Mita H, Yasueda H, Shida T
J Chromatogr. 1980 Feb 8;181(2):153-9. doi: 10.1016/s0378-4347(00)81600-x.
A mass fragmentographic method for the quantitative analysis of histamine in the supernatant from antigen-challenged leukocytes, whole blood, and urine is described. Histamine labeled with two 15N atoms was synthesized and added to the sample as an internal standard. N alpha-Heptafluorobutyryl-N tau-ethoxycarbonylhistamine was prepared for mass fragmentographic analysis and the molecular ions at m/z 379 and 381 were used for monitoring histamine and 15N2-labeled histamine, respectively. The quantitation limit of histamine was 2 ng by this method. The experimental error of the method was less than 7% at the level of 5 ng in the supernatant from antigen-challenged leukocytes. The value obtained by this method correlated well with that from radioisotopic enzymatic assay (r=0.990).
本文描述了一种用于定量分析抗原刺激白细胞、全血和尿液上清液中组胺的质量碎片分析法。合成了用两个(^{15}N)原子标记的组胺，并将其作为内标添加到样品中。制备了(Nα)-七氟丁酰基-(Nτ)-乙氧羰基组胺用于质量碎片分析，分别使用质荷比为(379)和(381)的分子离子监测组胺和(^{15}N_2)标记的组胺。该方法对组胺的定量限为(2 ng)。在抗原刺激白细胞上清液中(5 ng)水平下，该方法的实验误差小于(7%)。该方法获得的值与放射性同位素酶法获得的值相关性良好（(r = 0.990)）。
