High temperature purge and trap procedure for determining seven volatile N-nitrosamines in animal feed, using gas chromatography/thermal energy analyzer.
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.
D000821:Animal Feed / Q000032:analysis*; D002849:Chromatography, Gas / Q000295:instrumentation / Q000379:methods; D004052:Diethylnitrosamine / Q000032:analysis; D004128:Dimethylnitrosamine / Q000032:analysis; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D006358:Hot Temperature; D009242:N-Nitrosopyrrolidine / Q000032:analysis; D009602:Nitrosamines / Q000032:analysis*
D009602:Nitrosamines; C013161:N-nitroso(di-n-propyl)amine; D004052:Diethylnitrosamine; D004128:Dimethylnitrosamine; D009242:N-Nitrosopyrrolidine