scholarly journals Headspace Gas Chromatographic Determination of 1,3-Butadiene in Simulated Saliva

2000 ◽  
Vol 83 (4) ◽  
pp. 929-932 ◽  
Author(s):  
Shirley Abrantes ◽  
Tereza C Dos Santos ◽  
Grazieli SimÕES

Abstract A headspace gas chromatographic (GC) method was developed to determine 1,3-butadiene (1,3-BD) in simulated saliva in contact with chewing gum. The calibration graph was linear, and the limit of detection was 0.004 mg/L, which is well below the migration limit for this substance. The headspace GC method provides rapid and reliable analysis for monitoring 1,3-BD migration from chewing gum into simulated saliva. In this paper, we report headspace methodology for sensitive determination of 1,3-BD in chewing gum and results of selected analyses, enabling preliminary assessment of possible exposure to 1,3-BD through migration.

1987 ◽  
Vol 70 (1) ◽  
pp. 18-21
Author(s):  
Timothy P Mcneal ◽  
Charles V Breder

Abstract A headspace gas chromatographic procedure has been developed for the determination of 1,3-butadiene in rubber-modified plastics and in some foods. Polymer solutions or foods are equilibrated in sealed vials at 90°C, and headspace samples are injected into a gas chromatograph. 1,3-Butadiene residues are measured using a flame ionization detector and are quantitated by the method of standard additions or an external calibration curve. Refrigerator tubs, vegetable oil bottles, chewing gum, and foods in contact with this type of packaging were analyzed. Limits of quantitation varied with the matrix, ranging from 2 ng/g (ppb) in chewing gum to 20 ng/g in polymers. 1,3-Butadiene was found in one polymer at 53 ng/g with an 8% coefficient of variation. The procedure yields "apparent" trace levels of 1,3-butadiene, and confirmation by a complementary technique is required.


2014 ◽  
Vol 68 (11) ◽  
Author(s):  
Pavel Mikuška ◽  
Lukáš Bružeňák ◽  
Zbyněk Večeřa

AbstractA method for the rapid and sensitive determination of peroxyacetyl nitrate (PAN) in air based on a chemiluminescence reaction with an alkaline solution of luminol in the chemiluminescence aerosol detector is described. The PAN is chromatographically separated from nitrogen dioxide and ozone in a packed column filled with 5 % OV-1 on Chromosorb 30/60 and the eluted PAN is detected via the direct reaction with the luminol solution consisting of 0.002 mol L−1 luminol, 1 vol. % Brij-35 and 0.1 mol L−1 KOH. The limit of detection is 14.9 ng m−3 (3 ppt) of PAN. Alternatively, the PAN after separation is thermally converted to NO2 which is detected by the chemiluminescence reaction with a solution consisting of 0.002 mol L−1 luminol, 0.5 mol L−1 KOH, 0.2 mol L−1 Na2SO3, 0.1 mol L−1 KI, 0.05 mol L−1 EDTA and 0.5 vol. % triton X-100. The alternative approach affords the simultaneous determination of PAN and NO2. The limit of detection is 50 ppt of PAN and 50 ppt of NO2. The time resolution is 3 min. The method was applied to the measurement of ambient peroxyacetyl nitrate in air.


1986 ◽  
Vol 21 (12) ◽  
pp. 701-704 ◽  
Author(s):  
R. Binetti ◽  
S. Di Marzio ◽  
P. Di Prospero ◽  
L. Gramiccioni ◽  
G. Viviano ◽  
...  

2003 ◽  
Vol 86 (4) ◽  
pp. 759-763 ◽  
Author(s):  
Peter Cavlovic ◽  
Mohan Mankotia ◽  
Peter Pantazopoulos ◽  
Peter M Scott

Abstract Nightshade berries containing glycoalkaloids can be a contaminant in green peas. Methodology was developed to detect this contamination. The glycoalkaloid α-solasonine was extracted from frozen green peas with 1% (v/v) acetic acid, cleaned up on a C18 cartridge, and determined by liquid chromatography with UV detection at 200 nm. Method performance characteristics for the determination of α-solasonine include linearity from 140 to 1500 ng injected (r = 0.9996–0.9999); recovery ranging from 68 to 79%; limit of quantitation (LOQ) = 4.5 ppm (280 ng standard), and limit of detection = 0.64 ppm (40 ng standard). At the LOQ, the expanded uncertainty at 95% confidence was 0.38 × the reported value. The method was applied to the detection of α-solasonine in frozen green peas in a 2-year study of 60 samples of frozen green peas from Ontario, Canada. None of the samples contained α-solasonine. No unripe berries of Solanum nigrum were detected visually in the samples.


1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.


1985 ◽  
Vol 68 (5) ◽  
pp. 952-954
Author(s):  
Maria Luisa Serralheiro ◽  
Maria Lurdes Quinta

Abstract A method has been developed for the detection of aflatoxin Mi in milk. The toxin is extracted with chloroform, the extract is evaporated, and the residue is partitioned between carbon tetrachloride and an aqueous saline-methanol solution. The toxin is once again extracted with chloroform from the methanol solution and analyzed by thin layer chromatography. The limit of detection of Mi in powdered milk is 0.5 μg/ kg; recoveries of added Mj are about 83%. The limit of detection can be improved to 0.3 μg/kg if the plate is sprayed with an aqueous solution of H2S04 after development.


1984 ◽  
Vol 67 (5) ◽  
pp. 913-915
Author(s):  
Chih-Kuang Chou ◽  
David C Locke

Abstract A rapid, precise, and accurate liquid chromatographic (LC) method is described for the determination of benzoyl peroxide (BP) in acne preparations. BP is extracted from a water dispersion of the preparation with dichloromethane (DCM), and an aliquot is eluted from a C-18 reverse phase LC column with acetonitrile-O.lOM aqueous NaCI04. Selective and sensitive quantitation is accomplished with a reductive mode electrochemical detector. This detector is an order of magnitude more sensitive than a 240 nm UV absorption detector; the lower limit of detection is 2 ng for a 4 μL injection. The recovery of BP is 99.4% and the detector response is linear to at least 2 μg per 4 μL injection.


1976 ◽  
Vol 22 (6) ◽  
pp. 772-776 ◽  
Author(s):  
S A Harding ◽  
G F Johnson ◽  
H M Solomon

Abstract We describe a sensitive and precise gas-chromatographic method, in which cytosine is used as the internal standard, for determination of an antifungal agent, 5-fluorocytosine, in serum. The trimethylsilyl derivative of this drug is well separated from the internal standard and from normal serum constituents. Amphotericin B does not interfere with the determination of 5-fluorocytosine. The lower limit of detection for 5-fluorocytosine is 1 mg/liter when 200 mul of serum is analyzed. Within-run precision (CV), established by analysis of 10 replicates, was 4.5% at a concentration of 19.9 mg/liter. Twenty-five serum samples were analyzed for 5-fluorocytosine by a microbiological assay and by the gas-chromatographic method. Mean value observed with the bioassay was 78.5 mg/liter and with our procedure was 69.4 mg/liter. When values for our assay were regressed against values for the bioassay, slope of the least-squares line was 0.85, intercept was 2.7 mg/liter, and r was 0.93.


1979 ◽  
Vol 62 (1) ◽  
pp. 201-202 ◽  
Author(s):  
Robert D Stubblefield

Abstract Clearly defined zones of citrinin can be obtained on thin layer chromatographic (TLC) plates and measured by fluorodensitometry. Silica gel plates were prepared as a slurry with aqueous 0.05M Na2EDTA (ethylenediaminetetraacetic acid), spread at 0.5 mm wet thickness, and activated at 105°C for 1 hr. Plates were developed in acetic acid-benzene (5+95). The limit of detection was 10 ng citrinin/zone. Densitometric analysis (365 nm excitation, 505 nm emission) revealed that a linear relationship exists for levels of 10 ng to at least 100 ng/zone wtih a coefficient of variation of ±5%.


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