title: Liquid chromatographic/atmospheric pressure chemical ionization mass spectrometric analysis of synthetic elastase inhibitor peptide.
abstract: A liquid chromatographic/atmospheric pressure chemical ionization mass spectrometric method for the determination of tert-butyloxycarbonyl-Tyr-Leu-Val-CH2Cl (Boc-YLV-CH2Cl) was investigated. Boc-YLV-CH2Cl was eluted from a Cosmosil 5C8 column in a solvent system of 0.1% acetic acid-methanol (30: 70, v/v). The positive ion spectrum of Boc-YLV-CH2Cl showed a quasi-molecular ion at m/z 526 with fragment ions which provided structural information. Boc-YLV-CH2Cl was purified from blood and tissue samples with Sep-Pak C18 cartridges. The analysis in biological samples was performed by focusing the characteristic ion at m/z 526. The calibration graphs were linear over the concentration range studied (injected amounts of 9.5-190 pmol). The method was applied to the determination of Boc-YLV-CH2Cl in biological samples.
authors.affiliation: Faculty of Pharmaceutical Science, Kobe-gakuin University, Japan.
authors.forename: F
authors.initials: F
authors.lastname: Kasuya
authors.forename: K
authors.initials: K
authors.lastname: Igarashi
authors.forename: M
authors.initials: M
authors.lastname: Fukui
authors.forename: Y
authors.initials: Y
authors.lastname: Fukumori
authors.forename: H
authors.initials: H
authors.lastname: Tokumito
authors.forename: T
authors.initials: T
authors.lastname: Fukuda
authors.forename: Y
authors.initials: Y
authors.lastname: Tsuda
authors.forename: Y
authors.initials: Y
authors.lastname: Okada
mesh_terms: D000595:Amino Acid Sequence; D000818:Animals; D001274:Atmospheric Pressure; D002851:Chromatography, High Pressure Liquid; D008168:Lung / Q000737:chemistry; D008297:Male; D013058:Mass Spectrometry; D051379:Mice; D008815:Mice, Inbred Strains; D008969:Molecular Sequence Data; D010196:Pancreatic Elastase / Q000037:antagonists & inhibitors*; D015842:Serine Proteinase Inhibitors / Q000032:analysis*; D015843:Serpins
chemical_list: D015842:Serine Proteinase Inhibitors; D015843:Serpins; D010196:Pancreatic Elastase