Rapid Determination of Butylated Hydroxyanisole, tert-Butylhydroquinone, and Propyl Gallate in Edible Oils by Electron Capture Gas-Liquid Chromatography

1976 ◽  
Vol 59 (6) ◽  
pp. 1208-1212 ◽  
Author(s):  
B Denis Page ◽  
Barry P C Kennedy

Abstract A rapid method is described for the determination of 2- and 3-tert-butyl-4-hydroxyanisole (2- and 3-BHA), tert-butylhydroquinone (TBHQ), and propyl gallate (PG) as their heptafluorobutyrates in edible oils. A solution of the oil in ether-benzene is treated with heptafluorobutyric anhydride (HFBA) in the presence of trimethylamine as catalyst. Excess HFBA is destroyed and a suitably diluted aliquot is analyzed by electron capture gas-liquid chromatography. An internal standard is added before derivatization to aid quantitation and identification of the antioxidants. Average recoveries from an oil spiked at 1, 5, 5, and 5 ppm TBHQ, 2-BHA, 3-BHA, and PG were 110, 105, 106, and 102%, respectively. At these low levels, however, some late-eluting peaks interfered. Butylated hydroxytoluene is not determined by this method.

1977 ◽  
Vol 60 (3) ◽  
pp. 505-508
Author(s):  
Jozef R Senten ◽  
Jozef M Waumans ◽  
Jean M Clement

Abstract A method is described for the quantitative determination of butylated hydroxyanisole and butylated hydroxytoluene in edible oils. Both antioxidants are extracted with acetonitrile, and quantitated by gas-liquid chromatography, using a hydrogen flame ionization detection system and di-tert-butyl-4-hydroxyanisole as an internal standard. The standard addition technique is used. Recoveries from oils containing 70–400 ppm by weight of both antioxidants ranged from 88 to 104%.


1977 ◽  
Vol 23 (7) ◽  
pp. 1338-1339 ◽  
Author(s):  
E Rey ◽  
J M Turquais ◽  
G Olive

Abstract We used 100 microliters of plasma for the determination of diazepam. After the internal standard, prazepam, is added, the serum is directly extracted with diethyl ether, the extract is evaporated, the residue is dissolved in ethanol, and the drug is measured by gas-liquid chromatography, with use of an electron capture detector. With this procedure, 2.5 ng of diazepam in the sample can be speedily measured with specificity, accuracy, and reproducibility (CV = 4.5%).


1984 ◽  
Vol 219 (3) ◽  
pp. 883-889 ◽  
Author(s):  
A Gorchein

A derivative of delta-aminolaevulinic acid (AmLev), 2-methyl-3-acetyl-4-(3-propionic acid pentafluorobenzyl ester)pyrrole, with favourable properties for g.l.c. with electron-capture detection, was synthesized. Less than 1 pg could be detected on the column. 6-Amino-5-oxohexanoic acid formed the analogous derivative under similar conditions and was used as the internal standard in the development of a highly sensitive and specific assay for AmLev. The method has been applied to peripheral-venous and umbilical-cord plasma and to cerebrospinal fluid of normal and porphyric subjects.


1978 ◽  
Vol 24 (7) ◽  
pp. 1109-1111
Author(s):  
M Youssefi ◽  
S D Faust ◽  
S T Zenchelsky

Abstract We describe a rapid method for determining light halogenated hydrocarbons (LHH) in urine by electron capture gas-liquid chromatography. The hydrocarbons are extracted from urine into pentane. A 2-microliter injection of the pentane extract provides a detection limit of less than 1 microgram/liter.


1971 ◽  
Vol 51 (3) ◽  
pp. 447-454 ◽  
Author(s):  
W. COOPER ◽  
M. G. COYLE ◽  
J. A. MILLS

SUMMARY A method is described for estimating oestriol in 2–10 ml samples of human pregnancy peripheral plasma. It incorporates acid hydrolysis, chemical purification, methylation, chromatography on alumina columns, formation of a derivative and quantitative determination by gas chromatography. A radioactive internal standard was added to correct for procedural losses. Plasma oestriol determinations in five normal patients throughout pregnancy and delivery are reported.


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