil (CPDXPR) contaminants in manufacturing environments was developed. The necessary sensitivity of this method was estimated based on the detection limit for Penicillin G required by the FDA and the total surface area and volume of the manufacturing facility. The detection limits of this method were estimated to be 10 pg/ml for CMZ and 5 pg/ml for CPDXPR from the signal to noise ratio and as a result satisfactory sensitivity was achieved. The method was linear in a concentration range from 0.20 to 3.20 ng/ml. The accuracy and precision were verified by the determination of the amount of CMZ and CPDXPR added to the sampling materials, a glass plate and a silica fiber filter. The mean recoveries of nine replicated determinations from the glass plate were 99.1% with 5.58%R.S.D. for CMZ and 97.1% with 3.80%R.S.D. for CPDXPR, and those from the silica fiber filter were 100.7% with 4.50%R.S.D. for CMZ and 95.4% with 2.85%R.S.D. for CPDXPR. This method has been successfully applied to the determination of CMZ and CPDXPR contaminants in samples collected from an actual manufacturing environment.
authors.affiliation: Analytical and Quality Evaluation Research Laboratories, Sankyo Co. Ltd., 1-12-1 Shinomiya, Hiratsuka-shi, Kanagawa 254-0014, Japan. fukutu@sankyo.co.jp
authors.forename: Naoto
authors.initials: N
authors.lastname: Fukutsu
authors.forename: Yuichi
authors.initials: Y
authors.lastname: Sakamaki
authors.forename: Takao
authors.initials: T
authors.lastname: Kawasaki
authors.forename: Koichi
authors.initials: K
authors.lastname: Saito
authors.forename: Hiroyuki
authors.initials: H
authors.lastname: Nakazawa
mesh_terms: D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D015311:Cefmetazole / Q000032:analysis* / Q000302:isolation & purification; D015296:Ceftizoxime / Q000031:analogs & derivatives* / Q000032:analysis / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods; D004345:Drug Industry / Q000592:standards*; D004784:Environmental Monitoring / Q000379:methods*; D013058:Mass Spectrometry / Q000379:methods; D012680:Sensitivity and Specificity; D000097623:Cefpodoxime
chemical_list: D000900:Anti-Bacterial Agents; D015311:Cefmetazole; D015296:Ceftizoxime; D000097623:Cefpodoxime