Characterization of fluorinated ethylchloroformate derivatives of protein amino acids using positive and negative chemical ionization gas chromatography/mass spectrometry

1994 ◽  
Vol 23 (5) ◽  
pp. 277-282 ◽  
Author(s):  
Mahnaz Vatankhah ◽  
Mehdi Moini
Keyword(s):  
Mass Spectrometry ◽  
Amino Acids ◽  
Gas Chromatography ◽  
Chemical Ionization ◽  
Gas Chromatography Mass Spectrometry ◽  
Negative Chemical Ionization ◽  
Chromatography Mass Spectrometry ◽  
Protein Amino Acids ◽  
Derivatives Of

scholarly journals Serum total testosterone: immunoassay compared with negative chemical ionization gas chromatography-mass spectrometry

1996 ◽  
Vol 42 (5) ◽  
pp. 749-755 ◽  
Author(s):  
R L Fitzgerald ◽  
D A Herold
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Chemical Ionization ◽  
Gas Chromatography Mass Spectrometry ◽  
Poor Correlation ◽  
Total Testosterone ◽  
Silyl Ether ◽  
Negative Chemical Ionization ◽  
Serum Samples ◽  
Chromatography Mass Spectrometry

Abstract We have developed an electron capture negative chemical ionization gas chromatography-mass spectrometry (GC-MS) procedure to quantify serum testosterone in the clinically relevant range 0.69-69.3 nmol/L and used this procedure to assess Ciba Corning Diagnostics ACS:180 testosterone immunoassay. The GC-MS method involves liquid-liquid extraction of serum samples and synthesis of a pentafluorobenzyloxime/silyl ether derivative of testosterone with excellent chromatographic and electron capturing properties. The ACS testosterone assay is the first fully automated nonradioactive testosterone immunoassay approved by the US Food and Drug Administration. Patients' specimens (101, 57 males, 44 females) were analyzed by both techniques. A plot of the GC-MS (x) vs ACS (y) testosterone concentrations for men was linear (y = 1.07x + 0.19 nmol/L), showing excellent correlation (r2 = 0.98) between the two assays. Agreement of the two assays for female specimens was poor (y = 0.72x + 1.2 nmol/L), with a poor correlation (r2 = 0.31).

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