A method for the determination of total N-nitroso compounds (NOC) by chemical denitrosation and subsequent chemiluminescence detection of evolved NO is described. Denitrosation was accomplished with CuCl in HCl at 70 degrees C. The detection limit for N-nitrosoproline (NPRO) was 1 pmol. NO formation from NPRO was linear (R(2) = 0.999) from 4 pmol to 2 nmol. Among the possible interfering compounds tested, only S-nitroso compounds contribute any significant interference. This method had several advantages over other similar methods: (1) A commercially available one-piece reaction vessel and a NO analyzer with software were used. (2) NO release occurred rapidly and was easily measured and quantified. (3) Compared to HBr or HI, CuCl was more convenient to work with and safe. (4) CuCl was suitable for samples in aqueous and most organic solvents. The application of this method to food, personal care products, and human body fluids demonstrates its utility.

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Thermal Elimination of Phenyl Isocyanate from 3 (R1 = Ph; R8 = CH3).-The primary adduct 3 (R1 = Ph; R2 = CHa) (0.42 g, 0.001 mol) was heated for 20 min above its melting point at about 0.5 mm.After cooling and trituration with ether, the product crystallized from benzene-cyclohexane as colorless prisms of dimethyl 6-methyl-2-oxo-l-phenyIpyridine-4,5-dicarboxylate (4, Rl = Ph; R2 = CH3): 90%; mp [155][156][157][158] ir (KBr) 3001, 2950 (CH), 1740, 1725, 1660 cm-1 (CO); X™,0H 328 nm (log e 3.74), 251 (4.08), 203 (4.68); nmr (CDC1S) 7.90 (s, 3, C6 CHS), 6.17 (s, 3, C4 COOCH3), 6.10 (s, 3, C5 COOCH3), 3.09 (s, 1, Ha), 2.32-2.90 (m, 10, aromatic); mass spectrum, +•, rale (rel intensity) 301 (100).

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