Ionspray ionization-mass spectrometric separation and determination of heptafluorobutyryl derivatives of polyamines.
We describe here an application of ionspray ionization-mass spectrometry (IS-MS) for simultaneous determination of putrescine, spermidine, and spermine without the need for coupling with other separation techniques such as high-performance liquid chromatography or capillary electrophoresis. Because it was essential to increase the mass of these compounds to eliminate contaminated low-mass ions, heptafluorobutyryl (HFB) derivatives were chosen. It was found that each HFB-polyamine appeared as a single major cation carrying an ammonium ion in a solution of 50% acetonitrile-water containing 0.5% ammonium acetate at an orifice potential of 20 V. Under these conditions, the three polyamines after addition of 15N-labeled polyamines as internal standards, followed by heptafluorobutylation, were determined simultaneously. It was shown, using a sample injection bulb set between the syringe drive and ionspray probe, that the analysis time for data acquisition was about 3 min and the sensitivity was about 10 fmol. In addition, polyamines in rat liver were determined by this method after simple fractionation with a small column of CM-cellulose with reasonable accuracy and precision. Behaviors of acetylated polyamines were also described, and the results showed that the acetylated polyamines would become additional target compounds in the present method.
Furuumi
N
N
Faculty of Pharmaceutical Sciences, Josai University, Keyaki-dai 1-1, Saitama, Sakado, 350-0290, Japan.
Amano
D
D
Xu
Y J
YJ
Samejima
K
K
Niitsu
M
M
Shirahata
A
A
D000818:Animals; D008099:Liver / Q000737:chemistry; D013058:Mass Spectrometry / Q000379:methods*; D011073:Polyamines / Q000737:chemistry / Q000302:isolation & purification*; D051381:Rats; D012015:Reference Standards
D011073:Polyamines