Hartman P A, Stodola J D
Upjohn Company, Product Control-Analytical Development, Kalamazoo, MI 49001.
J Chromatogr. 1988 Jul 1;444:177-82. doi: 10.1016/s0021-9673(01)94020-8.
Separation of fertirelin acetate (FA) from process impurities, potential degradation products and related peptides including luteinizing hormone releasing hormone has been achieved by reversed-phase high-performance liquid chromatography (HPLC). A number of chromatographic conditions (column type, mobile phase composition, isocratic/gradient elution) and detection systems have been utilized to examine the bulk drug and formulation of FA. Examples of separations designed for potency and impurity determinations are described. Complete recovery of FA is obtained with an isocratic HPLC system. An external standard method is used to determine potency with a precision of less than 1% R.S.D. A gradient HPLC system is used to determine impurities with a precision of ca. 5-10% R.S.D. at the 1-2% impurity level. As little as ca. 0.1% (area%) of related peptides are detected at 214 nm.
通过反相高效液相色谱法（HPLC）实现了从工艺杂质、潜在降解产物以及包括促黄体激素释放激素在内的相关肽中分离醋酸促滤泡素（FA）。已采用多种色谱条件（柱类型、流动相组成、等度/梯度洗脱）和检测系统来检测FA的原料药和制剂。描述了为效价和杂质测定设计的分离示例。使用等度HPLC系统可实现FA的完全回收。采用外标法测定效价，精密度小于1%相对标准偏差（R.S.D.）。使用梯度HPLC系统测定杂质，在杂质水平为1 - 2%时，精密度约为5 - 10% R.S.D.。在214 nm处可检测到低至约0.1%（面积%）的相关肽。
