Identification of aromatic hydrocarbons in high-boiling fraction of pyrolysis oil by capillary gas-liquid chromatography and mass spectrometry

1982 ◽  
Vol 47 (2) ◽  
pp. 476-494 ◽  
Author(s):  
Jan Novrocík ◽  
Marta Novrocíková ◽  
Antonín Čapek
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Aromatic Hydrocarbons ◽  
Boiling Point ◽  
Capillary Gas Chromatography ◽  
Coal Tar ◽  
Normal Pressure ◽  
Gas Liquid Chromatography ◽  
Pyrolysis Oil

Capillary gas chromatography and mass spectrometry have been used for identification of most main high-boiling components of fraction of pyrolysis oil (boiling point 250 to 350° C under normal pressure) especially those boiling above the b.p. of acenaphthene. All methyl homologues of acenaphthene, phenanthrene, some isomeric methylfluorenes, trimethyl- and methylethyl naphthenes, phenylnaphthalenes, dimethylbiphenyls, benzindans, methylbenzindans and other aromatic hydrocarbons have been prepared as standards. In connection with the preparation of some trimethyl- and methylethylnaphthalenes a discussion is presented of the course of chloromethylation and acetylation of 1- and 2-methyl- and 2-ethylnaphthalenes. Content of methyl-homologues of some hydrocarbons (acenaphthene, fluorene, phenanthrene, and anthracene) in the high-boiling fraction of pyrolysis oil has been compared with that present in similar fraction of coal tar.

Monitoring drug concentrations in a case of combined overdosage with primidone and methsuximide.

1976 ◽  
Vol 22 (6) ◽  
pp. 915-921 ◽  
Author(s):  
G F Johnson ◽  
C J Least ◽  
J W Serum ◽  
E B Solow ◽  
H M Solomon
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Therapeutic Decision ◽  
Serum Samples ◽  
Monitoring Drug ◽  
Drug Concentrations

Abstract We describe a case of fatal overdosage with primidone and methsuximide. During the early phase of the patient's hospital course we found concentrations of methsuximide, N-desmethylmethsuximide, and primidone in serum that far exceeded the usual therapeutic concentrations, as determined by gas-liquid chromatography. Determination of N-desmethylmethsuximide in peritoneal fluid demonstrated concentrations comparable to those in serum. This led to the therapeutic decision to manage the patient by dialysis. Subsequently, serum samples collected during the course of hospitalization were analyzed quantitatively by gas-liquid chromatography for methsuximide, N-desmethylmethsuximide, primidone, phenobarbital, and diphenylhydantoin. Selected serum specimens were also analyzed by gas chromatography-mass spectrometry, and N-methyl-2-hydroxymethyl-2-phenylsuccinimide, a metabolite of methsuximide not previously described in human serum, was identified by analysis of its mass spectrum.

DISULPHATES OF NEUTRAL STEROIDS IN THE AMNIOTIC FLUID FROM ANENCEPHALIC PREGNANCIES

1971 ◽  
Vol 51 (1) ◽  
pp. 109-115 ◽  
Author(s):  
T. LUUKKAINEN ◽  
E. A. MICHIE ◽  
R. VIHKO
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Amniotic Fluid ◽  
Normal Pregnancy ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Human Bile ◽  
Normal Term ◽  
Pregnancy Urine

SUMMARY Steroid disulphate fractions were obtained by chromatography on Sephadex LH-20 from samples of amniotic fluid from three pregnancies complicated by anencephaly. Several of the steroids with a 3β-hydroxy-5-ene structure found in normal amniotic fluid could not be detected. 5-Androstene-3β,17α-diol, the main steroid disulphate in normal amniotic fluid was present in concentrations of <5% of the values at normal term. The disulphates of neutral steroids found in highest concentrations in the amniotic fluid of anencephalic pregnancies were those of isomeric pregnanediols; 5α-pregnane-3α,20α-diol, 5α-pregnane-3β,20α-diol and 5β-pregnane-3α,20α-diol. The quantities of these metabolites of progesterone in the amniotic fluid of anencephalic pregnancies were similar to those in normal pregnancies. A saturated 18-hydroxylated C19 steroid, most probably 3α,18-dihydroxy-5α-androstan-17-one, was identified by gas—liquid chromatography and gas chromatography—mass spectrometry. Although this compound has been previously identified in human bile and in normal pregnancy urine, this appears to be the first identification of a saturated C19 steroid in amniotic fluid.

Steroids in meconium and faeces from newborn infants

1972 ◽  
Vol 180 (1059) ◽  
pp. 179-186 ◽  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Newborn Infants ◽  
Gas Chromatography Mass Spectrometry ◽  
Gas Liquid Chromatography ◽  
Chromatography Mass Spectrometry

Gas—liquid chromatography and gas chromatography—mass spectrometry have been used to study the pattern of sterols in meconium and faeces from newborn infants. Meconium contained metabolites from various steps in the biosynthesis of cholesterol, e. g. lanosterol, 24, 25-dihydro-∆ 8 -lanosterol, 24, 25-dihydro-∆ 9 -lanosterol, 4 α ,14 α -dimethyl-5 α -cholest-7 (and 8)-en-3 β -ol, 4, 4-dimethyl-5 α -cholest-8-en-3 β -ol, 4, 4-dimethyl-5 α -cholesta-8, 14-dien-3 β -ol and ∆ 7 - and ∆ 8 -methostenol. Meconium and faeces from newborns also contained the sulphate esters of 20, 22-dihydroxycholesterol and of 22-, 23- and 24-hydroxycholesterol.

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