Bock U E, Waser P G
J Chromatogr. 1981 Sep 4;213(3):413-28. doi: 10.1016/s0021-9673(00)80493-8.
The catecholamines dopamine and noradrenaline were converted into the stable pentafluorobenzoyl (PFB) derivatives for their specific and quantitative gas chromatographic (GC) assay. This allowed their detection in the picogram range using an electron-capture detector. Acylation was performed with pentafluorbenzoyl chloride in the presence of pyridine and with acetonitrile as solvent. The structures of the PFB-catecholamines were confirmed by GC-mass spectrometry. A good separation was obtained on 5% OV-17 at 265 degrees C. The high adsorption activity of the PFB-catecholamines could be overcome by optimizing the reaction conditions and applying special GC precautions. Linearity of the method was demonstrated for 50- 500 ng of the catecholamines with detection at the picogram level. The application of the method to biological materials is demonstrated.
儿茶酚胺类物质多巴胺和去甲肾上腺素被转化为稳定的五氟苯甲酰(PFB)衍生物,用于其特异性和定量气相色谱(GC)分析。这使得使用电子捕获检测器能够在皮克范围内检测到它们。酰化反应在吡啶存在下用五氟苯甲酰氯进行,以乙腈作为溶剂。通过气相色谱-质谱联用仪确认了PFB-儿茶酚胺的结构。在265℃下使用5% OV-17可实现良好的分离。通过优化反应条件并采取特殊的气相色谱预防措施,可以克服PFB-儿茶酚胺的高吸附活性。该方法在50 - 500 ng儿茶酚胺范围内呈线性,检测限为皮克水平。证明了该方法在生物材料中的应用。