Rapid Dry Column Method for Determination of N-Nitrosopyrrolidine in Fried Bacon

Abstract

A rapid method has been developed for the determination of N-nitrosopyrrolidine (NPYR) in fried bacon at less than the 1 ppb level. Ground fried bacon is mixed with anhydrous sodium sulfate and Celite by using a glass mortar and pestle. This dry mixture is then added to a chromatographic column containing a layer of acid-Celite. The column is washed with pentane-dichloromethane, and the nitrosamines are eluted with pure dichloromethane. The eluate is concentrated, and the nitrosamines are quantitated by using a gas chromatograph interfaced with a thermal energy analyzer. Recovery of the nitrosamine internal standard, N-nitrosoazetidine, added at the 10 ppb level, was over 90%. The results obtained by this method are in good agreement with the mineral oil distillation procedure currently used in the FSIS monitoring program. Because 25 samples can be analyzed per day per person, this simple screening procedure offers advantages over other methods.

The determination of N-nitrosamines in food

“…Very similar techniques can be used for solid foods, typically cured meats. In the so‐called ‘dry column procedure’ cured meat is dispersed in the solid matrix of diatomaceous earth which is packed into a column and the N‐ nitrosamines eluted with solvent (Pensabene & Fiddler, 1982; Pensabene et al , 1982; Raoul et al , 1997; Yurchenko & Molder, 2007). Yurchenko (2006) studied these methods in detail using solvent mixtures and a range of SPE columns (Extrelut, Florisil, cyano, silica gel, aminopropyl, alumina, and an Extrelut–Florisil combination) for both extraction and clean up.…”

Effect of cesium-137 radiation on the formation of N-nitrosopyrrolidine in bacon

“…Reagents, A complete list of reagents needed for determining NPYR in fried bacon and its cooked-out fat was reported elsewhere (Pensabene and Fiddler, 1982;White et al, 1974). Bacon Processing.…”

Perchloric acid-Celite chromatographic technique for volatile N-nitrosamines

“…A thermal energy analyzer (TEA), Model TEA-502, manufactured by Thermo Electron Corp., interfaced with a Hewlett-Packard Model 5790A Series packed column gas chromatograph was used for separation and detection of the NAs. Specific conditions were as follows: column, 8 ft by 1/8 in o.d. stainless steel packed with 10% Carbowax 20M + 2% KOH on Chromosorb W AW, 80/100 mesh; programmed from 120 °C to 185 °C at 5.0 °C/min, final hold time 7.0 min, total run time 20.2 min; carrier gas, He, flow rate =* 12 mL/min; injector, glass lined, 250 °C; interface line, Vs in °-d. glass-lined stainless steel, 250 °C; TEA furnace, 525 °C; TEA cold trap, -151 °C; TEA detector pressure, =*1.6 torr.…”

“…To further purify the extract produced by this method, the technique © of acid-Celite chromatography has been used (7). In use for many years, it is still being used for DMN and IV-nitrosopyrrolidine (NPYR) in biological samples and food samples (8,9). However, attempts to use this column cleanup technique for other NAs such as diethylnitrosamine (DEN), din-propylnitrosamine (DPN), and IV-nitrosopiperidine (NPIP) have proved to be ineffective.…”

“…native schemes based on preferential accumulation at ordinary and modified electrodes have been proposed (1)(2)(3)(4)(5)(6)(7)(8)(9)(10)(11)(12)(13)(14). These new preconcentration/voltammetric methods offer both signal enhancement and a high degree of selectivity, compared to conventional (solution-phase) voltammetry.…”