THERMOSPRAY HIGH-PERFORMANCE LIQUID-CHROMATOGRAPHY MASS-SPECTROMETRIC DETERMINATION OF CYCLOSPORINS

被引:12
作者
ABIAN, J
STONE, A
MORROW, MG
CREER, MH
FINK, LM
LAY, JO
机构
[1] US FDA,NATL CTR TOXICOL RES,JEFFERSON,AR 72079
[2] UNIV ARKANSAS MED SCI HOSP,LITTLE ROCK,AR 72205
[3] JOHN L MCCLELLAN VET ADM MED CTR,DEPT PATHOL,DIV TOXICOL,LITTLE ROCK,AR 72205
关键词
D O I
10.1002/rcm.1290061111
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
The cyclic undecapeptides cyclosporin (Csp) A, CspD and dihydro CspC (HCspC) were analyzed by high-performance liquid chromatography/thermospray-mass spectrometry (HPLC/TSP-MS) on line with a UV detector. Positive ion partial (1000-1300 u) mass spectra of these compounds could be obtained with 1-2 pmol injected on column. Mass spectra were characterized by signals corresponding to the [M + H]+ ion as well as fragment ions derived from the loss of 112 (CspA and CspD) or 44, 114 and 114 + 44 (HCspC) mass units from the parent ion. The same qualitative profile was observed for negative-ion acquisition where the ions were formed by proton abstraction. The application of the technique to the characterization of CspA and its major hydroxylated and dealkylated metabolites in human blood samples is presented.
引用
收藏
页码:684 / 689
页数:6
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