title: Quantitative determination method for trace amount of penicillin contaminants in commercially available drug product by HPLC coupled with tandem mass spectrometry.
abstract: A quantitative determination method for trace amount of penicillin contaminants in an active pharmaceutical ingredient (API) has been developed. Selective extraction of penicillin contaminants from the matrix containing API and specific separation among penicillin contaminants were achieved through an on-line column switching technique with gradient elution, followed by tandem mass spectrometric determination. Validation was conducted on the developed method in terms of specificity, linearity, accuracy, precision, and detection limit, and appeared reasonable. The detection limit was estimated as 0.03 ng/ml or lower of the concentration of penicillin contaminants in the preparation, corresponding to 4 parts par billion (ppb) against the API. This fulfilled the regulatory requirement by the authorities.
authors.affiliation: Analytical Research Laboratories, Fujisawa Pharmaceutical Co., Ltd, Osaka, Japan.
authors.forename: Wataru
authors.initials: W
authors.lastname: Takada
authors.forename: Toshikazu
authors.initials: T
authors.lastname: Adachi
authors.forename: Noriaki
authors.initials: N
authors.lastname: Kihara
authors.forename: Satoshi
authors.initials: S
authors.lastname: Kitamura
authors.forename: Teruyuki
authors.initials: T
authors.lastname: Kitagawa
authors.forename: Masaki
authors.initials: M
authors.lastname: Mifune
authors.forename: Yutaka
authors.initials: Y
authors.lastname: Saito
mesh_terms: D000658:Amoxicillin / Q000032:analysis; D000667:Ampicillin / Q000032:analysis; D055598:Chemical Phenomena; D002627:Chemistry, Physical; D002851:Chromatography, High Pressure Liquid; D004340:Drug Contamination; D005436:Floxacillin / Q000032:analysis; D007202:Indicators and Reagents; D013058:Mass Spectrometry; D010406:Penicillins / Q000032:analysis*
chemical_list: D007202:Indicators and Reagents; D010406:Penicillins; D005436:Floxacillin; D000667:Ampicillin; D000658:Amoxicillin