HPLC/ECD 同时测定生物样品中的组织胺和去甲肾上腺素

目的：建立了高效液相色谱法（ＨＰＬＣ）配合电化学检测器（ＥＣＤ）同时分析组织和体液中的组织胺（Ｈｉｓ）和去甲肾上腺素（ＮＡ）的方法。方法：用邻苯二甲醛（ＯＰＡ）和２ 巯基乙醇（２－ＭＥ）进行柱前衍生，衍生产物在离子对试剂辛基磺酸钠的作用下，采用ＰａｔｉｓｉｌＯＤＳ柱，乙酸等试剂组成缓冲溶液与乙腈按７∶３配成流动相，３ 甲基组织胺（３ Ｍ Ｈｉｓ）为内标，检测器电位０．７Ｖ，结果：用该方法对小鼠心脏组织和血液中的Ｈｉｓ和ＮＡ进行同时测定，得到了满意的分离和检测结果，最低检测量约为１５ｐｇ（Ｓ／Ｎ＝３）。结论：这个研究提示，用一些特殊试剂与样品产生衍生物，是得到满意的分离结果而不影响灵敏度的途径。

Simultaneous Analysis Histamine and Noradrenaline in Biologic Sample by HPLC/ECD

Objective: This paper reports that a reversed phase high performance liquid chromatographic(HPLC) method had been established for the simultaneous separation and quantitative determination of histamine(His)and noradrenaline(NA).Methods: The method is simple and reliable.The isoindole products formed by precolume derivatization of His and NA with o phthalaldehyde(OPA) and 2 mercaptoethanol(2 ME),the analysis was carried out with Patisil ODS column,acetate buffer(pH=4.90) acetonitrile(7∶3) as mobile phase and 3 methylhistamine(3 M His) as internal standard.The detector potential was+0.7V for both compounds to keep background noise minimal.Results: Yielded a linear relationship of detection between the electrochemical signal and the compound content,A minimum detectable limit of 15 pg(S/N=3).An example of a practical application of the method to the determination of His and NA in rat cardiac tissus or humour is presented.Conclusion: The study suggests that derivatization of compounds with some special agents resultion in electrochemically active derivatives,may also be an approach sometimes required toachieve satisfactory separation without sacrificing detection sensitivity