Gas-chromatographic determination of homovanillic acid in human cerebrospinal fluid by electron capture detection and by mass fragmentography with a deuterated internal standard

1972 ◽  
Vol 44 (14) ◽  
pp. 2297-2301 ◽  
Author(s):  
Birgitta. Sjoquist ◽  
Erik. Anggard
1977 ◽  
Vol 60 (3) ◽  
pp. 710-715
Author(s):  
B Denis Page ◽  
Claudette F Charbonneau

Abstract A method is described for the quantitative determination of residual methylene chloride (MC) and trichloroethylene (TCE) in decaffeinated instant and ground roasted coffees. The residual solvents were isolated by a closed system vacuum distillation technique with toluene as a carrier solvent, chromatographed on Chromosorb 102, detected by both electron capture and electrolytic conductivity detectors, and quantitated by comparison with an internal standard. Average recoveries of MC from instant and ground coffees spiked at 1, 10, and 25 ppm were 100.0 (88-113), 93.2 (92-95), and 97.7% (94-102%); and for TCE, 97.2 (92-101), 96.2 (95-99), and 96.5% (92-100%), respectively. The results from both detectors are compared. At lower attenuations, levels less than 1 ppm can be readily measured. The procedure developed was applied to domestic and imported coffee samples.


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.


1985 ◽  
Vol 68 (2) ◽  
pp. 203-205
Author(s):  
Gordon Mckay

Abstract A method based on gas chromatography with electron capture detection was developed for the determination of ethylene dibromide (EDB) extracted from flour products. The procedure relies on the organic extraction of flour/water mixtures and uses an internal standard, 1- bromo-3-chloropropane. Recoveries of EDB at 10 and 100 ppb were 80.1 ± 2.8% (SD) and 84.4 ± 4.3%, respectively; recovery of the internal standard at the working concentration 500 ppb was 98.3 ± 6.7%. Calibration curves were linear over the range 5-400 ppb, with a mean overall coefficient of variation of <5%. The reliability of the procedure was assessed by using gas chromatography combined with mass spectrometry. Results are shown for determination of EDB in locally milled flour products.


1991 ◽  
Vol 74 (5) ◽  
pp. 830-835 ◽  
Author(s):  
Dalia M Gilvydis ◽  
Stephen M Walters

Abstract An interlaboratory study of the determination of captan, folpet, and captafol in tomatoes, cucumbers, and apples was conducted by 4 laboratories using wide-bore capillary column gas chromatography with electron capture detection. The 3 fungicides were determined using the Luke et al. multlresidue method modified to Include additional solvent elutlon in the optional Florisll column cleanup step used with this method. The crops were fortified with each fungicide at 3 levels per crop. Mean recoveries ranged from 86.2% for a 25.1 ppm level of captan in apples to 115.4% for a 0.288 ppm level of captafol In apples. Interlaboratory coefficients of variation ranged from 3.4% (24.7 ppm folpet) to 9.7% (0.243 ppm captafol) for tomatoes; from 2.8% (2.0 ppm captafol) to 8.2% (24.8 ppm captan) for cucumbers; and from 1.5% (0.234 ppm folpet) to 22.1% (0.266 ppm captafol) for apples.


1981 ◽  
Vol 64 (3) ◽  
pp. 584-591 ◽  
Author(s):  
Walter F Staruszkiewicz ◽  
John F Bond

Abstract A GLC procedure for the quantitative determination of the diamines putrescine and cadaverine has been developed, using their perfluoropropionyl derivatives. The amines were extracted from foods with methanol; an internal standard, hexanediamine, was added and a dry residue of their hydrochloride salts was prepared. The salts were derivatized with perfluoropropionic anhydride by heating for 30 min at 50°C. The reaction mixture was separated on an alumina column to remove excess reagent, and the derivatives were eluted with a solution of 30% ethyl acetate in toluene. GLC separations were performed on a 3% OV-225 column held at 180°C. The retention times were 4.3,5.7, and 7.0 min for the derivatives for putrescine, cadaverine, and the internal standard, respectively. Less than 1 μg diamine/g tissue could be quantitated, using either an electron capture detector or a nitrogen-specific detector. The procedure was applied to cheese and a variety of fishery products. An increase in the diamines correlated with the presence of decomposition in some of the products. A collaborative study of the method is planned.


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