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Measurement of thromboxane B 2 in human urine by isotope dilution and negative ion chemical ionization mass spectrometry
Author(s) -
Meese C. O.,
Fischer C.,
Thalheimer P.,
Fürst O.
Publication year - 1985
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.1200120919
Subject(s) - chemistry , chemical ionization , chromatography , mass spectrometry , isotope dilution , trimethylsilyl , urine , ether , thromboxane b2 , selected ion monitoring , gas chromatography–mass spectrometry , ion , ionization , platelet , organic chemistry , biochemistry , immunology , biology
A highly sensitive and specific assay for the quantification of thromboxane B 2 (TXB 2 ) (1) in human urine is described. The method is based on the use of low‐blank ( 1 H⩽0.2%) tetradeuterated internal standard 2 (18, 18, 19, 19‐ 2 H 4 ‐thromboxane B 2 ), whose chemical synthesis is reported. After purification and high‐performance liquid chromatography (HPLC) samples are derivatized to give an open‐chain derivative of thromboxane B 2 , the methoxime pentafluorobenzyl ester tris(trimethylsilyl) ether (TXB 2 ‐MO‐PFB‐TMS 3 ), most suitable for negative ion chemical ionization mass spectrometry. In the selected ion monitoring mode limits of detection per injection for pure standards and biological samples of 10 pg and 30 pg, respectively, are established. Normal urinary excretion of 1 in humans is 37–112 ng/24 h ( n = 12).