一种通过梯度高效液相色谱法测定美法仑及其相关杂质含量的稳定性指示方法。
A stability-indicating method for the determination of melphalan and related impurity content by gradient HPLC.
作者信息
Brightman K, Finlay G, Jarvis I, Knowlton T, Manktelow C T
机构信息
Glaxo Wellcome Operations, Dartford, Kent, UK.
出版信息
J Pharm Biomed Anal. 1999 Jul;20(3):439-47. doi: 10.1016/s0731-7085(99)00011-4.
A robust gradient high performance liquid chromatographic (HPLC) procedure is described for the simultaneous determination of melphalan content and related impurities in melphalan drug substance. The sample solution is prepared in methanol and injected. A linear gradient from 5 to 60% acetonitrile in water containing 0.05% v/v acetic acid, 0.01% v/v triethylamine, and 0.05% w/v ammonium acetate is applied over 20 min. The chromatographic conditions are capable of separating and quantifying all impurities found in routine production batches of melphalan at above 0.1% area/area. The method has been fully validated and is linear over the column loading range of 0-3 microg of melphalan. All related impurities occurring in routine batches at above 0.1% area/area have been identified, and structures assigned. The method has been applied to melphalan samples stored under stressed conditions, and shown to be stability-indicating.
描述了一种稳健的梯度高效液相色谱（HPLC）方法，用于同时测定美法仑原料药中美法仑的含量及相关杂质。样品溶液用甲醇配制并进样。在20分钟内施加从5%到60%乙腈的线性梯度，流动相为含有0.05%（v/v）乙酸、0.01%（v/v）三乙胺和0.05%（w/v）乙酸铵的水溶液。该色谱条件能够分离和定量常规生产批次美法仑中含量高于0.1%（面积/面积）的所有杂质。该方法已得到充分验证，在0 - 3微克美法仑的柱负载范围内呈线性。已鉴定出常规批次中含量高于0.1%（面积/面积）的所有相关杂质，并确定了其结构。该方法已应用于在加速条件下储存的美法仑样品，并显示出具有稳定性指示作用。
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