Gazdag M, Mihályfi K, Kemenesné B P, Görög S
Acta Pharm Hung. 1997 Sep;67(5):169-74.
High-performance liquid chromatographic (HPLC) and capillary electrophoretic (CE) methods have been developed for the separation of 22 related peptides (potential and real impurities) from a new immunostimulant tetrapeptide derivative (thymocartin, Arg-Lys-Asp-Val) being under clinical examination. The described methods are suitable for the purity control of the bulk drug material. In the course of the reversed-phase ion-pair HPLC separations C-18 columns (Hypersil BDS and Ultrasphere IP) were used. In the case of using sodium hexanesulphonate as the ion-pairing reagent, the eluent contained phosphate buffer (pH = 3) and 32% v/v methanol, while in another method a gradient system with a sodium perchlorate solution (pH = 2 set by perchloric acid) and acetonitrile was applied. The optimum separation in the CE investigations was achieved at pH = 3 using triethylammonium phosphate buffer and 10% v/v acetonitrile as the organic modifier.
已开发出高效液相色谱（HPLC）和毛细管电泳（CE）方法，用于从一种正在进行临床研究的新型免疫刺激四肽衍生物（胸腺卡汀，精氨酸-赖氨酸-天冬氨酸-缬氨酸）中分离出22种相关肽（潜在杂质和实际杂质）。所述方法适用于原料药的纯度控制。在反相离子对HPLC分离过程中，使用了C-18柱（Hypersil BDS和Ultrasphere IP）。在使用己烷磺酸钠作为离子对试剂的情况下，洗脱液含有磷酸盐缓冲液（pH = 3）和32% v/v甲醇，而在另一种方法中，应用了含有高氯酸钠溶液（由高氯酸调节pH = 2）和乙腈的梯度系统。在CE研究中，使用磷酸三乙铵缓冲液和10% v/v乙腈作为有机改性剂，在pH = 3时实现了最佳分离。
