SENSITIVE ERGOTAMINE DETERMINATION IN PHARMACEUTICALS AND BIOLOGICAL SAMPLES USING CLOUDS POINT PRECONCENTRATION AND SPECTROFLUORIMETRIC DETECTION

WANG, CHIEN CHUN; FERNANDEZ, LILIANA; GOMEZ, ROXANA A.

ANALYTICA CHIMICA ACTA

ELSEVIER SCIENCE BV

Lugar: Amsterdam; Año: 2013 vol. 768 p. 90 - 95

0003-2670

A new cloud point extraction (CPE) method for ergotamine analysis using fluorimetric detection isdescribed. Ergotamine from an aqueous solution was preconcentrated into a smaller surfactant-richphase using nonionic surfactant polyoxyethylene(7.5)nonylphenylether (PONPE 7.5). Differently fromthe conventional CPE procedure in which the resulting surfactant-rich phase is diluted by a fluidifi-cant before its analysis, in this method the fluorescence measurements were carried out directly ontothe undiluted surfactant-rich phase. The high viscosity provided by the undiluted surfactant rich phasegreatly 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 sensitivityallowing the ergotamine determination at trace level concentration. Under optimal experimental con-ditions, a linear calibration curve was obtained from 3.81 × 10−7 to 1.10 ␮g mL−1 , with detection andquantification limits of 0.11 and 0.38 pg mL−1 , respectively. The accuracy and versatility of the presentmethodology were proved by analyzing ergotamine in real samples of different natures such as pharma-ceuticals, urine and saliva.