Determination of the Analgesic Components of Spasmomigraine® Tablet by Liquid Chromatography with Ultraviolet Detection

Abstract

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.

Analysis of Ergot Alkaloids

“…For body tissues LC-MS methods are generally required to achieve the low detection limits necessary. With LC-UV ergotamine can be detected with other active ingredients using a C18 column with a mobile phase of methanol-water-triethylamine (60 + 40 + 0.1, v / v / v ) and detection at 254 nm [ 93 ].…”

Validated Stability Indicating Chromatographic Method for the Simultaneous Estimation of Camylofin with NSAID Drugs and a New Approach of Method Transfer from Classical HPLC to a Modern UPLC Instrument

“…Camylofin dihydrochloride (CMF) is an antimuscarinic drug which is used as an antispasmodic drug. Chemically, it is known as a 3-methylbutyl 2-(2-diethyl-aminoethylamino)-2-phenyl-acetate hydrochloride [1,2]. Diclofenac potassium (DCF) is a nonsteroidal anti-inflammatory drug (NSAID).…”

Determination of Camylofin Dihydrochloride and Nimesulide in Pharmaceutical Preparation by Gas Chromatography

“…The literature survey revealed that there is no method for the simultaneous determination of these compounds. There are other publications for determination of these compounds but in combination with other components by other analytical techniques like HPLC, spectrophotometry and colorimetric [4][5][6][7][8][9][10][11][12][13][14][15][16].There is a GC method reported for the analysis of Camylofin dihydrochloride [17]. There are, however, no publications for simultaneous determination of these drugs in such pharmaceutical preparation.…”