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Quantitative gas chromatographic mass spectrometric determination of pinaverium—bromide in human serum
Author(s) -
de Weerdt G. A.,
Beke R. P.,
Verdievel H. G.,
Barbier F.,
Jonckheere J. A.,
de Leenheer A. P.
Publication year - 1983
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.1200100310
Subject(s) - chemistry , chromatography , detection limit , bromide , selected ion monitoring , chemical ionization , flame ionization detector , gas chromatography , gas chromatography–mass spectrometry , mass spectrometry , ion , ionization , inorganic chemistry , organic chemistry
A method has been developed for quantitative determination of pinaverium‐bromide, a quaternary ammonium derivative with papaverine‐like activity, in human serum. The method involves a chloroform extraction of serum spiked with N ‐(6,6‐dimethyl bicyclo[3.1.1]2‐heptenyl‐ethoxyethyl)perhydro‐1,4‐oxazine as internal standard. After evaporation of the solvent, and reduction of the residue with Raney‐Nickel, the internal standard and the reduced pinaverium‐bromide are re‐extracted from the reaction mixture with toluene and analysed isothermally on a fused silica column coated with OV‐101. Although chemical ionization with methane revealed intense protonated molecular ions for both pinaverium‐bromide and the internal standard, selectivity and sensitivity were significantly lower in comparison with electron impact ionization at 70 eV. Therefore, quantification was performed in the electron impact mode by single ion monitoring of the common fragment ion at m / z 100.2. A linear detector response was observed up to 160 ng ml −1 . A within‐run assay precision better than 2% CV ( n =5) was found, and a detection limit of 1 ng pinaverium‐bromide ml −1 of serum was attained.