Janicot J L, Caude M, Rosset R
Laboratoire de Chimie Analytique de l'Ecole Supérieure de Physique et de Chimie de Paris, France.
J Chromatogr. 1988 Mar 25;437(2):351-64. doi: 10.1016/s0021-9673(00)90409-6.
The optimization of the separation of seven opium alkaloids by sub- and supercritical fluid chromatography (SFC) using packed columns and carbon dioxide as the primary mobile phase was studied. The influence of aminated polar modifiers on bare and aminopropyl-bonded silica was investigated. It was found that the presence of an amine in the mobile phase could enhance the retention of alkaloids on aminopropylsilica. Various separation schemes were possible depending on the type of analysis needed. An aminopropyl-bonded silica used with a carbon dioxide-methanol-triethylamine-water mixture (82.95:16.25:0.50:0.30, w/w) gave a very rapid separation (2 min). A bare silica with a carbon dioxide-methanol-methylamine-water mixture (83.37:16.25:0.15:0.23, w/w) gave longer analysis (10 min) but a higher resolution. This last procedure was applied to a poppy straw extract and to the determination of three alkaloids of interest after a peak purity study using a diode-array UV detector. For these alkaloids, SFC appears to be a promising technique for the routine analysis of opium alkaloids.
研究了使用填充柱并以二氧化碳作为主要流动相,通过亚临界和超临界流体色谱法(SFC)对七种鸦片生物碱进行分离的优化。研究了胺化极性改性剂对裸硅胶和氨丙基键合硅胶的影响。发现流动相中存在胺可增强生物碱在氨丙基硅胶上的保留。根据所需分析类型,可以采用各种分离方案。使用二氧化碳 - 甲醇 - 三乙胺 - 水混合物(82.95:16.25:0.50:0.30,w/w)的氨丙基键合硅胶实现了非常快速的分离(2分钟)。使用二氧化碳 - 甲醇 - 甲胺 - 水混合物(83.37:16.25:0.15:0.23,w/w)的裸硅胶分析时间更长(10分钟),但分辨率更高。在使用二极管阵列紫外检测器进行峰纯度研究后,最后一种方法应用于罂粟秸秆提取物以及三种目标生物碱的测定。对于这些生物碱,SFC似乎是用于鸦片生物碱常规分析的一种有前景的技术。