Screening Procedure for Detection of Volatile AT-Nitrosamines in Cooked Bacon by One-Trap Mineral Oil Vacuum Distillation and Thermal Energy Analyzer

1982 ◽  
Vol 65 (6) ◽  
pp. 1316-1318 ◽  
Author(s):  
Earl L Greenfield ◽  
G A Vasco ◽  
L Legette ◽  
Anthony Malanoski
Keyword(s):  
Liquid Nitrogen ◽  
Thermal Energy ◽  
Vacuum Distillation ◽  
Methylene Chloride ◽  
Mineral Oil ◽  
Rapid Screening ◽  
Screening Procedure ◽  
Energy Analyzer ◽  
Liquid Chromatograph

Abstract A rapid screening procedure for the detection of volatile N-nitrosamines in fried bacon has been developed for the regulatory monitoring of bacon. This procedure uses vacuum mineral oil distillation of an alkaline sample. The distillate is collected in a prewet trap immersed in liquid nitrogen. After thawing, the distillate is transferred to a separator. The trap is rinsed with methylene chloride which is then used to extract the nitrosamines. The methylene chloride is dried with Na2S04 and concentrated. A gas-liquid chromatograph coupled to a thermal energy analyzer is used to identify and quantitate the nitrosamines. Recoveries of 7 volatile N-nitrosamines added to 25 g fried bacon at the 10 ppb level (μg/kg) ranged from 78 to 92%.

Comparison of Three Methods for Determination of /V-Nitrosopyrrolidine in Fried Dry-Cured and Pump-Cured Bacon

1988 ◽  
Vol 71 (3) ◽  
pp. 504-508
Author(s):  
Anthony J Malanoski ◽  
Wertice J Smith ◽  
Thomas Phillipo
Keyword(s):  
Low Temperature ◽  
Thermal Energy ◽  
Validation Studies ◽  
Vacuum Distillation ◽  
Mineral Oil ◽  
Energy Analyzer ◽  
Coefficients Of Variation ◽  
The Individual

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

Mineral Oil Vacuum Distillation Method for Nitrosamines in Fried Bacon, with Thermal Energy Analyzer: Collaborative Study

1982 ◽  
Vol 65 (6) ◽  
pp. 1319-1332
Author(s):  
Earl L Greenfield ◽  
Wertice J Smith ◽  
Anthony J Malanoski ◽  
◽  
M Benson ◽  
...  
Keyword(s):  
Thermal Energy ◽  
Vacuum Distillation ◽  
Collaborative Study ◽  
Mineral Oil ◽  
Distillation Method ◽  
Energy Analyzer ◽  
Coefficients Of Variation

Abstract Nine laboratories participated in a collaborative study of a method for determining 6 nitrosamines, dimethylnitrosamine, diethylnitrosamine, dibutylnitrosamine, nitrosopiperidine, nitrosopyrrolidine, and nitrosomorpholine, in the 5-17 ppb range. The coefficients of variation for repeatability were 10.8, 8.5,10.4, 8.5, 8.7, and 7.8% with corresponding coefficients of variation for reproducibility of 16.4, 12.0,13.6,10.8,11.2, and 10.3% and recoveries of 89.6, 91.6, 84.7, 90.0, 89.6, and 88.1%, respectively. The method was adopted official first action.

Determination of /V-Nitrosodiethanolamine in Dinoseb Formulations by Mass Spectrometry and Thermal Energy Analyzer Detection

1987 ◽  
Vol 70 (5) ◽  
pp. 792-796
Author(s):  
Yuk Y Wigfield ◽  
Narine P Gurprasad ◽  
Monique Lanouette ◽  
Sharon Ripley
Keyword(s):  
Thermal Energy ◽  
Methylene Chloride ◽  
Limit Of Detection ◽  
Solvent System ◽  
Energy Analyzer ◽  
Liquid Chromatograph ◽  
Anion Exchange Column ◽  
Exchange Column ◽  
Cation Exchange Column ◽  
In Series

Abstract A new method is described to determine trace quantities of A'-nitrosodiethanolamine (NDE1A) in aqueous diethanolamine (DE1A) formulations and in oil solutions of dinoseb. A formate anion-exchange column is used in series with a cation-exchange column if there is DE1A in the formulation. The eluate is then passed through a Clin Elur8 column. Depending on the concentration of NDE1A in the sample, a packed silica-gel column is used to purify the extract further. This extract is analyzed on a liquid chromatograph coupled with a thermal energy analyzer (LC/TEA), using a mixture of methanol- hexane-methylene chloride containing 0.1% acetic acid (8 + 56 + 35) as the mobile phase. This solvent system gives good separation of NDE1A from trace quantities of dinoseb remaining in the extract. The NDE1A is also converted to the trimethylsilyl derivative and analyzed by gas chromatograph coupled with a mass spectrometer (GC/MS). Analyses of 11 commercial samples of dinoseb diethanolamine salt showed NDE1A levels of 116-2409 ppm expressed relative to the weight of dinoseb. In contrast, analyses of 2 samples of organic solutions of technical dinoseb showed NDE1A levels to be nondetectable and 0.3 ppm, respectively. Limit of detection by LC/ TEA is 6.5 ng (0.5 ppm), and by GC/MS it is 0.02 ng (0.15 ppm). Recoveries from samples spiked at 0.514-1664 ppm range from 92.2 to 105.2%

Dry Column-Thermal Energy Analyzer Method for Determining N-Nitrosopyrrolidine in Fried Bacon: Collaborative Study

1984 ◽  
Vol 67 (3) ◽  
pp. 521-525
Author(s):  
Walter Fiddler ◽  
John W Pensabene ◽  
Robert A Gates ◽  
John G Phillips ◽  
◽  
...  
Keyword(s):  
Thermal Energy ◽  
Collaborative Study ◽  
Internal Standard ◽  
Mineral Oil ◽  
Energy Analyzer ◽  
High Group ◽  
Average Recovery ◽  
Column Method ◽  
Coefficients Of Variation ◽  
Repeatability And Reproducibility

Abstract A dry column method for isolating N-nitrosopyrrolidine (NPYR) from fried, cure-pumped bacon and detection by gas chromatography-thermal energy analyzer (TEA) was studied collaboratively. Testing the results obtained from 11 collaborators for homogeneous variances among samples resulted in splitting the nonzero samples into 2 groups of sample levels, each with similar variances. Outlying results were identified by AOAC-recommended procedures, and laboratories having outliers within a group were excluded. Results from the 9 collaborators remaining in the low group yielded coefficients of variation (CV) of 6.00% and 7.47% for repeatability and reproducibility, respectively, and the 8 collaborators remaining in the high group yielded CV values of 5.64% and 13.72%, respectively. An 85.2% overall average recovery of the N-nitrosoazetidine internal standard was obtained with an average laboratory CV of 10.5%. The method has been adopted official first action as an alternative to the mineral oil distillation-TEA screening procedure.

Quantitation of the Nitrosamine 2-EthylhexyI-4-(N-Methyl-N-Nitrosoamino) Benzoate (NPABAO) in Sunscreen Products

1991 ◽  
Vol 74 (5) ◽  
pp. 766-771 ◽  
Author(s):  
Thomas A Meyer ◽  
Jimmy B Powell
Keyword(s):  
Thermal Energy ◽  
False Positive ◽  
Mobile Phase ◽  
Commercial Product ◽  
Energy Analyzer ◽  
Accurate Analysis ◽  
Liquid Chromatograph ◽  
Commercial Products ◽  
Minimum Detectable Limit ◽  
Sunscreen Products

Abstract We have devised a method to quantitate the nitrosamine, 2- ethylhexyM-(N-methyl-N-nitrosoamino) benzoate (NPABAO), In commercial products containing the sunscreen ingredient, Padimate 0. The method involves a minimum of cleanup steps to afford a nonaqueous extract from product emulsions suitable for analysis by a liquid chromatograph Interfaced to a thermal energy analyzer (LC/TEA). The method Is applicable to lotions, creams, and gels. Oils are normally soluble In the mobile phase and can be analyzed directly on the LC/TEA without additional cleanup procedures. The method has a minimum detectable limit of about 30 ppb and yields > 80% recovery. It is highly reproducible and generates no NPABAO artifactually prior to quantitation on the LC/TEA Application of the method to 22 different commercial product formulas disclosed that the level of NPABAO in each of the products Is below 250 ppb, with 18 of the products containing less than 100 ppb. Of interest was the observation that musk ketone, a common fragrance constituent, produces a false-positive TEA response that can Interfere with accurate analysis of NPABAO content In typical commercial products

Automatic liquid nitrogen controller for the thermal energy analyzer cold bath

1981 ◽  
Vol 53 (12) ◽  
pp. 1961-1962 ◽  
Author(s):  
James L. Owens ◽  
Oswald E. Kinast
Keyword(s):  
Liquid Nitrogen ◽  
Thermal Energy ◽  
Energy Analyzer ◽  
Cold Bath

High Temperature Purge and Trap Procedure for Determining Seven Volatile N-Nitrosamines in Animal Feed, Using Gas Chromatography/Thermal Energy Analyzer

1984 ◽  
Vol 67 (3) ◽  
pp. 557-562
Author(s):  
Stanley M Billedeau ◽  
Harold C Thompson ◽  
Eugene B Hansen ◽  
Barbara J Miller
Keyword(s):  
Gas Chromatography ◽  
High Temperature ◽  
Thermal Energy ◽  
Animal Feed ◽  
Mineral Oil ◽  
Nitroso Compounds ◽  
Energy Analyzer ◽  
Purge And Trap ◽  
Multiple Sample ◽  
Feed Samples

Abstract A rapid and sensitive procedure is described for determining 4 N- nitrosodialkylamines (dimethyl, diethyl, dipropyl, and dibutyl) and the N-nitroso analogs of piperidine, pyrrolidine, and morpholine in animal feed. The volatile N-nitrosamines were isolated by using a modified high temperature purge and trap apparatus designed for multiple sample cleanup. The feed sample was mixed with mineral oil and a nitrosation inhibitor, and the N-nitrosamines were purged onto a ThermoSorb/N cartridge, eluted with acetone–dichloromethane (1 + 1), and determined by gas chromatography, using a thermal energy analyzer. The effects of purge rate, purge time, and temperature on recovery are discussed. Feed samples spiked with 10, 50, and 200 ppb of the 7 N-nitroso compounds yielded recoveries ranging from 70 to 97%, with precision ranging from 1.3 to 5.4% and minimum detectable levels in the low parts-per-billion range.

Rapid Gas Chromatographic Method for Determining Ethyl Carbamate in Alcoholic Beverages with Thermal Energy Analyzer Detection

1988 ◽  
Vol 71 (3) ◽  
pp. 509-511
Author(s):  
Canas Benjamin J ◽  
Donald C HaVery ◽  
Frank L Joe
Keyword(s):  
Mass Spectrometry ◽  
Thermal Energy ◽  
Methylene Chloride ◽  
Limit Of Detection ◽  
Ethyl Carbamate ◽  
Alcoholic Beverages ◽  
Gas Chromatography Mass Spectrometry ◽  
Energy Analyzer ◽  
Elution Method ◽  
Gas Chromatographic Method

Abstract A rapid column elution method has been developed for the determination of ethyl carbamate (EC) in alcoholic beverages. The beverage is mixed with Celite and packed in a column containing deactivated alumina capped with a layer of sodium sulfate. EC is then eluted with methylene chloride. The method, using a gas chromatograph- thermal energy analyzer with a nitrogen converter for detection and quantitation of EC, has been applied to a variety of alcoholic beverages. Recoveries ± standard deviations of EC in wine and whisky fortified at the 20 and 133 µg/kg (ppb) levels averaged 87.3 ± 5.3 and 88.7 ± 3.6%, respectively. The method has a limit of detection of 1.5 ppb. Gas chromatography/mass spectrometry/ mass spectrometry was used to confirm the identity and quantitation of EC in selected beverage extracts.

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