Bethke H, Delz B, Stich K
J Chromatogr. 1976 Jul 21;123(1):193-203. doi: 10.1016/s0021-9673(00)81115-2.
A reversed-phase system of high-pressure liquid chromatography with solvent gradient is described for testing the purity of ergotamine as an active substance and for checking its concentration in pharmaceutical preparations. Because of its good resolution, this system can be used not only for the selective assay of ergotamine but also for the identification and quantitative determination, in the same chromatogram, of seven known isomerization and hydrolysis breakdown products. Simultaneous detection at two different UV wavelengths also makes it possible to measure further breakdown products formed by addition at the 9,10 double bond (lumi-compounds). The advantages of the system lie in the determination of all of the products within ca. 20 min, direct injection of low-dosage injection solutions and sensitive detection of polar breakdown products. The system is reproducible with regard to retention times and quantitative determination. It is suitable as a quality-control method for the routine determination of the content and purity of ergotamine preparations.
描述了一种带有溶剂梯度的反相高压液相色谱系统，用于检测作为活性物质的麦角胺的纯度，并检查其在药物制剂中的浓度。由于其良好的分离度，该系统不仅可用于麦角胺的选择性测定，还可用于在同一色谱图中鉴定和定量测定七种已知的异构化和水解分解产物。在两个不同的紫外波长下同时检测，还能够测量由9,10双键加成形成的进一步分解产物（发光化合物）。该系统的优点在于能在约20分钟内测定所有产物，可直接进样低剂量注射溶液，并且能灵敏检测极性分解产物。该系统在保留时间和定量测定方面具有可重复性。它适合作为一种质量控制方法，用于常规测定麦角胺制剂的含量和纯度。
