Sensitive ergotamine determination in pharmaceuticals and biological samples using cloud point preconcentration and spectrofluorimetric detection.

A new cloud point extraction (CPE) method for ergotamine analysis using fluorimetric detection is described. Ergotamine from an aqueous solution was preconcentrated into a smaller surfactant-rich phase using nonionic surfactant polyoxyethylene(7.5)nonylphenylether (PONPE 7.5). Differently from the conventional CPE procedure in which the resulting surfactant-rich phase is diluted by a fluidificant before its analysis, in this method the fluorescence measurements were carried out directly onto the undiluted surfactant-rich phase. The high viscosity provided by the undiluted surfactant rich phase greatly improved the fluorescence emission of ergotamine, leading to a total enhancement factor of 1325. This spectral advantage plus the preconcentration factor achieved, contributed to the method sensitivity allowing the ergotamine determination at trace level concentration. Under optimal experimental conditions, a linear calibration curve was obtained from 3.81×10(-7) to 1.10μgmL(-1), with detection and quantification limits of 0.11 and 0.38pgmL(-1), respectively. The accuracy and versatility of the present methodology were proved by analyzing ergotamine in real samples of different natures such as pharmaceuticals, urine and saliva. Copyright © 2013 Elsevier B.V. All rights reserved.

Citation

Chien C Wang, Liliana P Fernández, María Roxana Gómez. Sensitive ergotamine determination in pharmaceuticals and biological samples using cloud point preconcentration and spectrofluorimetric detection. Analytica chimica acta. 2013 Mar 20;768:90-5

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PMID: 23473254

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