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Quantitative measurement of clenbuterol at the femtomole level in plasma and urine by combined gas chromatography/negative ion chemical ionization mass spectrometry
Author(s) -
Girault J.,
Gobin P.,
Fourtillan J. B.
Publication year - 1990
Publication title -
biomedical and environmental mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.475
H-Index - 121
eISSN - 1096-9888
pISSN - 0887-6134
DOI - 10.1002/bms.1200190206
Subject(s) - chemistry , chromatography , clenbuterol , mass spectrometry , gas chromatography , chemical ionization , detection limit , gas chromatography–mass spectrometry , electron ionization , ethyl acetate , selected ion monitoring , ion source , reagent , ion , analytical chemistry (journal) , ionization , organic chemistry
A highly sensitive and specific assay was developed for the quantitative measurement of clenbuterol at the femtomole level in human plasma and urine. Clenbuterol and the internal standard ( 2 H 9 )clenbuterol were measured by gas chromatography/negative ion chemical ionization mass spectrometry with methane as the reagent gas. The two compounds of interest were extracted from the biological samples at pH 13 using ethyl acetate. After two subsequent purification steps, the cleaned‐up organic extract was derivatized with pentafluoropropionic anhydride. The mass spectrometer was set to monitor the abundant [M HCl] − ions of the perfluoroacyl derivatives ( m / z 368 and 377), which were generated in the ion source by an electron capture process. This assay required 1 ml of plasma or 0.5 ml of urine and the detection limit of the method was 5 pg ml −1 with a 12.8% relative standard deviation. The accuracy of the clenbuterol assay was also tested day to day with quality control specimens spiked blind to the analyst. The mean difference between the theoretical and actual values was lower than 4.1%.