Mahy N, Gelpi E
J Chromatogr. 1977 Jan 11;130:237-42. doi: 10.1016/s0021-9673(00)89800-3.
A new, rapid and simple gas-liquid chromatographic method is described for the simultaneous determination of histamine, 1-methylhistamine, 4-imidazoleacetic acid and 1-methyl-4-imidazoleacetic acid. These compounds are derivatized at 60 degrees in one fast 30-min reaction with bis(trimethylsilyl)acetamide-trimethylchlorosilane and are then separated on OV-17. No previous methylation of the acids is needed. A complete profile of the four metabolites can be obtained in 8 min with baseline resolution, and there are no tailing effects. The quantitative response curves are linear in the nanogram range, with detection limits of the order of 10 ng for the acids and 100 ng for the amines. The structures of these new trimethylsilyl derivatives have been verified by combined gas-liquid chromatography-mass spectrometry.
本文描述了一种新的、快速且简单的气液色谱方法,用于同时测定组胺、1-甲基组胺、4-咪唑乙酸和1-甲基-4-咪唑乙酸。这些化合物在60℃下与双(三甲基硅基)乙酰胺-三甲基氯硅烷在一个快速的30分钟反应中进行衍生化,然后在OV-17上分离。无需对酸进行预先甲基化。在8分钟内即可获得四种代谢物的完整图谱,基线分离度良好,且无拖尾效应。定量响应曲线在纳克范围内呈线性,酸的检测限约为10纳克,胺的检测限约为100纳克。这些新的三甲基硅基衍生物的结构已通过气液色谱-质谱联用得到验证。