The determination of cyclophosphamide and its metabolites in blood plasma as stable trifluoroacetyl derivatives by electron capture chemical ionization gas chromatography/mass spectrometry

1994 ◽  
Vol 23 (3) ◽  
pp. 149-158 ◽  
Author(s):  
G. Momerency ◽  
K. Van Cauwenberghe ◽  
P. H. Th. J. Slee ◽  
A. T. Van Oosterom ◽  
E. A. De Bruijn
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Blood Plasma ◽  
Electron Capture ◽  
Chemical Ionization ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
In Blood Plasma

scholarly journals Determination of blood lead by electron-capture negative chemical ionization gas chromatography-mass spectrometry

1996 ◽  
Vol 42 (2) ◽  
pp. 286-291 ◽  
Author(s):  
G S Baird ◽  
R L Fitzgerald ◽  
S K Aggarwal ◽  
D A Herold
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Electron Capture ◽  
Isotope Dilution ◽  
Chemical Ionization ◽  
Gas Chromatography Mass Spectrometry ◽  
Pyrrolidine Dithiocarbamate ◽  
Negative Chemical Ionization ◽  
Chromatography Mass Spectrometry

Abstract An electron-capture negative chemical ionization (NCI) gas chromatography-mass spectrometry (GC-MS) method for determination of lead (Pb) in blood samples is described. Extraction of Pb from the sample does not involve hot digestion but is based on treatment at ambient temperature. The blood sample is supplemented with a known amount of internal standard (204Pb) for isotope dilution and is treated with concentrated nitric acid. After adjusting the pH to 7, the Pb is extracted into toluene as the pyrrolidine-dithiocarbamate chelate. Samples are then derivatized with 4- fluorophenylmagnesium bromide to form Pb(FC6H4)4. The use of NCI offers enhanced sensitivity (by 75-fold better than previously used electron ionization), gives good precision and accuracy, and has no observable memory effect. The isotope dilution GCoff methodology typically agreed within 2-3% of expected values for the College of American Pathologists blood Pb specimens and the National Institute of Standards and Technology Standard Reference Material 955a.

Determination of Polychlorodibenzo-p-dioxins and Related Compounds in Commercial Chlorophenols

1972 ◽  
Vol 55 (1) ◽  
pp. 85-92 ◽  
Author(s):  
David Firestone ◽  
John Ress ◽  
N L Brown ◽  
R P Barron ◽  
J N Damico
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Electron Capture ◽  
Gas Chromatography Mass Spectrometry ◽  
Alumina Column ◽  
Spectrometric Data ◽  
Chromatography Mass Spectrometry ◽  
Related Compounds ◽  
Chromatographic Mass

Abstract Twenty-one commercial chlorophenols were examined for the presence of polychlorodibenzo- p-dioxins (chlorodioxins) and related compounds. The chlorophenols were dissolved in aqueous alkali, extracted with petroleum ether, and fractionated on an alumina column. Alumina fractions were examined by electron capture gas chromatography and combined gas chromatography-mass spectrometry. Chlorodioxin content was estimated by electron capture gas chromatography. The presence of chlorodioxins, polychlorodibenzofurans (chlorofurans), and polychlorodiphenyl ethers (chloroethers) was confirmed by combined gas chromatography-mass spectrometry. The 2,3,-7,8-tetrachlorodioxin was found in 3 of 6 samples of 2,4,5-trichlorophenol but was not detected in any of the 11 samples of tetra- and pentachlorophenol that were examined. Hexachlorodioxin was present at levels ranging from 0.17 to 39 ppm in all 8 pentachlorophenols examined. Hexa-, hepta-, and octachlorodioxins as well as a wide variety of chlorofurans and chloroethers of varying chlorine content were present in most of the tetra- and pentachlorophenols. In addition, the gas chromatographic- mass spectrometric data suggested that some of the chlorophenols contained methoxy- and dimethoxypolychlorofurans and methoxypolychloroethers as well as polychlorohy droxybiphenyl.

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