Petruczynik Anna
Medical University of Lublin, Department of Inorganic Chemistry, Staszica 6, 20-081 Lublin, Poland.
J AOAC Int. 2011 Jan-Feb;94(1):77-89.
Retention parameters of alkaloid standards were determined on different stationary phases, i.e., octadecyl silica, base-deactivated octadecyl silica, cyanopropyl silica, preconditioned cyanopropyl silica, and pentafluorophenyl, using different aqueous eluant systems: acetonitrile-water mixtures; buffered aqueous mobile phases at pH 3 or 7.8; and aqueous eluants containing ion-pairing reagents (octane-1-sulfonic acid sodium salt and pentane-1-sulfonic acid sodium salt) or silanol blockers (tetrabutyl ammonium chloride and diethylamine). Improved peak symmetry and separation selectivity for basic solutes was observed when basic buffer, ion-pairing reagents, and, especially, silanol blockers as mobile phase additives were applied. The best separation selectivity and most symmetric peaks for the investigated alkaloids were obtained in systems containing diethylamine in the mobile phase. The influence of acetonitrile concentration and kind and concentration of ion-pairing reagents or silanol blockers on retention, peak symmetry, and system efficiency was also examined. The most efficient and selective systems were used for separation of the investigated alkaloids and analysis of Fumaria officinalis and Glaucium flavum plant extracts.
使用不同的水性洗脱剂系统，在不同的固定相上测定生物碱标准品的保留参数，这些固定相包括十八烷基硅胶、碱钝化十八烷基硅胶、氰丙基硅胶、预处理氰丙基硅胶和五氟苯基，水性洗脱剂系统如下：乙腈 - 水混合物；pH为3或7.8的缓冲水性流动相；以及含有离子对试剂（辛烷 - 1 - 磺酸钠盐和戊烷 - 1 - 磺酸钠盐）或硅醇封端剂（四丁基氯化铵和二乙胺）的水性洗脱剂。当使用碱性缓冲液、离子对试剂，尤其是作为流动相添加剂的硅醇封端剂时，观察到碱性溶质的峰对称性和分离选择性得到改善。在所研究的生物碱中，在流动相中含有二乙胺的系统中获得了最佳的分离选择性和最对称的峰。还研究了乙腈浓度、离子对试剂或硅醇封端剂的种类和浓度对保留、峰对称性和系统效率的影响。使用最有效和选择性的系统分离所研究的生物碱，并分析紫堇和黄罂粟植物提取物。
