Determination of deoxyspergualin by gas chromatography-selected-ion monitoring.
A gas chromatographic-selected-ion monitoring method was developed for the sensitive and specific determination of deoxyspergualin in dog plasma using a capillary column and a C8-amide homologue of deoxyspergualin as an internal standard. Extraction and purification of deoxyspergualin from its constituents, 7-guanidinoheptanamide and glyoxylylspermidine, and its possible metabolites was achieved by using CM-Sephadex C-25 column chromatography with stepwise elution with sodium chloride solution. Treatment of deoxyspergualin with acetylacetone resulted in the formation of the volatile pyrimidine derivative of 7-guanidinoheptanamide accompanying hydrolytic cleavage in the alpha-hydroxyglycine moiety of deoxyspergualin. Deoxyspergualin could be determined in a concentration of 10 ng/ml in plasma. The method was applied to the determination of deoxyspergualin in plasma during and after intravenous infusion into dogs.
Yamashita
K
K
Research Laboratory, Nippon Kayaku Co., Ltd., Tokyo, Japan.
Watanabe
K
K
Koga
R
R
Mizuguchi
S
S
Hashimoto
Y
Y
Nakamura
T
T
Umezawa
H
H
D000818:Animals; D002849:Chromatography, Gas; D004285:Dogs; D008401:Gas Chromatography-Mass Spectrometry; D006146:Guanidines / Q000097:blood / Q000493:pharmacokinetics; D007202:Indicators and Reagents; D007262:Infusions, Intravenous
D006146:Guanidines; D007202:Indicators and Reagents; C037258:gusperimus