Improved Determination of Nitrotoluenes Using Liquid Chromatography with Photolytically Assisted Thermal Energy Analysis (LC-PAT)

1987 ◽  
Vol 32 (4) ◽  
pp. 12405J ◽  
Author(s):  
Carl M. Selavka ◽  
Richard E. Tontarski ◽  
Richard A. Strobel
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.


2005 ◽  
Vol 88 (2) ◽  
pp. 592-594 ◽  
Author(s):  
Hardy J Chou

Abstract A liquid chromatography (LC) method using a thermal energy analyzer (TEA) is described for the determination of diethanolamine (DEA) in shampoo products containing fatty acid diethanolamides. DEA was converted to N-nitrosodiethanolamine (NDELA) by dissolving a portion of the product in 6M acetic acid and mixing with sodium nitrite for 1 h at room temperature. The reaction mixture was dried, dissolved in acetone, and analyzed for NDELA by LC-TEA. The recovery of DEA from 2 shampoo products at fortification levels of 25, 250, and 1000 ppm ranged from 70 to 105%. Twenty shampoo products were analyzed by this method, and 19 were found to contain DEA at levels ranging from 140 to 15 200 ppm.


1977 ◽  
Vol 11 (6) ◽  
pp. 581-584 ◽  
Author(s):  
David H. Fine ◽  
David P. Rounbehler ◽  
Anna Rounbehler ◽  
Arlene Silvergleid ◽  
Eugene Sawicki ◽  
...  

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

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