Tanaka A, Iijima M, Kikuchi Y, Hoshino Y, Nose N
Saitama Institute of Public Health, Japan.
J Chromatogr. 1989 Apr 19;466:307-17. doi: 10.1016/s0021-9673(01)84626-4.
The determination of nicotinamide as 3-cyanopyridine after dehydration by heptafluorobutyric anhydride (HFB) was performed by gas-liquid chromatography (GLC) with flame ionization detection (GLC-FID) and a column of 5% OV-17 on Chromosorb W AW DMCS at 130 degrees C. Determination was possible with 3-100 micrograms of the dehydrated reaction mixture. The procedure for determining nicotinamide in various meats and meat products involves direct analysis by GLC-FID without a clean-up stage; the detection limit is 5 ppm and the recovery ranged from 93.4 to 104.6% (average 98.0%). Various possible interferents in the samples did not interfere in the production or determination of 3-cyanopyridine. The procedure is suitable for routine use. The dehydrated derivative of nicotinamide was confirmed as 3-cyanopyridine by combined gas chromatography-mass spectrometry and infrared spectrometry.
通过七氟丁酸酐(HFB)脱水后,采用气相色谱法(GLC)及火焰离子化检测(GLC-FID),在130℃下使用涂有5%OV-17的Chromosorb W AW DMCS色谱柱对烟酰胺进行3-氰基吡啶的测定。3至100微克脱水反应混合物即可进行测定。测定各种肉类及肉制品中烟酰胺的方法是直接通过GLC-FID分析,无需净化步骤;检测限为5 ppm,回收率在93.4%至104.6%之间(平均98.0%)。样品中各种可能的干扰物不会干扰3-氰基吡啶的生成或测定。该方法适用于常规使用。烟酰胺的脱水衍生物经气相色谱-质谱联用和红外光谱确认为3-氰基吡啶。