Liquid chromatographic/atmospheric pressure chemical ionization mass spectrometric analysis of synthetic elastase inhibitor peptide.
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.
Kasuya
F
F
Faculty of Pharmaceutical Science, Kobe-gakuin University, Japan.
Igarashi
K
K
Fukui
M
M
Fukumori
Y
Y
Tokumito
H
H
Fukuda
T
T
Tsuda
Y
Y
Okada
Y
Y
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
D015842:Serine Proteinase Inhibitors; D015843:Serpins; D010196:Pancreatic Elastase