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Das Thiadiazol (I) reagiert mit den Phenacylbromiden (II) zu den Thiadiazol‐phenacylsulfiden (III); diese gehen mit Polyphosphorsäure in die heterocyclischen Ammoniumsalze (IV) über.

A procedure was developed for the determination of the analgesic components of Spasmomigraine® tablets, which are ergotamine (I), propyphenazone (II), caffeine (III), camylofin (IV), and mecloxamine (V). They were subjected to high-performance liquid chromatography on a column (300 × 3.9 mm, 10 μm particle size) packed with μ-Bondapak C18. Separations were achieved with the mobile phase methanol–water–triethylamine (60 + 40 + 0.1, v/v/v) flowing at a rate of 1.5 mL/min, and quantitative determination was performed at 254 nm at ambient temperature for I–III; acetonitrile–25 mM KH2PO4–acetic acid (45 + 55 + 0.2, v/v/v), flowing at a rate of 1.5 mL/min and detection at 234 nm at ambient temperature, was used for IV and V. Methyl paraben was used as an internal standard. The detection limits were 0.35 (I), 5.0 (II), 1.5 (III), 3.0 (IV), and 2.0 g/mL (V). The method was accurate (mean recovery 98 ± 2%, n = 4) and precise (coefficient of variation <5%, n = 5). The proposed method is rapid and sensitive and, therefore, suitable for the routine control of these ingredients in multicomponent dosage forms.