Bellec G, Cauvin J M, Salaun M C, Le Calvé K, Dréano Y, Gouérou H, Ménez J F, Berthou F
Laboratoires de Biochimie-Nutrition, Faculté de Médecine, Brest, France.
J Chromatogr A. 1996 Mar 8;727(1):83-92. doi: 10.1016/0021-9673(95)01073-4.
N-Nitrosamines eluted from reversed-phase HPLC were quantitatively photohydrolysed in a UV photoreactor in aqueous solution to give the nitrite ion which could be determined colorimetrically with the Griess reagent. The chromatographic behavior of N-nitroso compounds (including 19 volatile dialkyl and 7 non-volatile N-nitrosamines) was studied on three octadecylsilane columns. The capacity factor varies linearly with the number of carbons atom of the n-dialkyl chains. N-nitrosamines bearing di-n-alkyl chains with the same number of carbon atoms could be separated with a highly polar mobile phase. The yield of photohydrolysis depends upon pH and time of exposure under UV light. The response was shown to be linear in the 0-200 ng range with a limit of detection of 8 pmoles injected for N-dialkyl nitrosamines. This limit was 20 pmoles for N-nitrosamines bearing two phenyl groups. Although N-nitrosamines could be detected at 230 nm without post-column reaction, such a reaction enhances the specificity of detection in biological matrices such as gastric juice or alcoholic beverages.
从反相高效液相色谱中洗脱的N-亚硝胺在紫外光反应器中于水溶液中进行定量光水解，生成亚硝酸根离子，该离子可用格里斯试剂进行比色测定。在三根十八烷基硅烷柱上研究了N-亚硝基化合物（包括19种挥发性二烷基和7种非挥发性N-亚硝胺）的色谱行为。容量因子与正二烷基链的碳原子数呈线性变化。带有相同碳原子数的二正烷基链的N-亚硝胺可用高极性流动相分离。光水解产率取决于pH值和紫外光照射时间。结果表明，在0-200 ng范围内响应呈线性，对于二烷基亚硝胺，进样检测限为8皮摩尔。对于带有两个苯基的N-亚硝胺，该检测限为20皮摩尔。尽管无需柱后反应即可在230 nm处检测到N-亚硝胺，但这种反应可提高在生物基质（如胃液或酒精饮料）中的检测特异性。
