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目的:对米拉贝隆主要降解产物的结构进行鉴定。方法:应用LC-MS对米拉贝隆4个主要降解产物进行了鉴定,色谱柱为COSMOSIL C_(18)-MS-II(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%三氟醋酸水溶液,梯度洗脱,流速1.0 m L·min~(-1);利用高效液相色谱对4个降解产物进行了制备,并进一步利用核磁共振技术和旋光仪进行了结构确证。结果:4个主要降解产物分别为米拉贝隆的酰胺基水解物:2-氨基-4-噻唑乙酸、2-氨基-4-甲基噻唑、(R)-2-[(4-氨基苯基乙基)氨基]-1-苯基乙醇,以及1个肟衍生物:(Z)-苯甲醛肟。结论:本法为米拉贝隆生产及贮存条件的选择提供了科学依据。
OBJECTIVE: To identify the structure of the major degradation products of mirabelon. Methods: The four major degradation products of Mirabellone were identified by LC-MS. The column was COSMOSIL C18-MS-II (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile 0.1% Fluoroacetic acid aqueous solution with gradient elution at a flow rate of 1.0 m L · min -1. Four degradation products were prepared by high performance liquid chromatography (HPLC) and further confirmed by NMR and Polarimeter. RESULTS: The four major degradation products were the amido hydrolyzates of milramycin respectively: 2-amino-4-thiazoleacetic acid, 2-amino-4-methylthiazole, Ethyl) amino] -1-phenylethanol, and 1 oxime derivative: (Z) -benzaldoxime. Conclusion: This Law provides a scientific basis for the selection of millafronin production and storage conditions.