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A PGE 2 ‐derivative for quantitative gas chromatographic mass spectrometric measurement in the selected ion monitoring mode
Author(s) -
Fischer C.
Publication year - 1984
Publication title -
biomedical mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0306-042X
DOI - 10.1002/bms.1200110304
Subject(s) - chromatography , selected ion monitoring , chemistry , calibration curve , mass spectrometry , deuterium , analytical chemistry (journal) , derivative (finance) , gas chromatography , ion , extraction (chemistry) , impurity , gas chromatography–mass spectrometry , capillary action , detection limit , materials science , physics , organic chemistry , quantum mechanics , financial economics , economics , composite material
The quantification of prostaglandin PGE 2 by gas chromatography mass spectrometry in the form of an easily prepared derivative is described. After extraction and purification of biological samples the compound was derivatized in two steps to 9‐enol‐PGE 2 ‐methylester‐trimethylsilylether, 9‐enol‐PGE 2 ‐Me‐TMS 3 . The molecular ion at m / z 582 with 40% relative abundance and the fragment ion at m / z 492 with 100% relative abundance permit a specific and sensitive evaluation in the selected ion monitoring mode. The high masses selected lie above the biological background. The calibration curve produced by adding known amounts (10–200 ng) of PGE 2 to blank human urine and with ( 2 H 4 )‐deuterated PGE 2 as internal standard gave a linear correlation. The separation from biological impurities was obtained on a 50 m glass capillary column and resulted in sharp and symmetrical peaks.