Determination of volatile N-nitrosamines in irradiated fermented sausage by gas chromatography coupled to a thermal energy analyzer

2004 ◽  
Vol 1054 (1-2) ◽  
pp. 403-407 ◽  
Author(s):  
M BYUN ◽  
H AHN ◽  
J KIM ◽  
J LEE ◽  
H YOOK ◽  
...  
1988 ◽  
Vol 71 (2) ◽  
pp. 333-336
Author(s):  
Dave Wotherspoon ◽  
Ralph Hindle

Abstract A quick method for determining /V-nitrosodipropylamine (NDPA) levels in trifluralin emulsifiable concentrate formulations is described. At least 18 samples can be analyzed at one time in a minimum of fumehood space, with up to 90% savings on solvents and materials. A sample aliquot is mixed with a solution containing nitrosamine recovery standards, and nitrosamines are separated by minicolumn cleanup. Internal standard is added directly to the eluate containing the nitrosamines, and levels are determined by gas chromatography with thermal energy analyzer. Recoveries of spiked nitrosamines ranged from 98 to 102%. Coefficients of variation for samples containing 0.5 ppm NDPA are 13%. Minimum detectable limit, calculated as 3 times the noise, is 0.06 ppm. Comparison with the method formerly used by this laboratory shows no significant difference in the analytical results at 95% confidence limits, and control experiments were performed to ensure that there was no artifact formation of NDPA.


1985 ◽  
Vol 68 (1) ◽  
pp. 41-43
Author(s):  
Holly D Ross ◽  
Joseph H Hotchkiss

Abstract The method described for determining N03~ in dried foods is based on extraction of N03~ from the sample with subsequent nitration of benzene. The nitrobenzene is extracted with ethyl acetate, analyzed by using a gas chromatograph-thermal energy analyzer (GC-TEA), and quantitated against a nitrobenzene standard. Sensitivity is 100-200 μg/ kg. Coefficients of variation for analyses of dried foods were 3-13%. Recovery of N03" from nonfat dry milk spiked at 10 mg/kg averaged 100%.


1986 ◽  
Vol 2 (6) ◽  
pp. 577-580 ◽  
Author(s):  
Masahiro TAKEUCHI ◽  
Kazuko MIZUISHI ◽  
Hideo YAMANOBE ◽  
Yohya WATANABE

1987 ◽  
Vol 70 (3) ◽  
pp. 434-438
Author(s):  
Nrisinha P Sen ◽  
Stephen W Seaman ◽  
Santosh C Kushwaha

Abstract A method is described for determining volatile nitrosamines in baby bottle rubber nipples and pacifiers. The method consists of (a) overnight soaking of the sample with dichloromethane in the presence of propyl gallate, an inhibitor for artifactual formation of nitrosamines; (b) extraction with dichloromethane using an ambient temperature column procedure; (c) distillation from aqueous alkali; (d) extraction of the aqueous distillate with dichloromethane and concentration of the extract using a Kuderna-Danish concentrator; and (e) final analysis by gas chromatography with detection by thermal energy analyzer. Major improvements over other published methods include a simpler extraction, a more efficient distillation and concentration to minimize losses, and incorporation of propyl gallate inhibitor as well as of a test to detect unsuitable dichloromethane solvent that otherwise might lead to artifactual formation. The method is highly accurate (~90% recovery) and precise (av. CV = 4.7% at >9 ppb levels) and is applicable to determination of nitrosamines in both rubber- and plastic-based products.


1994 ◽  
Vol 77 (1) ◽  
pp. 64-67 ◽  
Author(s):  
Randolph H Dyer

Abstract A gas chromatographic (GC) procedure for the determination of ethyl carbamate (urethane) in distilled spirits and wines using a thermal energy analyzer (TEA) system was collaboratively studied by 5 laboratories. Distilled spirits such as whiskey, brandy, gin, rum, and vodka containing low solids can be injected directly into the GC system without extraction. Liqueurs require extraction. Wine, beer, sake, and similar samples containing significant solids or other interferences are extracted prior to injection. The sample is analyzed by GC/TEA operating in the nitrogen mode with capillary column capability (30 m × 0.53 mm) and automatic injection. Helium is the carrier gas. The GC system is calibrated with a 100 ppb standard, followed by the samples. The concentration of ethyl carbamate is determined by multiplying peak area ratios by the concentration of the standard. For the distilled spirits, the recovery averaged 92%. The within-labora-tory repeatability (RSDr) ranged from 4.3 to 12.5%, with overall average of 8.0%, and reproducibility (RSDR) varied from 4.8 to 22.0%, with an overall average of 17.4%. For the wines, the recovery averaged 85%, and the RSDr ranged from 8.9 to 42.8%, with an overall average of 34.4%. The method has been adopted first action by AOAC INTERNATIONAL.


1983 ◽  
Vol 55 (6) ◽  
pp. 889-892 ◽  
Author(s):  
John H. Phillips ◽  
Robert J. Coraor ◽  
Steven R. Prescott

1975 ◽  
Vol 47 (7) ◽  
pp. 1188-1191 ◽  
Author(s):  
David H. Fine ◽  
Firooz. Rufeh ◽  
David. Lieb ◽  
David P. Rounbehler

1988 ◽  
Vol 71 (3) ◽  
pp. 504-508
Author(s):  
Anthony J Malanoski ◽  
Wertice J Smith ◽  
Thomas Phillipo

Abstract Three methods, the mineral oil distillation (MOD), the dry column (DC), and a low temperature vacuum distillation (LTVD), for the determination of iV-nitrosopyrrolidine in dry-cured and pump-cured bacon were compared. Each method uses the thermal energy analyzer for the determinative step. The coefficients of variation for repeatability were 10.3% (MOD), 7.2% (DC), and 9.1% (LTVD) for the dry-cured bacon study and 8.7% (MOD), 8.5% (DC), and 7.1% (LTVD) for the pump-cured bacon study. The pooled coefficients of variation for between-method reproducibility were 11.8% for the drycured bacon and 10.8% for the pump-cured bacon. The pooled coefficients of variation for repeatability were 9.0% for the dry-cured bacon and 8.2% for the pump-cured bacon. These values compare favorably with the values from previous collaborative or validation studies of the individual methods, and the methods can be considered to be equivalent


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.


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