Determination of dimethylnitrosamine in air, water, and soil by thermal energy analysis: measurements in Baltimore, Md.

1977 ◽  
Vol 11 (6) ◽  
pp. 581-584 ◽  
Author(s):  
David H. Fine ◽  
David P. Rounbehler ◽  
Anna Rounbehler ◽  
Arlene Silvergleid ◽  
Eugene Sawicki ◽  
...  
1987 ◽  
Vol 70 (1) ◽  
pp. 64-68 ◽  
Author(s):  
J Ian Gray ◽  
Michael A Stachiw

Abstract A collaborative study was conducted on the U.S. Food and Drug Administration (FDA) dichloromethane extraction method for determining volatile N-nitrosamines in baby bottle rubber nipples. Following dichloromethane extraction, A'-nitrosamines were determined by gas chromatography-thermal energy analysis. Six pairs of blind duplicate rubber nipple samples representing 6 lots were analyzed by 11 collaborating laboratories. All samples were portions taken from equilibrated composites of cut-up rubber nipples obtained from manufacturers in the United States. Recoveries of the internal standard (N-nitrosodipropylamine) at approximately 20 ppb ranged from 10 to 120%. Reproducibility relative standard deviations (RSDJ were between 35 and 45% for N-nitrosamine levels from 10 to 20 ppb. However, when data from laboratories with recoveries less than 75% were excluded (this is now specified in the method), RSD„ values were between 11 and 32% for N-nitrosamine levels from 6 to 26 ppb. Values were consistent with or better than those reported for other analytical techniques designed to quantitate trace contaminants at the low ppb level, e.g., afiatoxin in foods. The method has been adopted official first action for the quantitation of volatile N-nitrosamines in baby bottle rubber nipples.


1993 ◽  
Vol 76 (3) ◽  
pp. 578-581 ◽  
Author(s):  
Walter Fiddler ◽  
Robert C Doerr

Abstract A gas chromatographic (GC) procedure is described for the determination of dibutylamine (DBA) in ham at less than 1 ppm. Sample is extracted with 0.5N HCI, centrifuged, made basic, and then extracted with isopropyl alcohol. Final determination is by GC/thermal energy analysis in the nitrogen mode. Six replicate analyses of ham fortified with 0.5 ppm DBA gave a recovery of 90.2 ± 3.4%. Over a range of 0.5 to 3.0 ppm DBA, the repeatability was 0.07 ppm, and the coefficient of variation was 6.07%. Limit of detection was 01 ppm. Effectiveness of the procedure was demonstrated on selected ham samples.


1977 ◽  
Vol 11 (6) ◽  
pp. 577-580 ◽  
Author(s):  
David H. Fine ◽  
David P. Rounbehler ◽  
Eugene Sawicki ◽  
Ken Krost

1993 ◽  
Vol 21 (1-2) ◽  
pp. 1-9 ◽  
Author(s):  
George M. Janini ◽  
Stephen D. Fox ◽  
Michael L. Citro ◽  
Gary M. Muschik ◽  
Haleem J. Issaq

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